data_Phosphoric_acid_I_0.5_GPa_S_xtal
_database_code_depnum_ccdc_archive 'CCDC 1578418'
#==============================================================================

# PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic      2017-09-28
_journal_date_to_coeditor         ?
_journal_date_from_coeditor       ?
_journal_date_accepted     2017-10-06
_journal_date_printers_first      ?
_journal_date_printers_final      ?
_journal_date_proofs_out          ?
_journal_date_proofs_in           ?
_journal_coeditor_name            ?
_journal_coeditor_code      XK5045SUP1
_journal_coeditor_notes
; ?
;
_journal_paper_category      FA
_journal_techeditor_code      B171441
_iucr_compatibility_tag          ACTA95
_journal_techeditor_notes  
;
;
_journal_coden_ASTM               ?
_journal_name_full                ?
_journal_year                     ?
_journal_volume                   ?
_journal_issue                    ?
_journal_page_first               ?
_journal_page_last                ?
_journal_suppl_publ_number        ?
_journal_suppl_publ_pages         ?

#==============================================================================


_audit_creation_method            SHELXL-97

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk
_publ_contact_author_address 
; 
 Diamond Light Source,
 Harwell Science and Innovation Campus, 
 Fermi Avenue,
 Didcot,
 OX11 0DE 
; 

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'H3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'H3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         97.994
_chemical_compound_source        'Sigma Aldrich'

 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    5.707(2)
_cell_length_b                    4.820(2)
_cell_length_c                    11.436(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  94.75(5)
_cell_angle_gamma                 90.00
_cell_volume                      313.49(18)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_pressure        0.5 #GPa
_cell_measurement_reflns_used     24
_cell_measurement_theta_min       3.58
_cell_measurement_theta_max       15.31
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.175
_exptl_crystal_size_min           0.075
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.076
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              200
_exptl_absorpt_coefficient_mu     0.692
_exptl_absorpt_correction_type    analytical
_exptl_absorpt_correction_T_min   0.247
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    
;
Diamond anvil cell absorption correction:
Absorb 6.0, R. J. Angel, J. Appl. Cryst., 2004, 37, 486-492
;

_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Nonius CAD4'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             1255
_diffrn_reflns_av_R_equivalents   0.0858
_diffrn_reflns_av_sigmaI/netI     0.0604
_diffrn_reflns_limit_h_min        -3
_diffrn_reflns_limit_h_max        3
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_k_max        8
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.58
_diffrn_reflns_theta_max          39.07
_reflns_number_total              360
_reflns_number_gt                 294
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 
------------------------------------------------------------------------------------
 checkCIF alerts
 

PROBLEM: _atom_site_aniso_label is missing
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.197 Note  

RESONSE: These are from a refinement against high pressure data. Many reflections
have been obscured by the steel body of the pressure cell and thus not measured.
There were insufficient data to allow anisotropic refinement of the atoms; all
atoms were refined isotropically.


------------------------------------------------------------------------------------
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.1304P)²+1.4756P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.11(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          360
_refine_ls_number_parameters      22
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0989
_refine_ls_R_factor_gt            0.0720
_refine_ls_wR_factor_ref          0.2169
_refine_ls_wR_factor_gt           0.1860
_refine_ls_goodness_of_fit_ref    0.982
_refine_ls_restrained_S_all       0.982
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
P1 P 0.2081(12) 0.3022(3) 0.13871(16) 0.0219(6) Uiso 1 1 d . . .
O1 O 0.285(2) 0.1660(9) 0.2524(5) 0.0327(12) Uiso 1 1 d . . .
O2 O 0.324(2) 0.5937(9) 0.1276(4) 0.0295(11) Uiso 1 1 d . . .
H2 H 0.3613 0.6556 0.1933 0.035 Uiso 1 1 calc R . .
O3 O -0.073(3) 0.3353(11) 0.1180(5) 0.0351(14) Uiso 1 1 d . . .
H3 H -0.1219 0.4148 0.1744 0.042 Uiso 1 1 calc R . .
O4 O 0.275(2) 0.1373(9) 0.0298(4) 0.0289(11) Uiso 1 1 d . . .
H4 H 0.2660 -0.0295 0.0429 0.035 Uiso 1 1 calc R . .
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
P1 O1 1.489(7) . ?
P1 O4 1.551(5) . ?
P1 O2 1.562(7) . ?
P1 O3 1.608(17) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 P1 O4 113.7(5) . . ?
O1 P1 O2 111.8(6) . . ?
O4 P1 O2 105.2(4) . . ?
O1 P1 O3 112.9(6) . . ?
O4 P1 O3 103.8(6) . . ?
O2 P1 O3 108.7(5) . . ?
 
_diffrn_measured_fraction_theta_max    0.197
_diffrn_reflns_theta_full              39.07
_diffrn_measured_fraction_theta_full   0.197
_refine_diff_density_max    0.454
_refine_diff_density_min   -0.532
_refine_diff_density_rms    0.153

data_Phosphoric_acid_II_1.8_GPa_S_Xtal
_database_code_depnum_ccdc_archive 'CCDC 1578419'

_audit_creation_method            SHELXL-97

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'H3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'H3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         97.994
_chemical_compound_source        'Sigma Aldrich'
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, y+1/2, -z+1/2'
 
_cell_length_a                    4.619(5)
_cell_length_b                    8.479(17)
_cell_length_c                    14.38(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      563.0(18)
_cell_formula_units_Z             8
_cell_measurement_temperature     293(2)
_cell_measurement_pressure        1.8 #GPa
_cell_measurement_reflns_used     19
_cell_measurement_theta_min       4.84
_cell_measurement_theta_max       12.37
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.15
_exptl_crystal_size_min           0.075
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.312
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              400
_exptl_absorpt_coefficient_mu     0.770
_exptl_absorpt_correction_type    analytical
_exptl_absorpt_correction_T_min   0.247
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    
;
Diamond anvil cell absorption correction:
Absorb 6.0, R. J. Angel, J. Appl. Cryst., 2004, 37, 486-492
;
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Nonius CAD4'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             2503
_diffrn_reflns_av_R_equivalents   0.1453
_diffrn_reflns_av_sigmaI/netI     0.1109
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          2.79
_diffrn_reflns_theta_max          39.56
_reflns_number_total              1649
_reflns_number_gt                 1296
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 
------------------------------------------------------------------------------------
 checkCIF alerts
 
PROBLEM: The minimum difference density is < -0.1*ZMAX*0.75
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
PROBLEM: The value of Rint is greater than 0.12
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.479 Note  
PROBLEM: The value of Rint is greater than 0.12 .........      0.145 Report
PROBLEM: High R1 Value ..................................       0.12 Report
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.32 Report
PROBLEM: Large Reported Max.  (Positive) Residual Density       1.23 eA-3  
PROBLEM: Large Reported Min.  (Negative) Residual Density      -1.26 eA-3  
PROBLEM: s.u. on the      a  - Axis is (Too) Large ......      0.005 Ang.  
PROBLEM: s.u. on the      b  - Axis is (Too) Large ......      0.017 Ang.  
PROBLEM: s.u. on the      c  - Axis is (Too) Large ......      0.030 Ang.  
PROBLEM: Short Inter D-H..H-D       H13    ..  H22     ..       2.12 Ang.  

RESONSE: These are from a refinement against high pressure data. Many reflections
have been obscured by the steel body of the pressure cell and thus not measured. Low
data completeness has led to high R-factors, noisy data and large uncertainties. 
Short contacts are to be expected as a result of structure compression.


PROBLEM: Flack test results are meaningless.
PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken. 

------------------------------------------------------------------------------------
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0644P)²+10.8552P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.0(7)
_refine_ls_number_reflns          1649
_refine_ls_number_parameters      91
_refine_ls_number_restraints      8
_refine_ls_R_factor_all           0.1690
_refine_ls_R_factor_gt            0.1219
_refine_ls_wR_factor_ref          0.3223
_refine_ls_wR_factor_gt           0.2702
_refine_ls_goodness_of_fit_ref    1.104
_refine_ls_restrained_S_all       1.103
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
P11 P 0.8976(6) 0.2884(4) -0.23095(19) 0.0268(7) Uani 1 1 d D . .
O11 O 0.6809(16) 0.1560(13) -0.2046(6) 0.038(3) Uani 1 1 d D . .
H11 H 0.7241 0.1196 -0.1536 0.045 Uiso 1 1 calc R . .
O12 O 1.080(2) 0.3361(13) -0.1482(5) 0.037(2) Uani 1 1 d D . .
O13 O 0.7238(17) 0.4267(11) -0.2728(6) 0.033(2) Uani 1 1 d D . .
H13 H 0.6705 0.4857 -0.2309 0.040 Uiso 1 1 calc R . .
O14 O 1.073(2) 0.2219(15) -0.3135(5) 0.048(3) Uani 1 1 d D . .
H14 H 1.0807 0.2881 -0.3550 0.057 Uiso 1 1 calc R . .
P22 P 0.5562(5) 0.5113(4) 0.0017(2) 0.0260(7) Uani 1 1 d D . .
O21 O 0.7931(15) 0.6426(12) 0.0140(6) 0.031(2) Uani 1 1 d D . .
H21 H 0.9446 0.6021 0.0317 0.038 Uiso 1 1 calc R . .
O22 O 0.4625(16) 0.5321(12) -0.1009(5) 0.031(2) Uani 1 1 d D . .
H22 H 0.3804 0.4519 -0.1187 0.037 Uiso 1 1 calc R . .
O23 O 0.7011(19) 0.3511(12) 0.0174(6) 0.035(2) Uani 1 1 d D . .
H23 H 0.6020 0.2981 0.0530 0.042 Uiso 1 1 calc R . .
O24 O 0.3052(15) 0.5377(11) 0.0687(5) 0.0267(18) Uani 1 1 d D . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
P11 0.0254(11) 0.028(2) 0.0269(13) 0.0006(10) -0.0013(10) -0.0014(10)
O11 0.023(3) 0.055(9) 0.035(5) 0.004(4) -0.005(3) -0.004(4)
O12 0.038(4) 0.042(8) 0.029(4) 0.003(3) -0.007(3) -0.010(4)
O13 0.039(4) 0.031(8) 0.029(4) -0.001(3) 0.002(3) 0.011(4)
O14 0.050(5) 0.071(10) 0.022(4) -0.005(4) 0.012(4) 0.026(6)
P22 0.0216(9) 0.028(2) 0.0283(12) 0.0018(10) 0.0011(9) -0.0014(10)
O21 0.016(3) 0.029(7) 0.050(5) 0.009(3) -0.003(3) -0.001(3)
O22 0.036(4) 0.032(7) 0.025(4) 0.007(3) -0.003(3) -0.014(3)
O23 0.035(4) 0.016(8) 0.055(6) 0.008(3) 0.010(3) 0.010(4)
O24 0.025(3) 0.028(7) 0.027(4) -0.003(3) 0.003(2) -0.001(3)
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
P11 O12 1.512(8) . ?
P11 O14 1.542(8) . ?
P11 O13 1.544(9) . ?
P11 O11 1.551(9) . ?
P22 O24 1.524(7) . ?
P22 O23 1.531(9) . ?
P22 O22 1.547(8) . ?
P22 O21 1.571(8) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O12 P11 O14 114.2(6) . . ?
O12 P11 O13 113.1(6) . . ?
O14 P11 O13 104.5(5) . . ?
O12 P11 O11 111.2(5) . . ?
O14 P11 O11 105.2(7) . . ?
O13 P11 O11 108.0(5) . . ?
O24 P22 O23 111.7(5) . . ?
O24 P22 O22 111.9(5) . . ?
O23 P22 O22 111.3(5) . . ?
O24 P22 O21 110.8(5) . . ?
O23 P22 O21 107.9(5) . . ?
O22 P22 O21 102.8(5) . . ?
 
_diffrn_measured_fraction_theta_max    0.479
_diffrn_reflns_theta_full              39.56
_diffrn_measured_fraction_theta_full   0.479
_refine_diff_density_max    1.229
_refine_diff_density_min   -1.259
_refine_diff_density_rms    0.305

data_Phosphoric_acid_I_0.01_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578420'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk
_publ_contact_author_address 
; 
 Diamond Light Source,
 Harwell Science and Innovation Campus, 
 Fermi Avenue,
 Didcot,
 OX11 0DE 
; 

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  '-x, y+1/2, -z+1/2 '
  '-x, -y, -z '
  'x, -y+1/2, z+1/2 '

_cell_length_a      5.7493(5)
_cell_length_b      4.83921(33)
_cell_length_c      11.6170(8)
_cell_angle_alpha   90.0
_cell_angle_beta    95.150(7)
_cell_angle_gamma   90.0
_cell_volume        321.902(30)
_cell_formula_units_Z            4

_cell_measurement_temperature    295
_cell_measurement_pressure       0.01 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.084

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0458
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.13
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1901

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     54
_refine_ls_number_restraints     13
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.01

_computing_data_collection        'Custom ISIS software' 
_computing_cell_refinement        'GSAS' 

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Negative Isotropic ADP for P       .............     -0.003 Report
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of          P Check 

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the
neutron beam is attenuated by a substantial quantity of anvil material and can cause
issues with displacement parameter refinement.
Refinement of the P atom Uiso to a sensible value was not possible, the only 
alternative being to fix it to an arbitrary positive value.
Although the refined parameter is unphysical, no conclusions are being drawn from
fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus
of the corresponding manuscript is on molecular packing only.

------------------------------------------------------------------------------------
;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P  P       0.2153(15)   0.3027(15)   0.1388(6)    1.0   Uiso  -0.0031(23)    4
O  O1      0.2870(19)   0.1702(22)   0.2534(7)    1.0   Uiso   0.0080(13)    4
O  O2      0.3329(19)   0.5898(19)   0.1301(9)    1.0   Uiso   0.0080(13)    4
O  O3     -0.0537(16)   0.3391(23)   0.1249(9)    1.0   Uiso   0.0080(13)    4
O  O4      0.2914(22)   0.1316(18)   0.0363(8)    1.0   Uiso   0.0080(13)    4
D  D2      0.4818(25)   0.6095(33)   0.1758(11)   1.0   Uiso   0.0412(28)    4
D  D3     -0.1319(26)   0.4808(24)   0.1725(12)   1.0   Uiso   0.0412(28)    4
D  D4      0.2775(25)  -0.0632(22)   0.0478(12)   1.0   Uiso   0.0412(28)    4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   4.0        
                   D  12.0        
                   O  16.0        


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag   
P   O1   1.502(11) . . no     
P   O2   1.552(12) . . no     
P   O3   1.551(13) . . no     
P   O4   1.545(12) . . no
O2  D2   0.972(16) . . no     
O3  D3   1.013(16) . . no     
O4  D4   0.955(13) . . no
 
 
 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1  P   O2   110.7(7) . . . no       
O1  P   O3   109.4(7) . . . no       
O1  P   O4   112.4(7) . . . no
O2  P   O3   109.2(7) . . . no       
O2  P   O4   106.0(7) . . . no       
O3  P   O4   109.1(7) . . . no
P   O2  D2  115.0(12) . . . no       
P   O3  D3  120.5(13) . . . no       
P   O4  D4  112.9(12) . . . no


loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag    
O1  P  O2  D2    27.9(15) . . . . no    
O3  P  O2  D2   148.4(12) . . . . no    
O4  P  O2  D2   -94.2(13) . . . . no
O1  P  O3  D3    71.1(14) . . . . no    
O2  P  O3  D3   -50.2(14) . . . . no    
O4  P  O3  D3  -165.6(12) . . . . no
O1  P  O4  D4    37.6(15) . . . . no    
O2  P  O4  D4   158.6(12) . . . . no    
O3  P  O4  D4   -84.0(13) . . . . no



data_Phosphoric_acid_I_0.44_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578421'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  '-x, y+1/2, -z+1/2 '
  '-x, -y, -z '
  'x, -y+1/2, z+1/2 '

_cell_length_a     5.6927(4)
_cell_length_b     4.81609(27)
_cell_length_c     11.4468(7)
_cell_angle_alpha  90.0
_cell_angle_beta   94.704(6)
_cell_angle_gamma  90.0
_cell_volume       312.776(23)
_cell_formula_units_Z            4

_cell_measurement_temperature    295
_cell_measurement_pressure       0.44 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.145

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0510
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.27
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.2216

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     55
_refine_ls_number_restraints     13
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.04

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Negative Isotropic ADP for P       .............     -0.006 Report
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of          P Check 

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the
neutron beam is attenuated by a substantial quantity of anvil material and can cause
issues with displacement parameter refinement.
Refinement of the P atom Uiso to a sensible value was not possible, the only 
alternative being to fix it to an arbitrary positive value.
Although the refined parameter is unphysical, no conclusions are being drawn from
fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus
of the corresponding manuscript is on molecular packing only.

------------------------------------------------------------------------------------
;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P       0.2102(14)   0.3000(13)   0.1370(6)    1.0        Uiso  -0.0059(16)    4
O O1      0.2847(17)   0.1653(20)   0.2526(7)    1.0        Uiso   0.0131(12)    4
O O2      0.3194(19)   0.5925(17)   0.1283(8)    1.0        Uiso   0.0131(12)    4
O O3     -0.0609(16)   0.3227(21)   0.1226(8)    1.0        Uiso   0.0131(12)    4
O O4      0.2824(19)   0.1397(17)   0.0301(7)    1.0        Uiso   0.0131(12)    4
D D2      0.4720(21)   0.6320(26)   0.1733(10)   1.0        Uiso   0.0438(22)    4
D D3     -0.1351(22)   0.4736(22)   0.1725(11)   1.0        Uiso   0.0438(22)    4
D D4      0.2742(22)  -0.0628(19)   0.0424(11)   1.0        Uiso   0.0438(22)    4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   4.0        
                   D  12.0        
                   O  16.0        


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag   
P   O1   1.504(11) . . no     
P   O2   1.546(11) . . no     
P   O3   1.543(12) . . no     
P   O4   1.531(11) . . no
O2  D2   0.991(16) . . no     
O3  D3   1.036(14) . . no     
O4  D4   0.987(12) . . no
 
 
 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1  P   O2   111.4(7) . . . no       
O1  P   O3   109.4(7) . . . no       
O1  P   O4   114.2(6) . . . no
O2  P   O3   109.4(7) . . . no       
O2  P   O4   105.8(6) . . . no       
O3  P   O4   106.4(7) . . . no
P   O2  D2  118.8(11) . . . no       
P   O3  D3  116.2(10) . . . no       
P   O4  D4  111.4(10) . . . no



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag    
O1  P  O2  D2    27.9(14) . . . . no    
O3  P  O2  D2   149.0(12) . . . . no    
O4  P  O2  D2   -96.8(12) . . . . no
O1  P  O3  D3    74.2(12) . . . . no    
O2  P  O3  D3   -48.0(12) . . . . no    
O4  P  O3  D3  -161.9(10) . . . . no
O1  P  O4  D4    35.8(14) . . . . no    
O2  P  O4  D4   158.7(11) . . . . no    
O3  P  O4  D4   -85.1(12) . . . . no



data_Phosphoric_acid_I_0.93_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578422'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  '-x, y+1/2, -z+1/2 '
  '-x, -y, -z '
  'x, -y+1/2, z+1/2 '

_cell_length_a     5.6334(4)
_cell_length_b     4.78996(32)
_cell_length_c     11.3055(8)
_cell_angle_alpha  90.0
_cell_angle_beta   94.255(7)
_cell_angle_gamma  90.0
_cell_volume       304.226(25)
_cell_formula_units_Z            4

_cell_measurement_temperature    295
_cell_measurement_pressure       0.93 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.205

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0566
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.33
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor          0.1966

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     60
_refine_ls_number_restraints     13
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.02

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 


------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of          P Check 

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the
neutron beam is attenuated by a substantial quantity of anvil material and can cause
issues with displacement parameter refinement.
Refinement of the P atom Uiso to a sensible value was not possible, the only 
alternative being to fix it to an arbitrary positive value.
Although the refined parameter is unphysical, no conclusions are being drawn from
fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus
of the corresponding manuscript is on molecular packing only.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P       0.2086(17)   0.3017(15)   0.1349(6)    1.0        Uiso  -0.0004(24)    4
O O1      0.2906(21)   0.1693(22)   0.2526(9)    1.0        Uiso   0.0167(16)    4
O O2      0.3074(22)   0.6003(19)   0.1272(9)    1.0        Uiso   0.0167(16)    4
O O3     -0.0641(19)   0.3116(24)   0.1223(10)   1.0        Uiso   0.0167(16)    4
O O4      0.2828(21)   0.1376(19)   0.0285(8)    1.0        Uiso   0.0167(16)    4
D D2      0.4646(24)   0.6381(27)   0.1751(12)   1.0        Uiso   0.0442(24)    4
D D3     -0.1391(24)   0.4659(24)   0.1755(12)   1.0        Uiso   0.0442(24)    4
D D4      0.2722(25)  -0.0678(20)   0.0342(12)   1.0        Uiso   0.0442(24)    4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   4.0        
                   D  12.0        
                   O  16.0        


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag   
P   O1   1.516(12) . . no     
P   O2   1.539(12) . . no     
P   O3   1.533(14) . . no     
P   O4   1.522(12) . . no
O2  D2   1.023(16) . . no     
O3  D3   1.059(15) . . no     
O4  D4   0.989(13) . . no
 
 
 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1  P   O2   110.6(7) . . . no       
O1  P   O3   109.5(8) . . . no       
O1  P   O4   113.1(7) . . . no
O2  P   O3   109.1(7) . . . no       
O2  P   O4   108.3(7) . . . no       
O3  P   O4   106.0(7) . . . no
P   O2  D2  115.9(12) . . . no       
P   O3  D3  114.1(11) . . . no       
P   O4  D4  116.1(11) . . . no



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag    
O1  P  O2  D2    28.3(15) . . . . no    
O3  P  O2  D2   148.8(12) . . . . no    
O4  P  O2  D2   -96.2(13) . . . . no
O1  P  O3  D3    74.2(12) . . . . no    
O2  P  O3  D3   -47.0(13) . . . . no    
O4  P  O3  D3  -163.4(11) . . . . no
O1  P  O4  D4    40.1(15) . . . . no    
O2  P  O4  D4   163.1(12) . . . . no    
O3  P  O4  D4   -79.9(13) . . . . no



data_Phosphoric_acid_I_1.50_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578423'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  '-x, y+1/2, -z+1/2 '
  '-x, -y, -z '
  'x, -y+1/2, z+1/2 '

_cell_length_a     5.5686(4)
_cell_length_b     4.7647(4)
_cell_length_c     11.1762(9)
_cell_angle_alpha  90.0
_cell_angle_beta   93.810(7)
_cell_angle_gamma  90.0
_cell_volume       295.877(28)
_cell_formula_units_Z            4

_cell_measurement_temperature    295
_cell_measurement_pressure       1.50 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.268

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0571
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.30
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.159

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     60
_refine_ls_number_restraints     13
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.01

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Negative Isotropic ADP for P       .............     -0.005 Report
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of          P Check 

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the
neutron beam is attenuated by a substantial quantity of anvil material and can cause
issues with displacement parameter refinement.
Refinement of the P atom Uiso to a sensible value was not possible, the only 
alternative being to fix it to an arbitrary positive value.
Although the refined parameter is unphysical, no conclusions are being drawn from
fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus
of the corresponding manuscript is on molecular packing only.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P       0.2036(16)   0.3023(14)   0.1338(6)    1.0        Uiso  -0.0049(20)    4
O O1      0.2914(21)   0.1656(21)   0.2511(8)    1.0        Uiso   0.0167(16)    4
O O2      0.3043(22)   0.6009(18)   0.1258(10)   1.0        Uiso   0.0167(16)    4
O O3     -0.0710(18)   0.3084(23)   0.1230(10)   1.0        Uiso   0.0167(16)    4
O O4      0.2777(23)   0.1440(20)   0.0233(8)    1.0        Uiso   0.0167(16)    4
D D2      0.4652(24)   0.6464(23)   0.1732(12)   1.0        Uiso   0.0392(21)    4
D D3     -0.1487(21)   0.4585(24)   0.1751(11)   1.0        Uiso   0.0392(21)    4
D D4      0.2720(24)  -0.0636(19)   0.0272(13)   1.0        Uiso   0.0392(21)    4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   4.0        
                   D  12.0        
                   O  16.0        


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag   
P   O1   1.514(11) . . no     
P   O2   1.533(11) . . no     
P   O3   1.526(13) . . no     
P   O4   1.528(12) . . no
O2  D2   1.033(16) . . no     
O3  D3   1.039(15) . . no     
O4  D4   0.991(13) . . no
 
 
 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1  P   O2   110.6(7) . . . no       
O1  P   O3   109.8(8) . . . no       
O1  P   O4   113.5(7) . . . no
O2  P   O3   110.3(7) . . . no       
O2  P   O4   106.9(7) . . . no       
O3  P   O4   105.6(7) . . . no
P   O2  D2  118.1(10) . . . no       
P   O3  D3  115.0(10) . . . no       
P   O4  D4  116.5(11) . . . no



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag    
O1  P  O2  D2    26.8(15) . . . . no    
O3  P  O2  D2   148.4(12) . . . . no    
O4  P  O2  D2   -97.3(13) . . . . no
O1  P  O3  D3    75.8(12) . . . . no    
O2  P  O3  D3   -46.2(13) . . . . no    
O4  P  O3  D3  -161.4(11) . . . . no
O1  P  O4  D4    39.4(15) . . . . no    
O2  P  O4  D4   161.6(12) . . . . no    
O3  P  O4  D4   -81.0(13) . . . . no



data_Phosphoric_acid_I_1.79_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578424'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  '-x, y+1/2, -z+1/2 '
  '-x, -y, -z '
  'x, -y+1/2, z+1/2 '

_cell_length_a     5.5356(5)
_cell_length_b     4.7522(4)
_cell_length_c     11.1169(9)
_cell_angle_alpha  90.0
_cell_angle_beta   93.561(8)
_cell_angle_gamma  90.0
_cell_volume       291.879(29)
_cell_formula_units_Z            4

_cell_measurement_temperature    295
_cell_measurement_pressure       1.79 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.299

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0579
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.28
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1683

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     60
_refine_ls_number_restraints     13
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.01

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Negative Isotropic ADP for P       .............     -0.005 Report
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of          P Check 

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the
neutron beam is attenuated by a substantial quantity of anvil material and can cause
issues with displacement parameter refinement.
Refinement of the P atom Uiso to a sensible value was not possible, the only 
alternative being to fix it to an arbitrary positive value.
Although the refined parameter is unphysical, no conclusions are being drawn from
fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus
of the corresponding manuscript is on molecular packing only.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P       0.2031(16)   0.3009(14)   0.1326(6)    1.0        Uiso  -0.0050(20)    4
O O1      0.2887(21)   0.1616(21)   0.2498(8)    1.0        Uiso   0.0152(16)    4
O O2      0.3031(23)   0.6023(18)   0.1286(10)   1.0        Uiso   0.0152(16)    4
O O3     -0.0731(18)   0.3060(22)   0.1238(10)   1.0        Uiso   0.0152(16)    4
O O4      0.2865(22)   0.1445(20)   0.0213(8)    1.0        Uiso   0.0152(16)    4
D D2      0.4626(24)   0.6475(23)   0.1712(12)   1.0        Uiso   0.0386(21)    4
D D3     -0.1533(21)   0.4539(24)   0.1742(11)   1.0        Uiso   0.0386(21)    4
D D4      0.2700(23)  -0.0634(20)   0.0241(12)   1.0        Uiso   0.0386(21)    4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   4.0        
                   D  12.0        
                   O  16.0        


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag   
P   O1   1.511(11) . . no     
P   O2   1.537(11) . . no     
P   O3   1.526(13) . . no     
P   O4   1.539(12) . . no
O2  D2   1.002(16) . . no     
O3  D3   1.017(15) . . no     
O4  D4   0.994(13) . . no

 
 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1  P   O2   109.7(7) . . . no       
O1  P   O3   108.8(7) . . . no       
O1  P   O4   112.9(7) . . . no
O2  P   O3   110.1(7) . . . no       
O2  P   O4   107.4(7) . . . no       
O3  P   O4   107.9(7) . . . no
P   O2  D2  119.8(10) . . . no       
P   O3  D3  116.3(11) . . . no       
P   O4  D4  114.8(11) . . . no



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag    
O1  P  O2  D2    30.7(15) . . . . no    
O3  P  O2  D2   150.4(13) . . . . no    
O4  P  O2  D2   -92.4(14) . . . . no
O1  P  O3  D3    76.9(12) . . . . no    
O2  P  O3  D3   -43.4(14) . . . . no    
O4  P  O3  D3  -160.3(11) . . . . no
O1  P  O4  D4    44.2(14) . . . . no    
O2  P  O4  D4   165.2(12) . . . . no    
O3  P  O4  D4   -76.1(13) . . . . no



data_Phosphoric_acid_I_2.09_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578425'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  '-x, y+1/2, -z+1/2 '
  '-x, -y, -z '
  'x, -y+1/2, z+1/2 '

_cell_length_a     5.5049(5)
_cell_length_b     4.7401(4)
_cell_length_c     11.0668(10)
_cell_angle_alpha  90.0
_cell_angle_beta   93.355(9)
_cell_angle_gamma  90.0
_cell_volume       288.279(33)
_cell_formula_units_Z            4

_cell_measurement_temperature    295
_cell_measurement_pressure       2.09 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.327

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0639
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.35
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1481

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     60
_refine_ls_number_restraints     13
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.03

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Negative Isotropic ADP for P       .............     -0.010 Report
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of          P Check 

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the
neutron beam is attenuated by a substantial quantity of anvil material and can cause
issues with displacement parameter refinement.
Refinement of the P atom Uiso to a sensible value was not possible, the only 
alternative being to fix it to an arbitrary positive value.
Although the refined parameter is unphysical, no conclusions are being drawn from
fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus
of the corresponding manuscript is on molecular packing only.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P       0.2013(16)   0.2989(15)   0.1312(7)    1.0        Uiso  -0.0097(14)    4
O O1      0.2973(23)   0.1600(22)   0.2483(9)    1.0        Uiso   0.0195(18)    4
O O2      0.2947(25)   0.6052(19)   0.1297(11)   1.0        Uiso   0.0195(18)    4
O O3     -0.0769(19)   0.3000(24)   0.1250(11)   1.0        Uiso   0.0195(18)    4
O O4      0.2851(25)   0.1501(23)   0.0172(9)    1.0        Uiso   0.0195(18)    4
D D2      0.4622(25)   0.6515(23)   0.1720(13)   1.0        Uiso   0.0346(21)    4
D D3     -0.1550(21)   0.4515(25)   0.1755(11)   1.0        Uiso   0.0346(21)    4
D D4      0.2680(24)  -0.0578(21)   0.0201(12)   1.0        Uiso   0.0346(21)    4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   4.0        
                   D  12.0        
                   O  16.0        


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag   
P   O1   1.520(13) . . no     
P   O2   1.541(12) . . no     
P   O3   1.529(14) . . no     
P   O4   1.540(13) . . no
O2  D2   1.031(16) . . no     
O3  D3   1.022(15) . . no     
O4  D4   0.991(13) . . no

 
 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1  P   O2   108.5(8) . . . no       
O1  P   O3   109.6(8) . . . no       
O1  P   O4   113.2(7) . . . no
O2  P   O3   109.4(7) . . . no       
O2  P   O4   107.9(7) . . . no       
O3  P   O4   108.2(8) . . . no
P   O2  D2  119.2(10) . . . no       
P   O3  D3  115.5(11) . . . no       
P   O4  D4  113.3(11) . . . no



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag    
O1  P  O2  D2    31.7(16) . . . . no    
O3  P  O2  D2   151.3(13) . . . . no    
O4  P  O2  D2   -91.3(15) . . . . no
O1  P  O3  D3    78.5(13) . . . . no    
O2  P  O3  D3   -40.4(14) . . . . no    
O4  P  O3  D3  -157.6(11) . . . . no
O1  P  O4  D4    46.0(14) . . . . no    
O2  P  O4  D4   166.1(12) . . . . no    
O3  P  O4  D4   -75.7(13) . . . . no



data_Phosphoric_acid_I_2.79_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578426'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  '-x, y+1/2, -z+1/2 '
  '-x, -y, -z '
  'x, -y+1/2, z+1/2 '

_cell_length_a     5.4357(6)
_cell_length_b     4.7148(5)
_cell_length_c     10.9698(12)
_cell_angle_alpha  90.0
_cell_angle_beta   92.874(11)
_cell_angle_gamma  90.0
_cell_volume       280.79(4)
_cell_formula_units_Z            4

_cell_measurement_temperature    295
_cell_measurement_pressure       2.79 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.389

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0631
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.35
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1492

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     60
_refine_ls_number_restraints     13
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.01

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Negative Isotropic ADP for P       .............     -0.007 Report
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of          P Check 

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the
neutron beam is attenuated by a substantial quantity of anvil material and can cause
issues with displacement parameter refinement.
Refinement of the P atom Uiso to a sensible value was not possible, the only 
alternative being to fix it to an arbitrary positive value.
Although the refined parameter is unphysical, no conclusions are being drawn from
fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus
of the corresponding manuscript is on molecular packing only.

------------------------------------------------------------------------------------
;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P       0.2002(16)   0.3006(15)   0.1290(7)    1.0        Uiso  -0.0070(19)    4
O O1      0.3076(22)   0.1613(20)   0.2423(9)    1.0        Uiso   0.0147(17)    4
O O2      0.2890(25)   0.6106(18)   0.1342(11)   1.0        Uiso   0.0147(17)    4
O O3     -0.0825(19)   0.2968(23)   0.1251(11)   1.0        Uiso   0.0147(17)    4
O O4      0.2896(23)   0.1566(24)   0.0113(9)    1.0        Uiso   0.0147(17)    4
D D2      0.4556(26)   0.6576(24)   0.1735(15)   1.0        Uiso   0.0449(26)    4
D D3     -0.1635(21)   0.4522(26)   0.1769(12)   1.0        Uiso   0.0449(26)    4
D D4      0.2728(26)  -0.0558(24)   0.0168(13)   1.0        Uiso   0.0449(26)    4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   4.0        
                   D  12.0        
                   O  16.0        


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag   
P   O1   1.499(13) . . no     
P   O2   1.539(11) . . no     
P   O3   1.535(14) . . no     
P   O4   1.558(13) . . no
O2  D2     1.01(2) . . no     
O3  D3   1.039(17) . . no     
O4  D4   1.011(13) . . no


 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1  P   O2   106.1(7) . . . no       
O1  P   O3   111.6(8) . . . no       
O1  P   O4   111.8(7) . . . no
O2  P   O3   108.9(7) . . . no       
O2  P   O4   109.4(7) . . . no       
O3  P   O4   109.1(8) . . . no
P   O2  D2  120.0(10) . . . no       
P   O3  D3  115.5(11) . . . no       
P   O4  D4  110.4(12) . . . no



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag    
O1  P  O2  D2    32.7(17) . . . . no    
O3  P  O2  D2   152.9(15) . . . . no    
O4  P  O2  D2   -88.0(16) . . . . no
O1  P  O3  D3    80.2(13) . . . . no    
O2  P  O3  D3   -36.6(15) . . . . no    
O4  P  O3  D3  -155.9(12) . . . . no
O1  P  O4  D4    48.0(15) . . . . no    
O2  P  O4  D4   165.3(13) . . . . no    
O3  P  O4  D4   -75.8(14) . . . . no



data_Phosphoric_acid_I_3.17_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578427'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  '-x, y+1/2, -z+1/2 '
  '-x, -y, -z '
  'x, -y+1/2, z+1/2 '

_cell_length_a     5.4030(7)
_cell_length_b     4.7036(6)
_cell_length_c     10.9238(14)
_cell_angle_alpha  90.0
_cell_angle_beta   92.633(13)
_cell_angle_gamma  90.0
_cell_volume       277.32(4)
_cell_formula_units_Z            4

_cell_measurement_temperature    295
_cell_measurement_pressure       3.17 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.419

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0631
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.36
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1145


_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     60
_refine_ls_number_restraints     13
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.04

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Negative Isotropic ADP for P       .............     -0.011 Report
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of          P Check 

RESPONSE: These are high-pressure data recorded using a Paris-Edinburgh press - the
neutron beam is attenuated by a substantial quantity of anvil material and can cause
issues with displacement parameter refinement.
Refinement of the P atom Uiso to a sensible value was not possible, the only 
alternative being to fix it to an arbitrary positive value.
Although the refined parameter is unphysical, no conclusions are being drawn from
fine geometric details of the molecule (e.g. ADP's, bond lengths, etc). The focus
of the corresponding manuscript is on molecular packing only.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P       0.1982(16)   0.3010(15)   0.1285(7)    1.0        Uiso  -0.0108(13)    4
O O1      0.3122(22)   0.1631(21)   0.2410(9)    1.0        Uiso   0.0155(18)    4
O O2      0.2903(26)   0.6099(19)   0.1330(12)   1.0        Uiso   0.0155(18)    4
O O3     -0.0867(19)   0.2983(25)   0.1270(12)   1.0        Uiso   0.0155(18)    4
O O4      0.2914(24)   0.1588(25)   0.0101(9)    1.0        Uiso   0.0155(18)    4
D D2      0.4511(27)   0.6652(25)   0.1742(16)   1.0        Uiso   0.0456(27)    4
D D3     -0.1674(23)   0.4504(27)   0.1783(13)   1.0        Uiso   0.0456(27)    4
D D4      0.2687(28)  -0.0545(25)   0.0140(14)   1.0        Uiso   0.0456(27)    4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   4.0        
                   D  12.0        
                   O  16.0        


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag   
P   O1   1.497(13) . . no     
P   O2   1.535(12) . . no     
P   O3   1.539(13) . . no     
P   O4   1.559(13) . . no
O2  D2     1.00(2) . . no     
O3  D3   1.018(17) . . no     
O4  D4   1.015(13) . . no


 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1  P   O2   105.3(8) . . . no       
O1  P   O3   112.2(8) . . . no       
O1  P   O4   111.1(7) . . . no
O2  P   O3   109.3(8) . . . no       
O2  P   O4   108.4(8) . . . no       
O3  P   O4   110.3(8) . . . no
P   O2  D2  122.4(12) . . . no       
P   O3  D3  116.1(11) . . . no       
P   O4  D4  110.3(12) . . . no



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag    
O1  P  O2  D2       28(2) . . . . no    
O3  P  O2  D2   149.0(17) . . . . no    
O4  P  O2  D2   -90.7(18) . . . . no
O1  P  O3  D3    80.0(14) . . . . no    
O2  P  O3  D3   -36.4(16) . . . . no    
O4  P  O3  D3  -155.6(13) . . . . no
O1  P  O4  D4    51.5(15) . . . . no    
O2  P  O4  D4   166.7(13) . . . . no    
O3  P  O4  D4   -73.6(14) . . . . no

data_Phosphoric_acid_I_0.04_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578428'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  '-x, y+1/2, -z+1/2 '
  '-x, -y, -z '
  'x, -y+1/2, z+1/2 '

_cell_length_a       5.7466(8)
_cell_length_b       4.8378(7)
_cell_length_c       11.6028(15)
_cell_angle_alpha    90.0
_cell_angle_beta     95.107(13)
_cell_angle_gamma    90.0
_cell_volume         321.29(5)
_cell_formula_units_Z            4

_cell_measurement_temperature    295
_cell_measurement_pressure       0.04 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.088

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.1110
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   0.87
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.3058

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     59
_refine_ls_number_restraints     13
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.02

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P       0.2042(23)   0.3091(27)   0.1359(10)   1.0        Uiso   0.005(6)      4
O O1      0.2773(31)   0.174(4)     0.2499(11)   1.0        Uiso   0.0110(27)    4
O O2      0.3243(33)   0.5951(31)   0.1322(16)   1.0        Uiso   0.0110(27)    4
O O3     -0.0651(24)   0.347(4)     0.1213(15)   1.0        Uiso   0.0110(27)    4
O O4      0.282(4)     0.1341(31)   0.0343(12)   1.0        Uiso   0.0110(27)    4
D D2      0.475(4)     0.616(6)     0.1741(18)   1.0        Uiso   0.038(5)      4
D D3     -0.129(4)     0.479(4)     0.1714(19)   1.0        Uiso   0.038(5)      4
D D4      0.265(4)    -0.055(4)     0.0415(20)   1.0        Uiso   0.038(5)      4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   4.0        
                   D  12.0        
                   O  16.0        


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag   
P   O1   1.501(19) . . no     
P   O2     1.55(2) . . no     
P   O3   1.551(17) . . no     
P   O4     1.55(2) . . no
O2  D2     0.96(3) . . no     
O3  D3     0.96(3) . . no     
O4  D4     0.93(2) . . no


 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1  P   O2  108.9(12) . . . no       
O1  P   O3  110.2(12) . . . no       
O1  P   O4  110.8(12) . . . no
O2  P   O3  109.5(13) . . . no       
O2  P   O4  107.9(12) . . . no       
O3  P   O4  109.6(13) . . . no
P   O2  D2     118(2) . . . no       
P   O3  D3  116.4(19) . . . no       
P   O4  D4     115(2) . . . no



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag    
O1  P  O2  D2    31(3) . . . . no    
O3  P  O2  D2   152(2) . . . . no    
O4  P  O2  D2   -89(2) . . . . no
O1  P  O3  D3    69(2) . . . . no    
O2  P  O3  D3   -51(2) . . . . no    
O4  P  O3  D3  -169(2) . . . . no
O1  P  O4  D4    40(3) . . . . no    
O2  P  O4  D4   160(2) . . . . no    
O3  P  O4  D4   -81(3) . . . . no

data_Phosphoric_acid_II_0.86_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578429'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a     4.6648(4)
_cell_length_b     8.6057(7)
_cell_length_c     14.5932(11)
_cell_angle_alpha  90.0
_cell_angle_beta   90.0
_cell_angle_gamma  90.0
_cell_volume       585.83(5)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       0.86 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.291

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0428
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.32
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1366

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.01

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8891(25)   0.2929(12)  -0.2291(7)    1.0        Uiso   0.0057(8)     4
O O11     0.6771(31)   0.1643(16)  -0.1997(10)   1.0        Uiso   0.0057(8)     4
D D11     0.727(4)     0.0831(19)  -0.1584(11)   1.0        Uiso   0.0261(21)    4
O O12     1.0724(34)   0.3333(18)  -0.1459(9)    1.0        Uiso   0.0057(8)     4
O O13     0.7239(31)   0.4372(14)  -0.2648(10)   1.0        Uiso   0.0057(8)     4
D D13     0.665(4)     0.5094(22)  -0.2187(11)   1.0        Uiso   0.0261(21)    4
O O14     1.0771(30)   0.2288(17)  -0.3081(9)    1.0        Uiso   0.0057(8)     4
D D14     1.154(4)     0.2967(21)  -0.3550(10)   1.0        Uiso   0.0261(21)    4
P P22     0.5534(22)   0.5124(12)   0.0012(8)    1.0        Uiso   0.0057(8)     4
O O21     0.7890(26)   0.6360(14)   0.0170(11)   1.0        Uiso   0.0057(8)     4
D D21     0.9793(34)   0.6020(20)   0.0388(13)   1.0        Uiso   0.0261(21)    4
O O22     0.4563(30)   0.5284(18)  -0.1003(8)    1.0        Uiso   0.0057(8)     4
D D22     0.311(4)     0.4516(23)  -0.1151(12)   1.0        Uiso   0.0261(21)    4
O O23     0.6879(31)   0.3494(13)   0.0147(11)   1.0        Uiso   0.0057(8)     4
D D23     0.633(4)     0.2813(21)   0.0648(12)   1.0        Uiso   0.0261(21)    4
O O24     0.3058(29)   0.5313(17)   0.0691(9)    1.0        Uiso   0.0057(8)     4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11   1.545(17) . . no     
P11  O12   1.524(17) . . no     
P11  O13   1.551(16) . . no     
P11  O14   1.550(17) . . no
O11  D11     0.95(2) . . no     
O13  D13     0.95(2) . . no     
O14  D14     0.97(2) . . no
P22  O21   1.548(16) . . no     
P22  O22   1.555(17) . . no     
P22  O23   1.550(16) . . no      
P22  O24   1.528(17) . . no
O21  D21     0.99(2) . . no     
O22  D22     0.97(2) . . no     
O23  D23     0.97(2) . . no

 
 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  107.5(10) . . . no       
O11  P11  O13   110.4(9) . . . no       
O11  P11  O14  108.3(10) . . . no
O12  P11  O13  111.3(10) . . . no       
O12  P11  O14   110.9(9) . . . no       
O13  P11  O14  108.4(10) . . . no
P11  O11  D11  123.0(17) . . . no       
P11  O13  D13  115.1(16) . . . no       
P11  O14  D14  121.3(16) . . . no
O21  P22  O22  106.7(10) . . . no       
O21  P22  O23   108.3(9) . . . no       
O21  P22  O24  111.5(10) . . . no
O22  P22  O23  108.6(10) . . . no       
O22  P22  O24   112.9(9) . . . no       
O23  P22  O24  108.7(10) . . . no
P22  O21  D21  118.9(15) . . . no       
P22  O22  D22  110.9(15) . . . no       
P22  O23  D23  122.4(17) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11      -37(2) . . . . no    
O13  P11  O11  D11  -158.7(18) . . . . no    
O14  P11  O11  D11       83(2) . . . . no
O11  P11  O13  D13    85.6(19) . . . . no    
O12  P11  O13  D13      -34(2) . . . . no    
O14  P11  O13  D13  -155.9(17) . . . . no
O11  P11  O14  D14   150.0(18) . . . . no    
O12  P11  O14  D14   -92.3(19) . . . . no    
O13  P11  O14  D14       30(2) . . . . no
O22  P22  O21  D21  -123.0(19) . . . . no    
O23  P22  O21  D21       -6(2) . . . . no    
O24  P22  O21  D21   113.4(19) . . . . no
O21  P22  O22  D22   178.5(16) . . . . no    
O23  P22  O22  D22    62.0(18) . . . . no    
O24  P22  O22  D22   -58.6(19) . . . . no
O21  P22  O23  D23   113.8(19) . . . . no    
O22  P22  O23  D23  -130.7(19) . . . . no    
O24  P22  O23  D23       -8(2) . . . . no



data_Phosphoric_acid_II_1.24_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578430'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.6494(5)
_cell_length_b      8.5580(9)
_cell_length_c      14.5078(14)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        577.26(6)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       1.24 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.325

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0454
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.34
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1263

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.04

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8864(27)   0.2884(13)  -0.2291(8)    1.0        Uiso   0.0051(9)     4
O O11     0.676(4)     0.1572(18)  -0.2005(11)   1.0        Uiso   0.0051(9)     4
D D11     0.724(4)     0.0833(22)  -0.1555(12)   1.0        Uiso   0.0290(24)    4
O O12     1.070(4)     0.3350(20)  -0.1463(10)   1.0        Uiso   0.0051(9)     4
O O13     0.7241(34)   0.4337(15)  -0.2667(11)   1.0        Uiso   0.0051(9)     4
D D13     0.664(4)     0.5110(24)  -0.2216(13)   1.0        Uiso   0.0290(24)    4
O O14     1.0800(33)   0.2238(20)  -0.3074(10)   1.0        Uiso   0.0051(9)     4
D D14     1.146(5)     0.2981(24)  -0.3539(12)   1.0        Uiso   0.0290(24)    4
P P22     0.5518(24)   0.5108(12)  -0.0001(8)    1.0        Uiso   0.0051(9)     4
O O21     0.7839(28)   0.6384(15)   0.0138(11)   1.0        Uiso   0.0051(9)     4
D D21     0.976(4)     0.6039(23)   0.0323(16)   1.0        Uiso   0.0290(24)    4
O O22     0.4505(34)   0.5242(21)  -0.1018(9)    1.0        Uiso   0.0051(9)     4
D D22     0.298(4)     0.4535(28)  -0.1185(14)   1.0        Uiso   0.0290(24)    4
O O23     0.6882(33)   0.3478(14)   0.0139(12)   1.0        Uiso   0.0051(9)     4
D D23     0.632(5)     0.2812(23)   0.0649(13)   1.0        Uiso   0.0290(24)    4
O O24     0.3066(31)   0.5329(18)   0.0689(10)   1.0        Uiso   0.0051(9)     4

loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11     1.55(2) . . no     
P11  O12     1.53(2) . . no     
P11  O13   1.553(18) . . no     
P11  O14   1.552(19) . . no
O11  D11     0.94(2) . . no     
O13  D13     0.97(2) . . no     
O14  D14     0.98(2) . . no
P22  O21   1.548(17) . . no     
P22  O22   1.553(17) . . no     
P22  O23   1.545(16) . . no      
P22  O24   1.528(18) . . no
O21  D21     0.98(2) . . no     
O22  D22     0.96(3) . . no     
O23  D23     0.97(2) . . no


 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  109.4(11) . . . no       
O11  P11  O13  111.7(12) . . . no       
O11  P11  O14  107.8(11) . . . no
O12  P11  O13  109.8(11) . . . no       
O12  P11  O14  110.1(12) . . . no       
O13  P11  O14  108.0(11) . . . no
P11  O11  D11     122(2) . . . no       
P11  O13  D13  116.6(17) . . . no       
P11  O14  D14  117.3(18) . . . no
O21  P22  O22  106.5(10) . . . no       
O21  P22  O23   109.6(9) . . . no       
O21  P22  O24  110.3(10) . . . no
O22  P22  O23  108.3(11) . . . no       
O22  P22  O24   112.8(9) . . . no       
O23  P22  O24  109.3(11) . . . no
P22  O21  D21  117.4(15) . . . no       
P22  O22  D22  114.7(18) . . . no       
P22  O23  D23  121.5(18) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11      -32(2) . . . . no    
O13  P11  O11  D11     -154(2) . . . . no    
O14  P11  O11  D11       88(2) . . . . no
O11  P11  O13  D13    87.7(19) . . . . no    
O12  P11  O13  D13      -34(2) . . . . no    
O14  P11  O13  D13  -153.9(17) . . . . no
O11  P11  O14  D14      148(2) . . . . no    
O12  P11  O14  D14      -93(2) . . . . no    
O13  P11  O14  D14       27(2) . . . . no
O22  P22  O21  D21     -120(2) . . . . no    
O23  P22  O21  D21       -3(2) . . . . no    
O24  P22  O21  D21      117(2) . . . . no
O21  P22  O22  D22     -177(2) . . . . no    
O23  P22  O22  D22       66(2) . . . . no    
O24  P22  O22  D22      -56(2) . . . . no
O21  P22  O23  D23      114(2) . . . . no    
O22  P22  O23  D23     -130(2) . . . . no    
O24  P22  O23  D23       -7(2) . . . . no



data_Phosphoric_acid_II_1.65_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578431'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.6332(6)
_cell_length_b      8.5169(10)
_cell_length_c      14.4323(15)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        569.51(7)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       1.65 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.356

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0447
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.31
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.0979

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.04

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------


;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8886(26)   0.2897(13)  -0.2295(8)    1.0        Uiso   0.0032(8)     4
O O11     0.675(4)     0.1586(18)  -0.2011(11)   1.0        Uiso   0.0032(8)     4
D D11     0.729(4)     0.0871(22)  -0.1558(13)   1.0        Uiso   0.0280(23)    4
O O12     1.0715(35)   0.3340(19)  -0.1452(10)   1.0        Uiso   0.0032(8)     4
O O13     0.7227(34)   0.4356(15)  -0.2665(11)   1.0        Uiso   0.0032(8)     4
D D13     0.651(4)     0.5129(25)  -0.2217(13)   1.0        Uiso   0.0280(23)    4
O O14     1.0799(33)   0.2254(19)  -0.3089(10)   1.0        Uiso   0.0032(8)     4
D D14     1.141(5)     0.3000(25)  -0.3551(12)   1.0        Uiso   0.0280(23)    4
P P22     0.5562(23)   0.5122(12)   0.0009(8)    1.0        Uiso   0.0032(8)     4
O O21     0.7846(29)   0.6428(15)   0.0149(11)   1.0        Uiso   0.0032(8)     4
D D21     0.976(4)     0.6071(24)   0.0319(16)   1.0        Uiso   0.0280(23)    4
O O22     0.4582(34)   0.5229(21)  -0.1014(9)    1.0        Uiso   0.0032(8)     4
D D22     0.296(4)     0.4570(29)  -0.1191(14)   1.0        Uiso   0.0280(23)    4
O O23     0.6961(33)   0.3489(14)   0.0136(12)   1.0        Uiso   0.0032(8)     4
D D23     0.635(5)     0.2809(23)   0.0644(13)   1.0        Uiso   0.0280(23)    4
O O24     0.3018(31)   0.5306(17)   0.0685(9)    1.0        Uiso   0.0032(8)     4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11     1.55(2) . . no     
P11  O12     1.53(2) . . no     
P11  O13   1.556(18) . . no     
P11  O14   1.548(19) . . no
O11  D11     0.93(2) . . no     
O13  D13     0.98(2) . . no     
O14  D14     0.96(2) . . no
P22  O21   1.550(17) . . no     
P22  O22   1.547(17) . . no     
P22  O23   1.546(16) . . no      
P22  O24   1.537(17) . . no
O21  D21     0.97(2) . . no     
O22  D22     0.97(3) . . no     
O23  D23     0.98(2) . . no


 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  108.8(11) . . . no       
O11  P11  O13  110.5(12) . . . no       
O11  P11  O14  107.9(11) . . . no
O12  P11  O13  110.5(11) . . . no       
O12  P11  O14  111.0(12) . . . no       
O13  P11  O14  108.1(11) . . . no
P11  O11  D11     119(2) . . . no       
P11  O13  D13  118.6(17) . . . no       
P11  O14  D14  116.5(18) . . . no
O21  P22  O22  106.4(10) . . . no       
O21  P22  O23   110.1(9) . . . no       
O21  P22  O24  111.6(10) . . . no
O22  P22  O23  106.9(11) . . . no       
O22  P22  O24   112.0(9) . . . no       
O23  P22  O24  109.8(10) . . . no
P22  O21  D21  115.7(15) . . . no       
P22  O22  D22  116.3(18) . . . no       
P22  O23  D23  120.1(18) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11      -32(2) . . . . no    
O13  P11  O11  D11     -153(2) . . . . no    
O14  P11  O11  D11       89(2) . . . . no
O11  P11  O13  D13    84.8(19) . . . . no    
O12  P11  O13  D13      -36(2) . . . . no    
O14  P11  O13  D13  -157.4(17) . . . . no
O11  P11  O14  D14      146(2) . . . . no    
O12  P11  O14  D14      -94(2) . . . . no    
O13  P11  O14  D14       27(2) . . . . no
O22  P22  O21  D21     -118(2) . . . . no    
O23  P22  O21  D21       -3(2) . . . . no    
O24  P22  O21  D21      120(2) . . . . no
O21  P22  O22  D22     -172(2) . . . . no    
O23  P22  O22  D22       70(2) . . . . no    
O24  P22  O22  D22      -50(2) . . . . no
O21  P22  O23  D23      116(2) . . . . no    
O22  P22  O23  D23     -129(2) . . . . no    
O24  P22  O23  D23       -7(2) . . . . no



data_Phosphoric_acid_II_1.97_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578432'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.6206(5)
_cell_length_b      8.4810(9)
_cell_length_c      14.3880(14)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        563.83(6)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       1.97 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.38

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0392
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.20
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1002

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.02

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8908(25)   0.2917(13)  -0.2309(7)    1.0        Uiso   0.0041(8)     4
O O11     0.6760(33)   0.1628(17)  -0.1992(11)   1.0        Uiso   0.0041(8)     4
D D11     0.731(4)     0.0836(21)  -0.1560(12)   1.0        Uiso   0.0308(22)    4
O O12     1.0736(34)   0.3397(18)  -0.1475(10)   1.0        Uiso   0.0041(8)     4
O O13     0.7189(33)   0.4352(14)  -0.2690(10)   1.0        Uiso   0.0041(8)     4
D D13     0.651(4)     0.5106(25)  -0.2240(13)   1.0        Uiso   0.0308(22)    4
O O14     1.0801(32)   0.2218(18)  -0.3099(10)   1.0        Uiso   0.0041(8)     4
D D14     1.145(5)     0.2966(24)  -0.3561(12)   1.0        Uiso   0.0308(22)    4
P P22     0.5580(22)   0.5086(12)   0.0016(8)    1.0        Uiso   0.0041(8)     4
O O21     0.7902(28)   0.6376(14)   0.0165(11)   1.0        Uiso   0.0041(8)     4
D D21     0.981(4)     0.6029(22)   0.0321(16)   1.0        Uiso   0.0308(22)    4
O O22     0.4562(31)   0.5218(20)  -0.1008(8)    1.0        Uiso   0.0041(8)     4
D D22     0.299(4)     0.4561(28)  -0.1222(13)   1.0        Uiso   0.0308(22)    4
O O23     0.6963(31)   0.3433(13)   0.0129(11)   1.0        Uiso   0.0041(8)     4
D D23     0.645(4)     0.2808(22)   0.0658(13)   1.0        Uiso   0.0308(22)    4
O O24     0.3020(30)   0.5286(17)   0.0692(9)    1.0        Uiso   0.0041(8)     4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11   1.546(18) . . no     
P11  O12   1.523(17) . . no     
P11  O13   1.554(16) . . no     
P11  O14   1.551(17) . . no
O11  D11     0.95(2) . . no     
O13  D13     0.97(2) . . no     
O14  D14     0.97(2) . . no
P22  O21   1.547(16) . . no     
P22  O22   1.551(16) . . no     
P22  O23   1.549(15) . . no      
P22  O24   1.541(17) . . no
O21  D21     0.96(2) . . no     
O22  D22     0.97(3) . . no     
O23  D23     0.96(2) . . no


 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  108.3(10) . . . no       
O11  P11  O13   109.2(9) . . . no       
O11  P11  O14  107.9(10) . . . no
O12  P11  O13  110.7(10) . . . no       
O12  P11  O14   111.5(9) . . . no       
O13  P11  O14  109.2(10) . . . no
P11  O11  D11  121.3(17) . . . no       
P11  O13  D13  116.9(16) . . . no       
P11  O14  D14  115.2(17) . . . no
O21  P22  O22  106.9(10) . . . no       
O21  P22  O23   109.9(9) . . . no       
O21  P22  O24  111.5(10) . . . no
O22  P22  O23  106.9(11) . . . no       
O22  P22  O24   111.0(9) . . . no       
O23  P22  O24  110.5(10) . . . no
P22  O21  D21  117.1(15) . . . no       
P22  O22  D22  119.2(17) . . . no       
P22  O23  D23  118.8(16) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11      -38(2) . . . . no    
O13  P11  O11  D11  -158.5(19) . . . . no    
O14  P11  O11  D11       83(2) . . . . no
O11  P11  O13  D13    84.2(19) . . . . no    
O12  P11  O13  D13      -35(2) . . . . no    
O14  P11  O13  D13  -158.0(17) . . . . no
O11  P11  O14  D14   148.8(19) . . . . no    
O12  P11  O14  D14      -93(2) . . . . no    
O13  P11  O14  D14       30(2) . . . . no
O22  P22  O21  D21     -118(2) . . . . no    
O23  P22  O21  D21       -2(2) . . . . no    
O24  P22  O21  D21      121(2) . . . . no
O21  P22  O22  D22     -175(2) . . . . no    
O23  P22  O22  D22       67(2) . . . . no    
O24  P22  O22  D22      -53(2) . . . . no
O21  P22  O23  D23   110.4(19) . . . . no    
O22  P22  O23  D23  -133.9(18) . . . . no    
O24  P22  O23  D23      -13(2) . . . . no



data_Phosphoric_acid_II_2.32_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578433'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.6022(5)
_cell_length_b      8.4597(9)
_cell_length_c      14.3291(14)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        557.88(6)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       2.32 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.405

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0405
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.20
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1086

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.03

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8955(26)   0.2904(12)  -0.2303(7)    1.0        Uiso   0.0053(8)     4
O O11     0.6834(34)   0.1592(17)  -0.1987(10)   1.0        Uiso   0.0053(8)     4
D D11     0.719(4)     0.0807(20)  -0.1540(12)   1.0        Uiso   0.0320(23)    4
O O12     1.0794(34)   0.3382(18)  -0.1469(9)    1.0        Uiso   0.0053(8)     4
O O13     0.7255(33)   0.4359(14)  -0.2681(11)   1.0        Uiso   0.0053(8)     4
D D13     0.656(4)     0.5129(24)  -0.2230(13)   1.0        Uiso   0.0320(23)    4
O O14     1.0847(32)   0.2203(18)  -0.3095(9)    1.0        Uiso   0.0053(8)     4
D D14     1.136(5)     0.2934(23)  -0.3587(12)   1.0        Uiso   0.0320(23)    4
P P22     0.5552(22)   0.5110(12)  -0.0010(8)    1.0        Uiso   0.0053(8)     4
O O21     0.7886(27)   0.6402(15)   0.0134(11)   1.0        Uiso   0.0053(8)     4
D D21     0.977(4)     0.6040(22)   0.0325(15)   1.0        Uiso   0.0320(23)    4
O O22     0.4586(31)   0.5244(20)  -0.1042(9)    1.0        Uiso   0.0053(8)     4
D D22     0.287(4)     0.4659(27)  -0.1203(13)   1.0        Uiso   0.0320(23)    4
O O23     0.6925(31)   0.3452(14)   0.0112(11)   1.0        Uiso   0.0053(8)     4
D D23     0.646(4)     0.2821(21)   0.0657(13)   1.0        Uiso   0.0320(23)    4
O O24     0.2998(29)   0.5329(16)   0.0667(9)    1.0        Uiso   0.0053(8)     4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11   1.549(18) . . no     
P11  O12   1.517(18) . . no     
P11  O13   1.556(17) . . no     
P11  O14   1.548(18) . . no
O11  D11     0.94(2) . . no     
O13  D13     0.97(2) . . no     
O14  D14     0.97(2) . . no
P22  O21   1.548(17) . . no     
P22  O22   1.547(17) . . no     
P22  O23   1.550(16) . . no      
P22  O24   1.534(17) . . no
O21  D21     0.96(2) . . no     
O22  D22     0.96(3) . . no     
O23  D23     0.97(2) . . no


 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  108.2(10) . . . no       
O11  P11  O13  110.5(11) . . . no       
O11  P11  O14  107.2(10) . . . no
O12  P11  O13  110.0(10) . . . no       
O12  P11  O14  111.6(11) . . . no       
O13  P11  O14  109.3(10) . . . no
P11  O11  D11  126.5(17) . . . no       
P11  O13  D13  117.8(17) . . . no       
P11  O14  D14  115.4(17) . . . no
O21  P22  O22  106.0(10) . . . no       
O21  P22  O23   109.8(9) . . . no       
O21  P22  O24  111.3(10) . . . no
O22  P22  O23  106.8(11) . . . no       
O22  P22  O24   112.2(9) . . . no       
O23  P22  O24  110.6(10) . . . no
P22  O21  D21  116.2(15) . . . no       
P22  O22  D22  115.4(17) . . . no       
P22  O23  D23  119.9(16) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11      -34(2) . . . . no    
O13  P11  O11  D11     -154(2) . . . . no    
O14  P11  O11  D11       87(2) . . . . no
O11  P11  O13  D13    84.0(19) . . . . no    
O12  P11  O13  D13      -35(2) . . . . no    
O14  P11  O13  D13  -158.3(17) . . . . no
O11  P11  O14  D14   144.0(19) . . . . no    
O12  P11  O14  D14      -98(2) . . . . no    
O13  P11  O14  D14       24(2) . . . . no
O22  P22  O21  D21     -120(2) . . . . no    
O23  P22  O21  D21       -5(2) . . . . no    
O24  P22  O21  D21      118(2) . . . . no
O21  P22  O22  D22     -168(2) . . . . no    
O23  P22  O22  D22       75(2) . . . . no    
O24  P22  O22  D22      -46(2) . . . . no
O21  P22  O23  D23   109.2(19) . . . . no    
O22  P22  O23  D23  -136.3(18) . . . . no    
O24  P22  O23  D23      -14(2) . . . . no



data_Phosphoric_acid_II_2.45_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578434'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.5980(6)
_cell_length_b      8.4429(10)
_cell_length_c      14.3036(16)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        555.27(7)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       2.45 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.417

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0470
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.02
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1559

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.02

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8913(27)   0.2897(13)  -0.2305(8)    1.0        Uiso   0.0047(10)    4
O O11     0.672(4)     0.1609(18)  -0.1997(12)   1.0        Uiso   0.0047(10)    4
D D11     0.727(5)     0.0842(24)  -0.1541(14)   1.0        Uiso   0.0321(26)    4
O O12     1.075(4)     0.3377(20)  -0.1469(11)   1.0        Uiso   0.0047(10)    4
O O13     0.726(4)     0.4362(16)  -0.2690(12)   1.0        Uiso   0.0047(10)    4
D D13     0.656(5)     0.5220(28)  -0.2304(16)   1.0        Uiso   0.0321(26)    4
O O14     1.083(4)     0.2177(21)  -0.3088(10)   1.0        Uiso   0.0047(10)    4
D D14     1.126(6)     0.2878(25)  -0.3593(14)   1.0        Uiso   0.0321(26)    4
P P22     0.5623(24)   0.5078(13)   0.0008(9)    1.0        Uiso   0.0047(10)    4
O O21     0.7984(31)   0.6357(16)   0.0166(13)   1.0        Uiso   0.0047(10)    4
D D21     0.993(4)     0.6105(25)   0.0348(18)   1.0        Uiso   0.0321(26)    4
O O22     0.4619(33)   0.5233(23)  -0.1022(9)    1.0        Uiso   0.0047(10)    4
D D22     0.284(4)     0.4708(32)  -0.1181(15)   1.0        Uiso   0.0321(26)    4
O O23     0.697(4)     0.3411(14)   0.0147(12)   1.0        Uiso   0.0047(10)    4
D D23     0.653(5)     0.2796(24)   0.0688(14)   1.0        Uiso   0.0321(26)    4
O O24     0.3079(32)   0.5312(18)   0.0681(10)   1.0        Uiso   0.0047(10)    4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11     1.55(2) . . no     
P11  O12     1.52(2) . . no     
P11  O13   1.552(19) . . no     
P11  O14     1.55(2) . . no
O11  D11     0.95(3) . . no     
O13  D13     0.97(3) . . no     
O14  D14     0.95(2) . . no
P22  O21   1.548(17) . . no     
P22  O22   1.549(18) . . no     
P22  O23   1.551(17) . . no      
P22  O24   1.526(18) . . no
O21  D21     0.96(2) . . no     
O22  D22     0.96(2) . . no     
O23  D23     0.95(2) . . no


 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  109.1(11) . . . no       
O11  P11  O13  110.1(12) . . . no       
O11  P11  O14  107.6(11) . . . no
O12  P11  O13  109.7(11) . . . no       
O12  P11  O14  110.9(12) . . . no       
O13  P11  O14  109.5(11) . . . no
P11  O11  D11     120(2) . . . no       
P11  O13  D13     124(2) . . . no       
P11  O14  D14  115.1(19) . . . no
O21  P22  O22  106.8(11) . . . no       
O21  P22  O23  109.5(10) . . . no       
O21  P22  O24  110.7(11) . . . no
O22  P22  O23  108.4(11) . . . no       
O22  P22  O24   111.2(9) . . . no       
O23  P22  O24  110.1(11) . . . no
P22  O21  D21  123.0(16) . . . no       
P22  O22  D22  116.3(18) . . . no       
P22  O23  D23  120.7(19) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11   -36(2) . . . . no    
O13  P11  O11  D11  -156(2) . . . . no    
O14  P11  O11  D11    85(2) . . . . no
O11  P11  O13  D13    87(3) . . . . no    
O12  P11  O13  D13   -33(3) . . . . no    
O14  P11  O13  D13  -155(2) . . . . no
O11  P11  O14  D14   140(2) . . . . no    
O12  P11  O14  D14  -101(2) . . . . no    
O13  P11  O14  D14    20(3) . . . . no
O22  P22  O21  D21  -120(3) . . . . no    
O23  P22  O21  D21    -3(3) . . . . no    
O24  P22  O21  D21   119(3) . . . . no
O21  P22  O22  D22  -165(2) . . . . no    
O23  P22  O22  D22    78(2) . . . . no    
O24  P22  O22  D22   -44(2) . . . . no
O21  P22  O23  D23   107(2) . . . . no    
O22  P22  O23  D23  -137(2) . . . . no    
O24  P22  O23  D23   -15(3) . . . . no



data_Phosphoric_acid_II_2.63_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578435'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.5932(5)
_cell_length_b      8.4323(8)
_cell_length_c      14.2795(13)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        553.06(6)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       2.63 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.426

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0400
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.23
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.0949

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.05

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8943(24)   0.2905(12)  -0.2318(7)    1.0        Uiso   0.0031(7)     4
O O11     0.6760(32)   0.1619(16)  -0.1997(10)   1.0        Uiso   0.0031(7)     4
D D11     0.721(4)     0.0819(20)  -0.1551(11)   1.0        Uiso   0.0311(22)    4
O O12     1.0850(32)   0.3357(17)  -0.1477(9)    1.0        Uiso   0.0031(7)     4
O O13     0.7274(31)   0.4377(14)  -0.2700(10)   1.0        Uiso   0.0031(7)     4
D D13     0.649(4)     0.5096(24)  -0.2244(12)   1.0        Uiso   0.0311(22)    4
O O14     1.0751(30)   0.2164(17)  -0.3124(9)    1.0        Uiso   0.0031(7)     4
D D14     1.141(5)     0.2944(22)  -0.3570(11)   1.0        Uiso   0.0311(22)    4
P P22     0.5609(22)   0.5076(12)   0.0021(7)    1.0        Uiso   0.0031(7)     4
O O21     0.7947(28)   0.6370(14)   0.0182(11)   1.0        Uiso   0.0031(7)     4
D D21     0.9873(35)   0.6055(21)   0.0356(14)   1.0        Uiso   0.0311(22)    4
O O22     0.4612(29)   0.5238(18)  -0.1012(8)    1.0        Uiso   0.0031(7)     4
D D22     0.288(4)     0.4666(26)  -0.1207(12)   1.0        Uiso   0.0311(22)    4
O O23     0.6996(29)   0.3411(13)   0.0136(10)   1.0        Uiso   0.0031(7)     4
D D23     0.642(4)     0.2785(20)   0.0677(12)   1.0        Uiso   0.0311(22)    4
O O24     0.3016(27)   0.5273(16)   0.0699(9)    1.0        Uiso   0.0031(7)     4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11   1.546(17) . . no     
P11  O12   1.535(16) . . no     
P11  O13   1.558(16) . . no     
P11  O14   1.551(17) . . no
O11  D11     0.95(2) . . no     
O13  D13     0.96(2) . . no     
O14  D14     0.96(2) . . no
P22  O21   1.549(16) . . no     
P22  O22   1.551(15) . . no     
P22  O23   1.551(15) . . no      
P22  O24   1.543(16) . . no
O21  D21     0.95(2) . . no     
O22  D22     0.97(2) . . no     
O23  D23     0.97(2) . . no


 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  108.2(10) . . . no       
O11  P11  O13   110.1(9) . . . no       
O11  P11  O14   106.5(9) . . . no
O12  P11  O13  111.0(10) . . . no       
O12  P11  O14   112.0(9) . . . no       
O13  P11  O14   109.0(9) . . . no
P11  O11  D11  123.8(17) . . . no       
P11  O13  D13  116.9(16) . . . no       
P11  O14  D14  112.7(16) . . . no
O21  P22  O22  106.5(10) . . . no       
O21  P22  O23   109.7(9) . . . no       
O21  P22  O24  111.5(10) . . . no
O22  P22  O23  107.6(10) . . . no       
O22  P22  O24   111.0(9) . . . no       
O23  P22  O24   110.4(9) . . . no
P22  O21  D21  119.2(15) . . . no       
P22  O22  D22  118.2(16) . . . no       
P22  O23  D23  117.4(16) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11      -35(2) . . . . no    
O13  P11  O11  D11  -156.5(18) . . . . no    
O14  P11  O11  D11       86(2) . . . . no
O11  P11  O13  D13    79.5(19) . . . . no    
O12  P11  O13  D13      -40(2) . . . . no    
O14  P11  O13  D13  -164.0(17) . . . . no
O11  P11  O14  D14   150.3(18) . . . . no    
O12  P11  O14  D14   -91.6(19) . . . . no    
O13  P11  O14  D14       32(2) . . . . no
O22  P22  O21  D21     -119(2) . . . . no    
O23  P22  O21  D21       -3(2) . . . . no    
O24  P22  O21  D21      120(2) . . . . no
O21  P22  O22  D22     -168(2) . . . . no    
O23  P22  O22  D22       75(2) . . . . no    
O24  P22  O22  D22      -46(2) . . . . no
O21  P22  O23  D23   110.9(18) . . . . no    
O22  P22  O23  D23  -133.7(17) . . . . no    
O24  P22  O23  D23      -12(2) . . . . no



data_Phosphoric_acid_II_2.78_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578436'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.5868(7)
_cell_length_b      8.4232(13)
_cell_length_c      14.2653(19)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        551.15(8)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       2.78 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.435

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0546
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   0.96
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1234

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.03

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8918(31)   0.2890(15)  -0.2303(8)    1.0        Uiso   0.0037(11)    4
O O11     0.670(4)     0.1612(20)  -0.1987(13)   1.0        Uiso   0.0037(11)    4
D D11     0.720(6)     0.0810(26)  -0.1542(15)   1.0        Uiso   0.0285(29)    4
O O12     1.083(4)     0.3344(23)  -0.1478(11)   1.0        Uiso   0.0037(11)    4
O O13     0.726(4)     0.4378(18)  -0.2663(13)   1.0        Uiso   0.0037(11)    4
D D13     0.656(5)     0.5184(32)  -0.2242(17)   1.0        Uiso   0.0285(29)    4
O O14     1.079(4)     0.2182(23)  -0.3105(11)   1.0        Uiso   0.0037(11)    4
D D14     1.137(6)     0.2880(28)  -0.3602(15)   1.0        Uiso   0.0285(29)    4
P P22     0.5599(26)   0.5103(14)  -0.0006(9)    1.0        Uiso   0.0037(11)    4
O O21     0.7903(34)   0.6406(18)   0.0187(15)   1.0        Uiso   0.0037(11)    4
D D21     0.987(4)     0.6087(29)   0.0319(21)   1.0        Uiso   0.0285(29)    4
O O22     0.463(4)     0.5248(25)  -0.1043(10)   1.0        Uiso   0.0037(11)    4
D D22     0.295(5)     0.466(4)    -0.1217(17)   1.0        Uiso   0.0285(29)    4
O O23     0.700(4)     0.3447(16)   0.0141(14)   1.0        Uiso   0.0037(11)    4
D D23     0.647(6)     0.2797(28)   0.0663(16)   1.0        Uiso   0.0285(29)    4
O O24     0.302(4)     0.5296(20)   0.0649(11)   1.0        Uiso   0.0037(11)    4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11     1.55(2) . . no     
P11  O12     1.52(2) . . no     
P11  O13     1.55(2) . . no     
P11  O14     1.55(2) . . no
O11  D11     0.95(3) . . no     
O13  D13     0.96(3) . . no     
O14  D14     0.96(3) . . no
P22  O21     1.55(2) . . no     
P22  O22     1.55(2) . . no     
P22  O23   1.550(19) . . no      
P22  O24     1.52(2) . . no
O21  D21     0.96(2) . . no     
O22  D22     0.95(3) . . no     
O23  D23     0.95(3) . . no


 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  109.1(12) . . . no       
O11  P11  O13  109.6(12) . . . no       
O11  P11  O14  108.1(12) . . . no
O12  P11  O13  109.8(12) . . . no       
O12  P11  O14  110.5(13) . . . no       
O13  P11  O14  109.8(12) . . . no
P11  O11  D11     122(2) . . . no       
P11  O13  D13     122(2) . . . no       
P11  O14  D14     118(2) . . . no
O21  P22  O22  108.0(13) . . . no       
O21  P22  O23  109.4(12) . . . no       
O21  P22  O24  110.2(12) . . . no
O22  P22  O23  108.7(12) . . . no       
O22  P22  O24  110.8(12) . . . no       
O23  P22  O24  109.8(12) . . . no
P22  O21  D21     119(2) . . . no       
P22  O22  D22     116(2) . . . no       
P22  O23  D23     121(2) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11   -36(3) . . . . no    
O13  P11  O11  D11  -156(2) . . . . no    
O14  P11  O11  D11    85(3) . . . . no
O11  P11  O13  D13    84(3) . . . . no    
O12  P11  O13  D13   -36(3) . . . . no    
O14  P11  O13  D13  -158(2) . . . . no
O11  P11  O14  D14   144(2) . . . . no    
O12  P11  O14  D14   -97(2) . . . . no    
O13  P11  O14  D14    24(3) . . . . no
O22  P22  O21  D21  -114(3) . . . . no    
O23  P22  O21  D21     5(3) . . . . no    
O24  P22  O21  D21   125(3) . . . . no
O21  P22  O22  D22  -168(3) . . . . no    
O23  P22  O22  D22    74(3) . . . . no    
O24  P22  O22  D22   -47(3) . . . . no
O21  P22  O23  D23   109(3) . . . . no    
O22  P22  O23  D23  -133(3) . . . . no    
O24  P22  O23  D23   -12(3) . . . . no



data_Phosphoric_acid_II_2.91_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578437'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.5831(5)
_cell_length_b      8.4110(9)
_cell_length_c      14.2424(14)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        549.02(6)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       2.91 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.444

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0399
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.20
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.0952

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.03

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8925(25)   0.2892(12)  -0.2305(7)    1.0        Uiso   0.0031(8)     4
O O11     0.6724(32)   0.1608(17)  -0.1990(10)   1.0        Uiso   0.0031(8)     4
D D11     0.726(4)     0.0819(21)  -0.1546(12)   1.0        Uiso   0.0284(21)    4
O O12     1.0763(33)   0.3384(18)  -0.1460(9)    1.0        Uiso   0.0031(8)     4
O O13     0.7252(33)   0.4364(15)  -0.2688(11)   1.0        Uiso   0.0031(8)     4
D D13     0.660(4)     0.5176(24)  -0.2251(13)   1.0        Uiso   0.0284(21)    4
O O14     1.0860(31)   0.2174(18)  -0.3091(9)    1.0        Uiso   0.0031(8)     4
D D14     1.130(5)     0.2914(23)  -0.3585(12)   1.0        Uiso   0.0284(21)    4
P P22     0.5600(23)   0.5104(12)  -0.0021(8)    1.0        Uiso   0.0031(8)     4
O O21     0.7938(28)   0.6410(14)   0.0119(11)   1.0        Uiso   0.0031(8)     4
D D21     0.981(4)     0.6092(22)   0.0339(15)   1.0        Uiso   0.0284(21)    4
O O22     0.4634(30)   0.5243(20)  -0.1059(9)    1.0        Uiso   0.0031(8)     4
D D22     0.289(4)     0.4677(27)  -0.1207(13)   1.0        Uiso   0.0284(21)    4
O O23     0.7024(32)   0.3453(14)   0.0123(11)   1.0        Uiso   0.0031(8)     4
D D23     0.649(4)     0.2810(21)   0.0669(13)   1.0        Uiso   0.0284(21)    4
O O24     0.2976(29)   0.5298(16)   0.0660(9)    1.0        Uiso   0.0031(8)     4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11   1.547(17) . . no     
P11  O12   1.524(17) . . no     
P11  O13   1.557(17) . . no     
P11  O14   1.549(17) . . no
O11  D11     0.95(2) . . no     
O13  D13     0.97(2) . . no     
O14  D14     0.96(2) . . no
P22  O21   1.548(16) . . no     
P22  O22   1.548(17) . . no     
P22  O23   1.547(16) . . no      
P22  O24   1.552(17) . . no
O21  D21     0.95(2) . . no     
O22  D22     0.95(2) . . no     
O23  D23     0.98(2) . . no


 
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  108.7(10) . . . no       
O11  P11  O13   109.5(9) . . . no       
O11  P11  O14  108.1(10) . . . no
O12  P11  O13  109.5(10) . . . no       
O12  P11  O14   111.2(9) . . . no       
O13  P11  O14  109.8(10) . . . no
P11  O11  D11  120.7(16) . . . no       
P11  O13  D13  119.2(17) . . . no       
P11  O14  D14  113.5(17) . . . no
O21  P22  O22  105.6(10) . . . no       
O21  P22  O23   109.2(9) . . . no       
O21  P22  O24  112.4(10) . . . no
O22  P22  O23  108.3(11) . . . no       
O22  P22  O24   111.5(9) . . . no       
O23  P22  O24  109.7(10) . . . no
P22  O21  D21  117.8(15) . . . no       
P22  O22  D22  114.6(17) . . . no       
P22  O23  D23  119.8(16) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11      -38(2) . . . . no    
O13  P11  O11  D11  -157.3(18) . . . . no    
O14  P11  O11  D11       83(2) . . . . no
O11  P11  O13  D13    86.1(19) . . . . no    
O12  P11  O13  D13      -33(2) . . . . no    
O14  P11  O13  D13  -155.3(17) . . . . no
O11  P11  O14  D14   141.0(18) . . . . no    
O12  P11  O14  D14   -99.7(19) . . . . no    
O13  P11  O14  D14       22(2) . . . . no
O22  P22  O21  D21     -123(2) . . . . no    
O23  P22  O21  D21       -7(2) . . . . no    
O24  P22  O21  D21      115(2) . . . . no
O21  P22  O22  D22     -166(2) . . . . no    
O23  P22  O22  D22       77(2) . . . . no    
O24  P22  O22  D22      -44(2) . . . . no
O21  P22  O23  D23   111.4(19) . . . . no    
O22  P22  O23  D23  -134.1(18) . . . . no    
O24  P22  O23  D23      -12(2) . . . . no



data_Phosphoric_acid_II_3.04_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578438'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.5791(8)
_cell_length_b      8.4031(14)
_cell_length_c      14.2214(21)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        547.22(9)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       3.04 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.452

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0578
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.00
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.156

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.02

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8876(33)   0.2908(16)  -0.2316(10)   1.0        Uiso   0.0063(13)    4
O O11     0.666(4)     0.1641(24)  -0.1977(15)   1.0        Uiso   0.0063(13)    4
D D11     0.725(6)     0.0858(31)  -0.1531(18)   1.0        Uiso   0.0347(34)    4
O O12     1.078(5)     0.3390(26)  -0.1496(13)   1.0        Uiso   0.0063(13)    4
O O13     0.726(5)     0.4389(20)  -0.2709(15)   1.0        Uiso   0.0063(13)    4
D D13     0.642(6)     0.508(4)    -0.2257(18)   1.0        Uiso   0.0347(34)    4
O O14     1.076(4)     0.2175(25)  -0.3110(13)   1.0        Uiso   0.0063(13)    4
D D14     1.124(7)     0.2940(33)  -0.3591(17)   1.0        Uiso   0.0347(34)    4
P P22     0.5631(30)   0.5112(15)   0.0001(10)   1.0        Uiso   0.0063(13)    4
O O21     0.788(4)     0.6463(20)   0.0150(16)   1.0        Uiso   0.0063(13)    4
D D21     0.973(5)     0.6021(33)   0.0332(24)   1.0        Uiso   0.0347(34)    4
O O22     0.463(4)     0.5200(29)  -0.1038(11)   1.0        Uiso   0.0063(13)    4
D D22     0.292(6)     0.462(4)    -0.1205(19)   1.0        Uiso   0.0347(34)    4
O O23     0.711(4)     0.3476(18)   0.0164(16)   1.0        Uiso   0.0063(13)    4
D D23     0.656(6)     0.2764(31)   0.0662(18)   1.0        Uiso   0.0347(34)    4
O O24     0.304(4)     0.5316(22)   0.0669(13)   1.0        Uiso   0.0063(13)    4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11   1.55(2) . . no     
P11  O12   1.51(3) . . no     
P11  O13   1.55(2) . . no     
P11  O14   1.55(2) . . no
O11  D11   0.95(3) . . no     
O13  D13   0.95(4) . . no     
O14  D14   0.96(3) . . no
P22  O21   1.55(2) . . no     
P22  O22   1.55(2) . . no     
P22  O23   1.55(2) . . no      
P22  O24   1.53(2) . . no
O21  D21   0.96(3) . . no     
O22  D22   0.95(4) . . no     
O23  D23   0.96(3) . . no



loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  108.8(14) . . . no       
O11  P11  O13  110.5(13) . . . no       
O11  P11  O14  108.7(13) . . . no
O12  P11  O13  109.8(15) . . . no       
O12  P11  O14  110.4(14) . . . no       
O13  P11  O14  108.7(13) . . . no
P11  O11  D11     120(2) . . . no       
P11  O13  D13     116(3) . . . no       
P11  O14  D14     113(2) . . . no
O21  P22  O22  107.0(14) . . . no       
O21  P22  O23  109.8(13) . . . no       
O21  P22  O24  110.4(13) . . . no
O22  P22  O23  108.3(15) . . . no       
O22  P22  O24  111.0(13) . . . no       
O23  P22  O24  110.3(13) . . . no
P22  O21  D21     110(2) . . . no       
P22  O22  D22     117(2) . . . no       
P22  O23  D23     123(2) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11   -37(3) . . . . no    
O13  P11  O11  D11  -158(3) . . . . no    
O14  P11  O11  D11    83(3) . . . . no
O11  P11  O13  D13    76(3) . . . . no    
O12  P11  O13  D13   -45(3) . . . . no    
O14  P11  O13  D13  -165(3) . . . . no
O11  P11  O14  D14   144(2) . . . . no    
O12  P11  O14  D14   -97(3) . . . . no    
O13  P11  O14  D14    23(3) . . . . no
O22  P22  O21  D21  -119(3) . . . . no    
O23  P22  O21  D21    -2(3) . . . . no    
O24  P22  O21  D21   120(3) . . . . no
O21  P22  O22  D22  -166(3) . . . . no    
O23  P22  O22  D22    76(3) . . . . no    
O24  P22  O22  D22   -45(3) . . . . no
O21  P22  O23  D23   116(3) . . . . no    
O22  P22  O23  D23  -127(3) . . . . no    
O24  P22  O23  D23    -6(3) . . . . no



data_Phosphoric_acid_II_3.42_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578439'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.5689(7)
_cell_length_b      8.3733(12)
_cell_length_c      14.1755(18)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        542.32(8)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       3.42 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.474

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0503
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.07
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1236

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.02

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8833(28)   0.2857(14)  -0.2325(8)    1.0        Uiso   0.0031(10)    4
O O11     0.661(4)     0.1572(19)  -0.2001(12)   1.0        Uiso   0.0031(10)    4
D D11     0.720(6)     0.0849(27)  -0.1521(16)   1.0        Uiso   0.0358(31)    4
O O12     1.072(4)     0.3357(21)  -0.1497(11)   1.0        Uiso   0.0031(10)    4
O O13     0.717(4)     0.4330(17)  -0.2721(13)   1.0        Uiso   0.0031(10)    4
D D13     0.662(5)     0.5138(31)  -0.2277(17)   1.0        Uiso   0.0358(31)    4
O O14     1.073(4)     0.2111(22)  -0.3116(11)   1.0        Uiso   0.0031(10)    4
D D14     1.133(6)     0.2913(29)  -0.3557(16)   1.0        Uiso   0.0358(31)    4
P P22     0.5613(26)   0.5093(13)   0.0006(9)    1.0        Uiso   0.0031(10)    4
O O21     0.7902(34)   0.6430(17)   0.0170(14)   1.0        Uiso   0.0031(10)    4
D D21     0.984(4)     0.6094(29)   0.0347(20)   1.0        Uiso   0.0358(31)    4
O O22     0.4598(35)   0.5238(24)  -0.1033(9)    1.0        Uiso   0.0031(10)    4
D D22     0.285(5)     0.466(4)    -0.1187(17)   1.0        Uiso   0.0358(31)    4
O O23     0.707(4)     0.3436(15)   0.0142(13)   1.0        Uiso   0.0031(10)    4
D D23     0.639(5)     0.2777(27)   0.0658(16)   1.0        Uiso   0.0358(31)    4
O O24     0.3018(33)   0.5272(19)   0.0667(11)   1.0        Uiso   0.0031(10)    4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11     1.55(2) . . no     
P11  O12     1.52(2) . . no     
P11  O13     1.55(2) . . no     
P11  O14     1.55(2) . . no
O11  D11     0.95(3) . . no     
O13  D13     0.96(3) . . no     
O14  D14     0.96(3) . . no
P22  O21   1.550(19) . . no     
P22  O22   1.548(19) . . no     
P22  O23   1.552(18) . . no      
P22  O24     1.52(2) . . no
O21  D21     0.97(2) . . no     
O22  D22     0.96(3) . . no     
O23  D23     0.97(3) . . no



loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  109.7(11) . . . no       
O11  P11  O13  109.8(12) . . . no       
O11  P11  O14  107.5(11) . . . no
O12  P11  O13  109.7(11) . . . no       
O12  P11  O14  110.7(12) . . . no       
O13  P11  O14  109.4(11) . . . no
P11  O11  D11     118(2) . . . no       
P11  O13  D13     117(2) . . . no       
P11  O14  D14     111(2) . . . no
O21  P22  O22  106.7(12) . . . no       
O21  P22  O23  109.7(12) . . . no       
O21  P22  O24  111.3(11) . . . no
O22  P22  O23  108.5(12) . . . no       
O22  P22  O24  110.3(12) . . . no       
O23  P22  O24  110.3(12) . . . no
P22  O21  D21  116.5(19) . . . no       
P22  O22  D22     115(2) . . . no       
P22  O23  D23     118(2) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11   -33(3) . . . . no    
O13  P11  O11  D11  -154(2) . . . . no    
O14  P11  O11  D11    87(2) . . . . no
O11  P11  O13  D13    88(2) . . . . no    
O12  P11  O13  D13   -33(3) . . . . no    
O14  P11  O13  D13  -154(2) . . . . no
O11  P11  O14  D14   149(2) . . . . no    
O12  P11  O14  D14   -92(2) . . . . no    
O13  P11  O14  D14    29(3) . . . . no
O22  P22  O21  D21  -119(3) . . . . no    
O23  P22  O21  D21    -2(3) . . . . no    
O24  P22  O21  D21   120(3) . . . . no
O21  P22  O22  D22  -165(2) . . . . no    
O23  P22  O22  D22    77(3) . . . . no    
O24  P22  O22  D22   -45(3) . . . . no
O21  P22  O23  D23   115(2) . . . . no    
O22  P22  O23  D23  -128(2) . . . . no    
O24  P22  O23  D23    -8(3) . . . . no



data_Phosphoric_acid_II_3.60_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578440'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.5639(6)
_cell_length_b      8.3606(10)
_cell_length_c      14.1535(15)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        540.05(7)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       3.60 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.485

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0401
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.20
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1029

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.02

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8863(25)   0.2900(13)  -0.2314(8)    1.0        Uiso   0.0021(8)     4
O O11     0.6640(32)   0.1609(17)  -0.2001(11)   1.0        Uiso   0.0021(8)     4
D D11     0.716(5)     0.0828(22)  -0.1533(14)   1.0        Uiso   0.0318(24)    4
O O12     1.0749(32)   0.3400(18)  -0.1471(10)   1.0        Uiso   0.0021(8)     4
O O13     0.7231(32)   0.4372(15)  -0.2726(11)   1.0        Uiso   0.0021(8)     4
D D13     0.647(4)     0.5090(27)  -0.2272(14)   1.0        Uiso   0.0318(24)    4
O O14     1.0761(31)   0.2155(19)  -0.3107(10)   1.0        Uiso   0.0021(8)     4
D D14     1.134(5)     0.2920(25)  -0.3582(13)   1.0        Uiso   0.0318(24)    4
P P22     0.5636(24)   0.5104(12)  -0.0015(8)    1.0        Uiso   0.0021(8)     4
O O21     0.8016(31)   0.6395(15)   0.0147(12)   1.0        Uiso   0.0021(8)     4
D D21     0.996(4)     0.6085(23)   0.0372(16)   1.0        Uiso   0.0318(24)    4
O O22     0.4606(31)   0.5289(19)  -0.1052(9)    1.0        Uiso   0.0021(8)     4
D D22     0.285(4)     0.4706(29)  -0.1209(14)   1.0        Uiso   0.0318(24)    4
O O23     0.7069(33)   0.3436(14)   0.0114(11)   1.0        Uiso   0.0021(8)     4
D D23     0.640(4)     0.2793(23)   0.0652(14)   1.0        Uiso   0.0318(24)    4
O O24     0.2993(30)   0.5279(16)   0.0659(9)    1.0        Uiso   0.0021(8)     4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11   1.545(17) . . no     
P11  O12   1.531(18) . . no     
P11  O13   1.552(17) . . no     
P11  O14   1.549(18) . . no
O11  D11     0.96(2) . . no     
O13  D13     0.95(3) . . no     
O14  D14     0.97(2) . . no
P22  O21   1.548(16) . . no     
P22  O22   1.549(17) . . no     
P22  O23   1.551(16) . . no      
P22  O24   1.547(17) . . no
O21  D21     0.98(2) . . no     
O22  D22     0.96(2) . . no     
O23  D23     0.98(2) . . no



loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  109.7(10) . . . no       
O11  P11  O13   110.3(9) . . . no       
O11  P11  O14  107.1(10) . . . no
O12  P11  O13  110.3(10) . . . no       
O12  P11  O14   111.1(9) . . . no       
O13  P11  O14  108.4(10) . . . no
P11  O11  D11  120.7(18) . . . no       
P11  O13  D13  115.1(19) . . . no       
P11  O14  D14  113.1(17) . . . no
O21  P22  O22  106.5(10) . . . no       
O21  P22  O23   108.3(9) . . . no       
O21  P22  O24  113.0(10) . . . no
O22  P22  O23  109.2(10) . . . no       
O22  P22  O24   109.7(9) . . . no       
O23  P22  O24  110.0(10) . . . no
P22  O21  D21  120.2(15) . . . no       
P22  O22  D22  114.9(17) . . . no       
P22  O23  D23  117.1(16) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11      -35(2) . . . . no    
O13  P11  O11  D11  -156.5(19) . . . . no    
O14  P11  O11  D11       86(2) . . . . no
O11  P11  O13  D13       81(2) . . . . no    
O12  P11  O13  D13      -41(2) . . . . no    
O14  P11  O13  D13  -162.5(18) . . . . no
O11  P11  O14  D14   145.8(18) . . . . no    
O12  P11  O14  D14      -95(2) . . . . no    
O13  P11  O14  D14       27(2) . . . . no
O22  P22  O21  D21     -124(2) . . . . no    
O23  P22  O21  D21       -7(2) . . . . no    
O24  P22  O21  D21      115(2) . . . . no
O21  P22  O22  D22     -168(2) . . . . no    
O23  P22  O22  D22       76(2) . . . . no    
O24  P22  O22  D22      -45(2) . . . . no
O21  P22  O23  D23   114.0(18) . . . . no    
O22  P22  O23  D23  -130.4(18) . . . . no    
O24  P22  O23  D23      -10(2) . . . . no



data_Phosphoric_acid_II_3.74_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578441'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.5599(9)
_cell_length_b      8.3496(15)
_cell_length_c      14.1332(23)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        538.10(10)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       3.74 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.494

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0597
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.01
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor          0.1292

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.03

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8845(31)   0.2873(16)  -0.2335(9)    1.0        Uiso   0.0025(12)    4
O O11     0.667(4)     0.1562(22)  -0.2008(14)   1.0        Uiso   0.0025(12)    4
D D11     0.699(8)     0.0829(35)  -0.1498(19)   1.0        Uiso   0.050(4)      4
O O12     1.072(4)     0.3399(25)  -0.1507(12)   1.0        Uiso   0.0025(12)    4
O O13     0.715(4)     0.4340(19)  -0.2727(15)   1.0        Uiso   0.0025(12)    4
D D13     0.642(6)     0.507(4)    -0.2268(21)   1.0        Uiso   0.050(4)      4
O O14     1.078(4)     0.2158(25)  -0.3131(12)   1.0        Uiso   0.0025(12)    4
D D14     1.124(8)     0.295(4)    -0.3601(20)   1.0        Uiso   0.050(4)      4
P P22     0.5639(30)   0.5081(15)   0.0000(10)   1.0        Uiso   0.0025(12)    4
O O21     0.791(4)     0.6417(20)   0.0200(16)   1.0        Uiso   0.0025(12)    4
D D21     0.985(5)     0.606(4)     0.0347(30)   1.0        Uiso   0.050(4)      4
O O22     0.459(4)     0.5244(27)  -0.1038(11)   1.0        Uiso   0.0025(12)    4
D D22     0.281(6)     0.472(5)    -0.1208(21)   1.0        Uiso   0.050(4)      4
O O23     0.712(4)     0.3426(18)   0.0130(15)   1.0        Uiso   0.0025(12)    4
D D23     0.661(7)     0.278(4)     0.0663(19)   1.0        Uiso   0.050(4)      4
O O24     0.304(4)     0.5229(22)   0.0672(12)   1.0        Uiso   0.0025(12)    4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11   1.55(2) . . no     
P11  O12   1.51(2) . . no     
P11  O13   1.55(2) . . no     
P11  O14   1.55(2) . . no
O11  D11   0.96(4) . . no     
O13  D13   0.95(4) . . no     
O14  D14   0.96(4) . . no
P22  O21   1.55(2) . . no     
P22  O22   1.55(2) . . no     
P22  O23   1.55(2) . . no      
P22  O24   1.52(2) . . no
O21  D21   0.96(3) . . no     
O22  D22   0.95(4) . . no     
O23  D23   0.96(3) . . no



loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  109.7(12) . . . no       
O11  P11  O13  110.1(12) . . . no       
O11  P11  O14  108.0(12) . . . no
O12  P11  O13  109.2(12) . . . no       
O12  P11  O14  110.7(13) . . . no       
O13  P11  O14  109.2(13) . . . no
P11  O11  D11     125(3) . . . no       
P11  O13  D13     116(3) . . . no       
P11  O14  D14     111(2) . . . no
O21  P22  O22  108.5(14) . . . no       
O21  P22  O23  109.3(12) . . . no       
O21  P22  O24  110.3(13) . . . no
O22  P22  O23  108.9(14) . . . no       
O22  P22  O24  110.0(13) . . . no       
O23  P22  O24  109.8(13) . . . no
P22  O21  D21     116(2) . . . no       
P22  O22  D22     118(2) . . . no       
P22  O23  D23     119(3) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11   -28(3) . . . . no    
O13  P11  O11  D11  -148(3) . . . . no    
O14  P11  O11  D11    93(3) . . . . no
O11  P11  O13  D13    82(3) . . . . no    
O12  P11  O13  D13   -39(3) . . . . no    
O14  P11  O13  D13  -160(2) . . . . no
O11  P11  O14  D14   145(3) . . . . no    
O12  P11  O14  D14   -96(3) . . . . no    
O13  P11  O14  D14    25(3) . . . . no
O22  P22  O21  D21  -117(3) . . . . no    
O23  P22  O21  D21     2(4) . . . . no    
O24  P22  O21  D21   123(3) . . . . no
O21  P22  O22  D22  -162(3) . . . . no    
O23  P22  O22  D22    79(3) . . . . no    
O24  P22  O22  D22   -41(4) . . . . no
O21  P22  O23  D23   109(3) . . . . no    
O22  P22  O23  D23  -133(3) . . . . no    
O24  P22  O23  D23   -12(3) . . . . no



data_Phosphoric_acid_II_3.96_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578442'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.5549(7)
_cell_length_b      8.3362(12)
_cell_length_c      14.1067(18)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        535.64(8)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       3.96 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.505

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0476
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.14
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.1104

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.01

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8824(28)   0.2885(14)  -0.2306(8)    1.0        Uiso   0.0025(10)    4
O O11     0.659(4)     0.1592(19)  -0.1991(12)   1.0        Uiso   0.0025(10)    4
D D11     0.712(6)     0.0854(26)  -0.1505(15)   1.0        Uiso   0.0308(27)    4
O O12     1.072(4)     0.3387(20)  -0.1478(11)   1.0        Uiso   0.0025(10)    4
O O13     0.717(4)     0.4371(17)  -0.2698(13)   1.0        Uiso   0.0025(10)    4
D D13     0.653(5)     0.5207(31)  -0.2291(16)   1.0        Uiso   0.0308(27)    4
O O14     1.076(4)     0.2150(22)  -0.3097(10)   1.0        Uiso   0.0025(10)    4
D D14     1.136(6)     0.2835(28)  -0.3609(14)   1.0        Uiso   0.0308(27)    4
P P22     0.5599(26)   0.5115(13)  -0.0020(9)    1.0        Uiso   0.0025(10)    4
O O21     0.7951(34)   0.6420(17)   0.0166(13)   1.0        Uiso   0.0025(10)    4
D D21     0.991(4)     0.6085(26)   0.0305(20)   1.0        Uiso   0.0308(27)    4
O O22     0.4598(35)   0.5290(22)  -0.1064(10)   1.0        Uiso   0.0025(10)    4
D D22     0.286(5)     0.4695(34)  -0.1212(16)   1.0        Uiso   0.0308(27)    4
O O23     0.704(4)     0.3445(15)   0.0111(13)   1.0        Uiso   0.0025(10)    4
D D23     0.650(5)     0.2827(26)   0.0674(16)   1.0        Uiso   0.0308(27)    4
O O24     0.2972(33)   0.5293(18)   0.0642(11)   1.0        Uiso   0.0025(10)    4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11     1.55(2) . . no     
P11  O12     1.51(2) . . no     
P11  O13     1.55(2) . . no     
P11  O14     1.55(2) . . no
O11  D11     0.95(3) . . no     
O13  D13     0.95(3) . . no     
O14  D14     0.96(3) . . no
P22  O21   1.549(19) . . no     
P22  O22   1.549(19) . . no     
P22  O23   1.550(18) . . no      
P22  O24     1.53(2) . . no
O21  D21     0.96(2) . . no     
O22  D22     0.96(3) . . no     
O23  D23     0.98(3) . . no



loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  110.4(11) . . . no       
O11  P11  O13  109.9(12) . . . no       
O11  P11  O14  107.8(11) . . . no
O12  P11  O13  109.3(11) . . . no       
O12  P11  O14  109.9(12) . . . no       
O13  P11  O14  109.6(11) . . . no
P11  O11  D11     120(2) . . . no       
P11  O13  D13     121(2) . . . no       
P11  O14  D14     118(2) . . . no
O21  P22  O22  107.4(12) . . . no       
O21  P22  O23  108.6(12) . . . no       
O21  P22  O24  111.8(11) . . . no
O22  P22  O23  108.8(12) . . . no       
O22  P22  O24  110.0(12) . . . no       
O23  P22  O24  110.3(11) . . . no
P22  O21  D21     119(2) . . . no       
P22  O22  D22  113.8(19) . . . no       
P22  O23  D23     118(2) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11   -32(3) . . . . no    
O13  P11  O11  D11  -153(2) . . . . no    
O14  P11  O11  D11    88(2) . . . . no
O11  P11  O13  D13    87(3) . . . . no    
O12  P11  O13  D13   -34(3) . . . . no    
O14  P11  O13  D13  -155(2) . . . . no
O11  P11  O14  D14   143(2) . . . . no    
O12  P11  O14  D14   -96(2) . . . . no    
O13  P11  O14  D14    24(3) . . . . no
O22  P22  O21  D21  -116(3) . . . . no    
O23  P22  O21  D21     2(3) . . . . no    
O24  P22  O21  D21   124(3) . . . . no
O21  P22  O22  D22  -167(2) . . . . no    
O23  P22  O22  D22    76(2) . . . . no    
O24  P22  O22  D22   -45(2) . . . . no
O21  P22  O23  D23   108(2) . . . . no    
O22  P22  O23  D23  -136(2) . . . . no    
O24  P22  O23  D23   -15(3) . . . . no



data_Phosphoric_acid_II_4.36_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578443'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.5456(7)
_cell_length_b      8.3104(13)
_cell_length_c      14.0631(19)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        531.25(8)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       4.36 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.526

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0462
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.17
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.106

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.02

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8832(28)   0.2869(15)  -0.2313(8)    1.0        Uiso   0.0027(10)    4
O O11     0.658(4)     0.1597(20)  -0.1975(13)   1.0        Uiso   0.0027(10)    4
D D11     0.701(7)     0.0801(26)  -0.1505(16)   1.0        Uiso   0.0338(29)    4
O O12     1.074(4)     0.3402(22)  -0.1490(11)   1.0        Uiso   0.0027(10)    4
O O13     0.720(4)     0.4341(18)  -0.2737(13)   1.0        Uiso   0.0027(10)    4
D D13     0.659(5)     0.5165(32)  -0.2313(17)   1.0        Uiso   0.0338(29)    4
O O14     1.074(4)     0.2082(22)  -0.3098(11)   1.0        Uiso   0.0027(10)    4
D D14     1.136(7)     0.2859(31)  -0.3566(16)   1.0        Uiso   0.0338(29)    4
P P22     0.5658(27)   0.5124(13)  -0.0019(9)    1.0        Uiso   0.0027(10)    4
O O21     0.798(4)     0.6451(17)   0.0158(14)   1.0        Uiso   0.0027(10)    4
D D21     0.990(4)     0.6075(28)   0.0363(20)   1.0        Uiso   0.0338(29)    4
O O22     0.464(4)     0.5281(24)  -0.1068(10)   1.0        Uiso   0.0027(10)    4
D D22     0.293(5)     0.464(4)    -0.1196(17)   1.0        Uiso   0.0338(29)    4
O O23     0.716(4)     0.3470(16)   0.0140(14)   1.0        Uiso   0.0027(10)    4
D D23     0.640(5)     0.2843(29)   0.0666(17)   1.0        Uiso   0.0338(29)    4
O O24     0.2997(34)   0.5287(19)   0.0637(11)   1.0        Uiso   0.0027(10)    4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11     1.54(2) . . no     
P11  O12     1.51(2) . . no     
P11  O13     1.55(2) . . no     
P11  O14     1.55(2) . . no
O11  D11     0.96(3) . . no     
O13  D13     0.95(3) . . no     
O14  D14     0.97(3) . . no
P22  O21     1.55(2) . . no     
P22  O22   1.552(19) . . no     
P22  O23   1.551(19) . . no      
P22  O24     1.53(2) . . no
O21  D21     0.97(3) . . no     
O22  D22     0.96(3) . . no     
O23  D23     0.97(3) . . no



loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  110.1(12) . . . no       
O11  P11  O13  109.9(12) . . . no       
O11  P11  O14  107.5(12) . . . no
O12  P11  O13  109.8(12) . . . no       
O12  P11  O14  110.3(12) . . . no       
O13  P11  O14  109.1(11) . . . no
P11  O11  D11     124(2) . . . no       
P11  O13  D13     118(2) . . . no       
P11  O14  D14     111(2) . . . no
O21  P22  O22  107.3(12) . . . no       
O21  P22  O23  108.0(12) . . . no       
O21  P22  O24  112.3(12) . . . no
O22  P22  O23  110.0(12) . . . no       
O22  P22  O24  109.3(12) . . . no       
O23  P22  O24  109.9(12) . . . no
P22  O21  D21  115.8(19) . . . no       
P22  O22  D22     112(2) . . . no       
P22  O23  D23     116(2) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11   -36(3) . . . . no    
O13  P11  O11  D11  -157(2) . . . . no    
O14  P11  O11  D11    84(3) . . . . no
O11  P11  O13  D13    86(2) . . . . no    
O12  P11  O13  D13   -35(3) . . . . no    
O14  P11  O13  D13  -156(2) . . . . no
O11  P11  O14  D14   148(2) . . . . no    
O12  P11  O14  D14   -92(2) . . . . no    
O13  P11  O14  D14    29(3) . . . . no
O22  P22  O21  D21  -121(3) . . . . no    
O23  P22  O21  D21    -3(3) . . . . no    
O24  P22  O21  D21   119(2) . . . . no
O21  P22  O22  D22  -169(2) . . . . no    
O23  P22  O22  D22    74(3) . . . . no    
O24  P22  O22  D22   -47(3) . . . . no
O21  P22  O23  D23   116(2) . . . . no    
O22  P22  O23  D23  -128(2) . . . . no    
O24  P22  O23  D23    -7(3) . . . . no



data_Phosphoric_acid_II_5.02_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578444'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a       4.5338(7)
_cell_length_b       8.2726(12)
_cell_length_c       13.9867(18)
_cell_angle_alpha    90.0
_cell_angle_beta     90.0
_cell_angle_gamma    90.0
_cell_volume         524.58(8)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       5.02 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.558

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0391
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.27
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor          0.0868

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.04

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8796(27)   0.2867(14)  -0.2328(8)    1.0        Uiso   0.0015(9)     4
O O11     0.6546(34)   0.1579(19)  -0.1992(11)   1.0        Uiso   0.0015(9)     4
D D11     0.702(6)     0.0904(27)  -0.1476(15)   1.0        Uiso   0.0345(27)    4
O O12     1.0694(35)   0.3382(20)  -0.1492(11)   1.0        Uiso   0.0015(9)     4
O O13     0.717(4)     0.4371(17)  -0.2730(13)   1.0        Uiso   0.0015(9)     4
D D13     0.649(5)     0.5182(32)  -0.2313(17)   1.0        Uiso   0.0345(27)    4
O O14     1.068(4)     0.2086(21)  -0.3127(11)   1.0        Uiso   0.0015(9)     4
D D14     1.134(6)     0.2886(29)  -0.3583(15)   1.0        Uiso   0.0345(27)    4
P P22     0.5675(26)   0.5128(13)  -0.0009(9)    1.0        Uiso   0.0015(9)     4
O O21     0.8041(35)   0.6450(17)   0.0146(13)   1.0        Uiso   0.0015(9)     4
D D21     1.001(4)     0.6117(26)   0.0331(18)   1.0        Uiso   0.0345(27)    4
O O22     0.4617(34)   0.5331(21)  -0.1055(9)    1.0        Uiso   0.0015(9)     4
D D22     0.289(5)     0.4708(34)  -0.1207(16)   1.0        Uiso   0.0345(27)    4
O O23     0.717(4)     0.3453(15)   0.0116(13)   1.0        Uiso   0.0015(9)     4
D D23     0.651(5)     0.2807(27)   0.0668(16)   1.0        Uiso   0.0345(27)    4
O O24     0.3025(32)   0.5285(18)   0.0664(10)   1.0        Uiso   0.0015(9)     4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11   1.548(19) . . no     
P11  O12     1.51(2) . . no     
P11  O13     1.55(2) . . no     
P11  O14     1.55(2) . . no
O11  D11     0.94(3) . . no     
O13  D13     0.94(3) . . no     
O14  D14     0.97(3) . . no
P22  O21     1.55(2) . . no     
P22  O22   1.549(18) . . no     
P22  O23   1.551(18) . . no      
P22  O24   1.532(19) . . no
O21  D21     0.97(3) . . no     
O22  D22     0.96(3) . . no     
O23  D23     0.98(3) . . no



loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12  109.4(11) . . . no       
O11  P11  O13  110.4(12) . . . no       
O11  P11  O14  107.3(11) . . . no
O12  P11  O13  109.0(11) . . . no       
O12  P11  O14  111.3(12) . . . no       
O13  P11  O14  109.5(11) . . . no
P11  O11  D11     120(2) . . . no       
P11  O13  D13     120(2) . . . no       
P11  O14  D14     111(2) . . . no
O21  P22  O22  105.7(11) . . . no       
O21  P22  O23  108.4(12) . . . no       
O21  P22  O24  113.4(11) . . . no
O22  P22  O23  109.8(11) . . . no       
O22  P22  O24  109.1(11) . . . no       
O23  P22  O24  110.4(11) . . . no
P22  O21  D21  118.4(19) . . . no       
P22  O22  D22  113.9(18) . . . no       
P22  O23  D23     116(2) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11   -29(3) . . . . no    
O13  P11  O11  D11  -148(2) . . . . no    
O14  P11  O11  D11    92(2) . . . . no
O11  P11  O13  D13    84(2) . . . . no    
O12  P11  O13  D13   -37(3) . . . . no    
O14  P11  O13  D13  -159(2) . . . . no
O11  P11  O14  D14   150(2) . . . . no    
O12  P11  O14  D14   -91(2) . . . . no    
O13  P11  O14  D14    30(2) . . . . no
O22  P22  O21  D21  -121(2) . . . . no    
O23  P22  O21  D21    -4(3) . . . . no    
O24  P22  O21  D21   119(2) . . . . no
O21  P22  O22  D22  -169(2) . . . . no    
O23  P22  O22  D22    74(2) . . . . no    
O24  P22  O22  D22   -47(2) . . . . no
O21  P22  O23  D23   114(2) . . . . no    
O22  P22  O23  D23  -131(2) . . . . no    
O24  P22  O23  D23   -11(2) . . . . no



data_Phosphoric_acid_II_5.66_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578445'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.5214(6)
_cell_length_b      8.2332(11)
_cell_length_c      13.9189(16)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        518.14(7)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       5.66 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.59

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.0407
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.09
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.0562

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.04

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8764(24)   0.2867(13)  -0.2339(7)    1.0        Uiso   0.0013(8)     4
O O11     0.6523(30)   0.1565(17)  -0.2001(10)   1.0        Uiso   0.0013(8)     4
D D11     0.719(5)     0.0876(21)  -0.1497(13)   1.0        Uiso   0.0183(17)    4
O O12     1.0629(30)   0.3366(18)  -0.1490(9)    1.0        Uiso   0.0013(8)     4
O O13     0.7173(33)   0.4374(15)  -0.2767(11)   1.0        Uiso   0.0013(8)     4
D D13     0.6509(34)   0.5188(24)  -0.2371(13)   1.0        Uiso   0.0183(17)    4
O O14     1.0676(31)   0.2041(19)  -0.3120(9)    1.0        Uiso   0.0013(8)     4
D D14     1.137(5)     0.2845(23)  -0.3579(11)   1.0        Uiso   0.0183(17)    4
P P22     0.5680(21)   0.5171(11)  -0.0003(7)    1.0        Uiso   0.0013(8)     4
O O21     0.8035(29)   0.6502(15)   0.0173(11)   1.0        Uiso   0.0013(8)     4
D D21     1.0030(33)   0.6162(21)   0.0323(14)   1.0        Uiso   0.0183(17)    4
O O22     0.4643(30)   0.5359(18)  -0.1059(8)    1.0        Uiso   0.0013(8)     4
D D22     0.294(4)     0.4703(25)  -0.1217(12)   1.0        Uiso   0.0183(17)    4
O O23     0.7133(31)   0.3474(13)   0.0122(11)   1.0        Uiso   0.0013(8)     4
D D23     0.641(4)     0.2807(21)   0.0653(13)   1.0        Uiso   0.0183(17)    4
O O24     0.3036(27)   0.5330(16)   0.0655(9)    1.0        Uiso   0.0013(8)     4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11   1.548(17) . . no     
P11  O12   1.510(16) . . no     
P11  O13   1.553(17) . . no     
P11  O14   1.549(17) . . no
O11  D11     0.95(2) . . no     
O13  D13     0.92(2) . . no     
O14  D14     0.97(2) . . no
P22  O21   1.549(16) . . no     
P22  O22   1.551(15) . . no     
P22  O23   1.553(15) . . no      
P22  O24   1.510(16) . . no
O21  D21     0.97(2) . . no     
O22  D22     0.97(2) . . no     
O23  D23     0.98(2) . . no



loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12   108.5(9) . . . no       
O11  P11  O13   111.5(9) . . . no       
O11  P11  O14  106.0(10) . . . no
O12  P11  O13  110.0(10) . . . no       
O12  P11  O14   110.8(9) . . . no       
O13  P11  O14  110.0(10) . . . no
P11  O11  D11  115.3(17) . . . no       
P11  O13  D13  120.3(17) . . . no       
P11  O14  D14  109.9(17) . . . no
O21  P22  O22   106.8(9) . . . no       
O21  P22  O23   109.1(9) . . . no       
O21  P22  O24   112.8(9) . . . no
O22  P22  O23  108.9(10) . . . no       
O22  P22  O24   109.1(9) . . . no       
O23  P22  O24   110.1(9) . . . no
P22  O21  D21  118.0(15) . . . no       
P22  O22  D22  113.6(15) . . . no       
P22  O23  D23  116.6(16) . . . no 

 
 
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11      -32(2) . . . . no    
O13  P11  O11  D11  -152.9(17) . . . . no    
O14  P11  O11  D11    87.4(18) . . . . no
O11  P11  O13  D13    84.7(18) . . . . no    
O12  P11  O13  D13   -35.7(19) . . . . no    
O14  P11  O13  D13  -158.0(16) . . . . no
O11  P11  O14  D14   150.7(17) . . . . no    
O12  P11  O14  D14   -91.8(18) . . . . no    
O13  P11  O14  D14    30.0(19) . . . . no
O22  P22  O21  D21  -116.8(19) . . . . no    
O23  P22  O21  D21        1(2) . . . . no    
O24  P22  O21  D21   123.5(19) . . . . no
O21  P22  O22  D22  -170.7(16) . . . . no    
O23  P22  O22  D22    71.6(18) . . . . no    
O24  P22  O22  D22   -48.6(19) . . . . no
O21  P22  O23  D23   115.2(18) . . . . no    
O22  P22  O23  D23  -128.6(17) . . . . no    
O24  P22  O23  D23       -9(2) . . . . no



data_Phosphoric_acid_II_6.26_GPa
_database_code_depnum_ccdc_archive 'CCDC 1578446'

loop_
_publ_author_name
'Bull, Craig'
'Funnell, Nicholas'
'Pulham, Colin'
'Marshall, William'
'Allan, David'

_publ_contact_author_name        'Allan, David'
_publ_contact_author_email       david.allan@diamond.ac.uk

_publ_section_title              
;
A new high-pressure polymorph of phosphoric acid
;

_chemical_name_systematic        
;
Phosphoric acid
;
_chemical_name_common            'Phosphoric acid'
_chemical_melting_point          '315.5 K'
_chemical_formula_moiety         'D3 O4 P'

_chemical_formula_structural     ?
_chemical_formula_sum            'D3 O4 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         101.01
_chemical_compound_source        'Sigma Aldrich'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
 _symmetry_equiv_pos_as_xyz
  'x, y, z '
  'x+1/2, -y+1/2, -z '
  '-x, y+1/2, -z+1/2 '
  '-x+1/2, -y, z+1/2 '

_cell_length_a      4.5121(7)
_cell_length_b      8.2009(12)
_cell_length_c      13.8569(17)
_cell_angle_alpha   90.0
_cell_angle_beta    90.0
_cell_angle_gamma   90.0
_cell_volume        512.75(7)
_cell_formula_units_Z            8

_cell_measurement_temperature    295
_cell_measurement_pressure       6.26 #GPa

_cell_special_details            
;
Cell parameters included in refinement
;

_exptl_crystal_density_diffrn    2.617

_pd_spec_mounting                'TiZr Capsule'
_pd_spec_mount_mode              transmission
_pd_char_colour                  'white'
_chemical_absolute_configuration .

_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
Calculated using custom ISIS routines.
;

_pd_instr_location               'ISIS Neutron Facility, Rutherford Appleton Laboratory'
_diffrn_ambient_temperature      295
_diffrn_source                   'Pulsed neutron source'
_diffrn_source_target            'W'
_diffrn_radiation_type           Neutron
_diffrn_measurement_device_type  'PEARL diffractometer'
_diffrn_radiation_monochromator  'none'
_diffrn_detector                 'ZnS scintillator'
_diffrn_detector_type            custom

_pd_meas_scan_method             Time-of-flight
_pd_meas_special_details         
;
Time of flight method using a pulsed neutron source
;

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          12800
_pd_instr_dist_spec/detc         800
_pd_meas_2theta_fixed            90

_pd_proc_ls_profile_function     
;
Voigt function convoluted with a back-to-back double exponential.
;

_pd_proc_ls_background_function  'Chebychev polynomial'

_pd_proc_ls_pref_orient_corr     
;
No requirement for preferred orientation correction
;

_pd_proc_ls_prof_R_factor        ? 
_pd_proc_ls_prof_wR_factor       0.1110
_pd_proc_ls_prof_R_expected      ?
_refine_ls_goodness_of_fit_all   1.06
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         0.0511

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_pd_proc_number_of_points        ?
_refine_ls_number_parameters     84
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_shift/su_max          0.02

_pd_proc_info_excluded_regions   
;
?

;
_pd_proc_info_data_reduction     
;
Custom ISIS software
;

_refine_special_details          
;
Geometric restraints are detailed in the manuscript. 

------------------------------------------------------------------------------------
Check-cif alerts

PROBLEM: No Wavelength found in CIF - 0.71073 Ang Assumed     Please Check

RESPONSE: The time of flight method was used


PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  

RESPONSE: No action taken.

------------------------------------------------------------------------------------

;

loop_
      _atom_site_type_symbol
      _atom_site_label
      _atom_site_fract_x
      _atom_site_fract_y
      _atom_site_fract_z
      _atom_site_occupancy
      _atom_site_thermal_displace_type
      _atom_site_U_iso_or_equiv
      _atom_site_symmetry_multiplicity
P P11     0.8790(25)   0.2851(13)  -0.2328(7)    1.0        Uiso   0.0016(9)     4
O O11     0.6548(32)   0.1522(17)  -0.2017(9)    1.0        Uiso   0.0016(9)     4
D D11     0.708(5)     0.0975(22)  -0.1439(12)   1.0        Uiso   0.0206(19)    4
O O12     1.0649(30)   0.3318(18)  -0.1470(9)    1.0        Uiso   0.0016(9)     4
O O13     0.7176(35)   0.4394(15)  -0.2706(11)   1.0        Uiso   0.0016(9)     4
D D13     0.649(4)     0.5331(23)  -0.2407(13)   1.0        Uiso   0.0206(19)    4
O O14     1.0691(33)   0.2106(20)  -0.3147(9)    1.0        Uiso   0.0016(9)     4
D D14     1.139(5)     0.2913(24)  -0.3597(12)   1.0        Uiso   0.0206(19)    4
P P22     0.5699(22)   0.5197(11)   0.0000(7)    1.0        Uiso   0.0016(9)     4
O O21     0.7990(30)   0.6564(15)   0.0194(12)   1.0        Uiso   0.0016(9)     4
D D21     1.0011(35)   0.6197(22)   0.0275(15)   1.0        Uiso   0.0206(19)    4
O O22     0.4643(32)   0.5356(18)  -0.1060(8)    1.0        Uiso   0.0016(9)     4
D D22     0.290(4)     0.4765(26)  -0.1255(12)   1.0        Uiso   0.0206(19)    4
O O23     0.7191(32)   0.3511(14)   0.0153(12)   1.0        Uiso   0.0016(9)     4
D D23     0.649(4)     0.2766(22)   0.0650(13)   1.0        Uiso   0.0206(19)    4
O O24     0.3051(27)   0.5345(16)   0.0639(9)    1.0        Uiso   0.0016(9)     4


loop_ _atom_type_symbol
      _atom_type_number_in_cell
                   P   8.0        
                   O  32.0        
                   D  24.0          


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P11  O11   1.548(17) . . no     
P11  O12   1.505(16) . . no     
P11  O13   1.550(17) . . no     
P11  O14   1.547(17) . . no
O11  D11     0.95(2) . . no     
O13  D13     0.93(2) . . no     
O14  D14     0.96(2) . . no
P22  O21   1.548(16) . . no     
P22  O22   1.550(15) . . no     
P22  O23   1.552(15) . . no      
P22  O24   1.493(16) . . no
O21  D21     0.97(2) . . no     
O22  D22     0.96(2) . . no     
O23  D23     0.97(2) . . no



loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11  P11  O12   108.9(9) . . . no       
O11  P11  O13  111.3(10) . . . no       
O11  P11  O14  106.8(10) . . . no
O12  P11  O13  108.7(10) . . . no       
O12  P11  O14   111.8(9) . . . no       
O13  P11  O14  109.4(10) . . . no
P11  O11  D11  113.7(17) . . . no       
P11  O13  D13  133.1(18) . . . no       
P11  O14  D14  113.0(17) . . . no
O21  P22  O22  108.0(10) . . . no       
O21  P22  O23   109.4(9) . . . no       
O21  P22  O24   111.9(9) . . . no
O22  P22  O23  109.8(10) . . . no       
O22  P22  O24   107.9(9) . . . no       
O23  P22  O24   109.8(9) . . . no
P22  O21  D21  115.2(15) . . . no       
P22  O22  D22  118.5(15) . . . no       
P22  O23  D23  120.9(16) . . . no 



loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12  P11  O11  D11      -19(2) . . . . no    
O13  P11  O11  D11  -138.8(17) . . . . no    
O14  P11  O11  D11   101.9(18) . . . . no
O11  P11  O13  D13       89(3) . . . . no    
O12  P11  O13  D13      -31(3) . . . . no    
O14  P11  O13  D13     -153(2) . . . . no
O11  P11  O14  D14   150.3(18) . . . . no    
O12  P11  O14  D14   -90.7(19) . . . . no    
O13  P11  O14  D14       30(2) . . . . no
O22  P22  O21  D21     -110(2) . . . . no    
O23  P22  O21  D21        9(2) . . . . no    
O24  P22  O21  D21   131.2(19) . . . . no
O21  P22  O22  D22     -166(2) . . . . no    
O23  P22  O22  D22       75(2) . . . . no    
O24  P22  O22  D22      -45(2) . . . . no
O21  P22  O23  D23   117.7(19) . . . . no    
O22  P22  O23  D23  -123.9(19) . . . . no    
O24  P22  O23  D23       -5(2) . . . . no

