 
data_danburite_1.1GPa
#==============================================================================

# PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic      2017-05-31
_journal_date_to_coeditor         ?
_journal_date_from_coeditor       ?
_journal_date_accepted     2017-07-18
_journal_date_printers_first      ?
_journal_date_printers_final      ?
_journal_date_proofs_out          ?
_journal_date_proofs_in           ?
_journal_coeditor_name            ?
_journal_coeditor_code      LT5006SUP1
_journal_coeditor_notes
; ?
;
_journal_paper_category      FA
_journal_techeditor_code      M171061
_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         ?

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



_publ_requested_journal          'International Union of Crystallography' 

_publ_contact_author_name        'Anna Pakhomova'
_publ_contact_author_address     
;Deutsches Elektronen-Synchrotron (DESY)
Notkestrasse 85
22607 Hamburg
Germany
;
_publ_contact_author_email       anna.pakhomova@desy.de
_publ_contact_author_phone       00494089985457
loop_
_publ_author_name
_publ_author_address
'Pakhomova, Anna'
;Deutsches Elektronen-Synchrotron (DESY)
Notkestrasse 85
22607 Hamburg
Germany
;
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         danburite
_chemical_name_common             danburite
_chemical_melting_point           ?
_chemical_formula_moiety          'B2 Ca O8 Si2' 
_chemical_formula_sum
 'B2 Ca O8 Si2' 
_chemical_formula_weight          245.88

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'B'  'B'  -0.0005   0.0001
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'  -0.0010   0.0008
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.0082   0.0108
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ca'  'Ca'   0.0424   0.0512
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            62
_space_group_name_H-M_alt         'P n a m'
_space_group_name_Hall            '-P 2c 2n'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

 
data_danburite_22.6GPa
_database_code_depnum_ccdc_archive 'CCDC 1562973'


_publ_requested_journal          'International Union of Crystallography' 

_publ_contact_author_name        'Anna Pakhomova'
_publ_contact_author_address     
;Deutsches Elektronen-Synchrotron (DESY)
Notkestrasse 85
22607 Hamburg
Germany
;
_publ_contact_author_email       anna.pakhomova@desy.de
_publ_contact_author_phone       00494089985457
loop_
_publ_author_name
_publ_author_address
'Pakhomova, Anna'
;Deutsches Elektronen-Synchrotron (DESY)
Notkestrasse 85
22607 Hamburg
Germany
;

_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         danburite
_chemical_name_common             danburite
_chemical_melting_point           ?
_chemical_formula_moiety          'B2 Ca O8 Si2' 
_chemical_formula_sum
 'B2 Ca O8 Si2' 
_chemical_formula_weight          245.88

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'B'  'B'  -0.0005   0.0001
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'  -0.0010   0.0008
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.0082   0.0108
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ca'  'Ca'   0.0424   0.0512
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            62
_space_group_name_H-M_alt         'P n a m'
_space_group_name_Hall            '-P 2c 2n'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 '-x+1/2, y+1/2, -z'
 'x+1/2, -y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, y, -z-1/2'
 'x-1/2, -y-1/2, z'
 '-x-1/2, y-1/2, z-1/2'
 
_cell_length_a                    6.8576(3)
_cell_length_b                    8.1526(3)
_cell_length_c                    7.7457(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      433.04(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_pressure        22600000
_cell_measurement_reflns_used     1462
_cell_measurement_theta_min       1.9150
_cell_measurement_theta_max       16.8350
 
_exptl_crystal_description        'plate crystal'
_exptl_crystal_colour             colorless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_density_diffrn     3.771          
_exptl_crystal_F_000              488
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.020
_exptl_crystal_size_mid           0.015
_exptl_crystal_size_min           0.010
_exptl_absorpt_coefficient_mu     0.200
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_ambient_pressure          22600000
_diffrn_radiation_wavelength      0.29024
_diffrn_radiation_type            synchrotron
_diffrn_source                    synchrotron
_diffrn_source_type              'PETRA III, Beamline P02.2'
_diffrn_measurement_device_type   'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             2397
_diffrn_reflns_av_unetI/netI      0.0229
_diffrn_reflns_av_R_equivalents   0.0191
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          1.914
_diffrn_reflns_theta_max          16.875
_diffrn_reflns_theta_full         10.029
_diffrn_measured_fraction_theta_max   0.513
_diffrn_measured_fraction_theta_full  0.798
_diffrn_reflns_Laue_measured_fraction_max    0.513
_diffrn_reflns_Laue_measured_fraction_full   0.798
_diffrn_reflns_point_group_measured_fraction_max   0.513
_diffrn_reflns_point_group_measured_fraction_full  0.798
_reflns_number_total              977
_reflns_number_gt                 926
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction         
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0392P)²+0.1215P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.31(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          977
_refine_ls_number_parameters      65
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0293
_refine_ls_R_factor_gt            0.0262
_refine_ls_wR_factor_ref          0.0723
_refine_ls_wR_factor_gt           0.0698
_refine_ls_goodness_of_fit_ref    1.190
_refine_ls_restrained_S_all       1.190
_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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ca1 Ca 0.29419(6) 0.10190(4) 0.2500 0.00719(9) Uani 1 2 d S T P . .
Si1 Si 0.03614(5) 0.20673(4) -0.07259(4) 0.00489(10) Uani 1 1 d . . . . .
O1 O 0.24215(15) 0.11070(9) -0.06377(11) 0.00669(15) Uani 1 1 d . . . . .
O2 O 0.11319(15) 0.39013(9) -0.05885(10) 0.00566(15) Uani 1 1 d . . . . .
O3 O 0.41806(15) 0.35396(10) 0.09171(10) 0.00630(15) Uani 1 1 d . . . . .
O4 O 0.5693(2) 0.65715(14) 0.2500 0.00591(19) Uani 1 2 d S T P . .
O5 O 0.1327(2) 0.39500(13) 0.2500 0.0059(2) Uani 1 2 d S T P . .
B1 B 0.2286(2) 0.43902(14) 0.40961(13) 0.00560(19) Uani 1 1 d . . . . .
 
 
_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
Ca1 O5 2.3218(15) 7_665 ?
Ca1 O2 2.3614(8) 3_545 ?
Ca1 O2 2.3614(8) 8_656 ?
Ca1 O1 2.4574(8) 6_556 ?
Ca1 O1 2.4575(8) . ?
Ca1 O3 2.5392(9) 6_556 ?
Ca1 O3 2.5392(9) . ?
Ca1 O4 2.6152(12) 7_565 ?
Ca1 O5 2.6336(12) . ?
Ca1 O3 2.8786(11) 7_565 ?
Ca1 O3 2.8786(11) 4_455 ?
Ca1 B1 2.9562(11) 8_655 ?
Si1 O3 1.5875(9) 7_565 ?
Si1 O2 1.5894(8) . ?
Si1 O4 1.6044(7) 3_545 ?
Si1 O1 1.6166(10) . ?
Si1 Si1 2.7483(6) 6 ?
Si1 Ca1 3.3809(4) 7_565 ?
O1 B1 1.4289(14) 8_655 ?
O2 B1 1.4566(15) 6_556 ?
O2 Ca1 2.3614(8) 3 ?
O3 B1 1.4727(17) 6_556 ?
O3 Si1 1.5875(9) 7_665 ?
O3 Ca1 2.8785(11) 7_665 ?
O4 Si1 1.6044(7) 3 ?
O4 Si1 1.6044(7) 8_666 ?
O4 Ca1 2.6152(12) 7_665 ?
O5 B1 1.4454(14) 6_556 ?
O5 B1 1.4455(14) . ?
O5 Ca1 2.3218(15) 7_565 ?
B1 O1 1.4289(14) 8_666 ?
B1 O2 1.4566(15) 6_556 ?
B1 O3 1.4727(17) 6_556 ?
B1 Ca1 2.9562(11) 3_556 ?
B1 Ca1 3.2426(14) 7_565 ?
 
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
O5 Ca1 O2 74.87(3) 7_665 3_545 ?
O5 Ca1 O2 74.87(3) 7_665 8_656 ?
O2 Ca1 O2 77.66(4) 3_545 8_656 ?
O5 Ca1 O1 98.33(3) 7_665 6_556 ?
O2 Ca1 O1 132.88(3) 3_545 6_556 ?
O2 Ca1 O1 55.97(3) 8_656 6_556 ?
O5 Ca1 O1 98.33(3) 7_665 . ?
O2 Ca1 O1 55.97(3) 3_545 . ?
O2 Ca1 O1 132.88(3) 8_656 . ?
O1 Ca1 O1 162.97(5) 6_556 . ?
O5 Ca1 O3 69.92(3) 7_665 6_556 ?
O2 Ca1 O3 143.56(4) 3_545 6_556 ?
O2 Ca1 O3 101.48(3) 8_656 6_556 ?
O1 Ca1 O3 63.09(3) 6_556 6_556 ?
O1 Ca1 O3 120.16(3) . 6_556 ?
O5 Ca1 O3 69.92(3) 7_665 . ?
O2 Ca1 O3 101.48(3) 3_545 . ?
O2 Ca1 O3 143.56(4) 8_656 . ?
O1 Ca1 O3 120.16(3) 6_556 . ?
O1 Ca1 O3 63.09(3) . . ?
O3 Ca1 O3 57.74(4) 6_556 . ?
O5 Ca1 O4 126.77(4) 7_665 7_565 ?
O2 Ca1 O4 64.42(3) 3_545 7_565 ?
O2 Ca1 O4 64.42(3) 8_656 7_565 ?
O1 Ca1 O4 86.44(2) 6_556 7_565 ?
O1 Ca1 O4 86.44(2) . 7_565 ?
O3 Ca1 O4 148.30(2) 6_556 7_565 ?
O3 Ca1 O4 148.30(2) . 7_565 ?
O5 Ca1 O5 114.24(4) 7_665 . ?
O2 Ca1 O5 140.94(2) 3_545 . ?
O2 Ca1 O5 140.94(2) 8_656 . ?
O1 Ca1 O5 84.98(2) 6_556 . ?
O1 Ca1 O5 84.98(2) . . ?
O3 Ca1 O5 53.58(3) 6_556 . ?
O3 Ca1 O5 53.58(3) . . ?
O4 Ca1 O5 119.00(4) 7_565 . ?
O5 Ca1 O3 153.464(19) 7_665 7_565 ?
O2 Ca1 O3 93.75(3) 3_545 7_565 ?
O2 Ca1 O3 126.83(3) 8_656 7_565 ?
O1 Ca1 O3 106.71(3) 6_556 7_565 ?
O1 Ca1 O3 56.29(3) . 7_565 ?
O3 Ca1 O3 113.84(3) 6_556 7_565 ?
O3 Ca1 O3 89.59(2) . 7_565 ?
O4 Ca1 O3 64.69(3) 7_565 7_565 ?
O5 Ca1 O3 60.65(3) . 7_565 ?
O5 Ca1 O3 153.464(19) 7_665 4_455 ?
O2 Ca1 O3 126.83(3) 3_545 4_455 ?
O2 Ca1 O3 93.75(3) 8_656 4_455 ?
O1 Ca1 O3 56.29(3) 6_556 4_455 ?
O1 Ca1 O3 106.71(3) . 4_455 ?
O3 Ca1 O3 89.59(2) 6_556 4_455 ?
O3 Ca1 O3 113.84(3) . 4_455 ?
O4 Ca1 O3 64.69(3) 7_565 4_455 ?
O5 Ca1 O3 60.65(3) . 4_455 ?
O3 Ca1 O3 50.42(3) 7_565 4_455 ?
O5 Ca1 B1 93.31(3) 7_665 8_655 ?
O2 Ca1 B1 29.15(3) 3_545 8_655 ?
O2 Ca1 B1 104.18(3) 8_656 8_655 ?
O1 Ca1 B1 152.56(3) 6_556 8_655 ?
O1 Ca1 B1 28.76(3) . 8_655 ?
O3 Ca1 B1 144.28(3) 6_556 8_655 ?
O3 Ca1 B1 87.17(3) . 8_655 ?
O4 Ca1 B1 66.80(3) 7_565 8_655 ?
O5 Ca1 B1 112.66(3) . 8_655 ?
O3 Ca1 B1 68.22(3) 7_565 8_655 ?
O3 Ca1 B1 112.87(3) 4_455 8_655 ?
O3 Si1 O2 114.15(4) 7_565 . ?
O3 Si1 O4 112.23(6) 7_565 3_545 ?
O2 Si1 O4 116.37(5) . 3_545 ?
O3 Si1 O1 105.13(5) 7_565 . ?
O2 Si1 O1 99.34(5) . . ?
O4 Si1 O1 107.94(6) 3_545 . ?
O3 Si1 Si1 143.29(3) 7_565 6 ?
O2 Si1 Si1 93.84(3) . 6 ?
O4 Si1 Si1 31.08(4) 3_545 6 ?
O1 Si1 Si1 92.42(3) . 6 ?
O3 Si1 Ca1 64.54(4) 7_565 . ?
O2 Si1 Ca1 90.87(3) . . ?
O4 Si1 Ca1 148.90(4) 3_545 . ?
O1 Si1 Ca1 49.47(3) . . ?
Si1 Si1 Ca1 141.816(8) 6 . ?
O3 Si1 Ca1 45.65(3) 7_565 7_565 ?
O2 Si1 Ca1 71.31(3) . 7_565 ?
O4 Si1 Ca1 121.88(5) 3_545 7_565 ?
O1 Si1 Ca1 128.40(3) . 7_565 ?
Si1 Si1 Ca1 137.651(7) 6 7_565 ?
Ca1 Si1 Ca1 79.416(8) . 7_565 ?
B1 O1 Si1 126.22(9) 8_655 . ?
B1 O1 Ca1 95.38(6) 8_655 . ?
Si1 O1 Ca1 100.54(4) . . ?
B1 O2 Si1 119.42(7) 6_556 . ?
B1 O2 Ca1 98.71(6) 6_556 3 ?
Si1 O2 Ca1 137.33(4) . 3 ?
B1 O3 Si1 126.24(7) 6_556 7_665 ?
B1 O3 Ca1 95.12(7) 6_556 . ?
Si1 O3 Ca1 107.79(4) 7_665 . ?
B1 O3 Ca1 137.27(6) 6_556 7_665 ?
Si1 O3 Ca1 85.60(4) 7_665 7_665 ?
Ca1 O3 Ca1 101.26(3) . 7_665 ?
Si1 O4 Si1 117.85(8) 3 8_666 ?
Si1 O4 Ca1 117.98(4) 3 7_665 ?
Si1 O4 Ca1 117.98(4) 8_666 7_665 ?
B1 O5 B1 117.58(14) 6_556 . ?
B1 O5 Ca1 116.88(8) 6_556 7_565 ?
B1 O5 Ca1 116.88(8) . 7_565 ?
B1 O5 Ca1 91.95(7) 6_556 . ?
B1 O5 Ca1 91.95(7) . . ?
Ca1 O5 Ca1 115.48(5) 7_565 . ?
O1 B1 O5 115.50(9) 8_666 . ?
O1 B1 O2 103.28(8) 8_666 6_556 ?
O5 B1 O2 111.33(11) . 6_556 ?
O1 B1 O3 109.78(10) 8_666 6_556 ?
O5 B1 O3 106.16(9) . 6_556 ?
O2 B1 O3 110.85(9) 6_556 6_556 ?
O1 B1 Ca1 55.86(5) 8_666 3_556 ?
O5 B1 Ca1 148.24(9) . 3_556 ?
O2 B1 Ca1 52.15(5) 6_556 3_556 ?
O3 B1 Ca1 105.33(6) 6_556 3_556 ?
O1 B1 Ca1 157.13(8) 8_666 . ?
O5 B1 Ca1 59.75(6) . . ?
O2 B1 Ca1 98.94(6) 6_556 . ?
O3 B1 Ca1 56.10(5) 6_556 . ?
Ca1 B1 Ca1 140.79(4) 3_556 . ?
O1 B1 Ca1 106.54(8) 8_666 7_565 ?
O5 B1 Ca1 39.69(7) . 7_565 ?
O2 B1 Ca1 77.01(7) 6_556 7_565 ?
O3 B1 Ca1 139.41(7) 6_556 7_565 ?
Ca1 B1 Ca1 109.74(4) 3_556 7_565 ?
Ca1 B1 Ca1 83.58(3) . 7_565 ?
 
_refine_diff_density_max    0.642
_refine_diff_density_min   -0.753
_refine_diff_density_rms    0.151



 
data_danburite_25.4GPa
_database_code_depnum_ccdc_archive 'CCDC 1562974'



_publ_requested_journal          'International Union of Crystallography'

_publ_contact_author_name        'Anna Pakhomova'
_publ_contact_author_address     
;Deutsches Elektronen-Synchrotron (DESY)
Notkestrasse 85
22607 Hamburg
Germany
;
_publ_contact_author_email       anna.pakhomova@desy.de
_publ_contact_author_phone       00494089985457
loop_
_publ_author_name
_publ_author_address
'Pakhomova, Anna'
;Deutsches Elektronen-Synchrotron (DESY)
Notkestrasse 85
22607 Hamburg
Germany
; 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         danburite
_chemical_name_common             danburite
_chemical_melting_point           ?
_chemical_formula_moiety          'B2 Ca O8 Si2' 
_chemical_formula_sum
 'B2 Ca O8 Si2' 
_chemical_formula_weight          245.88

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'B'  'B'  -0.0005   0.0001
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'  -0.0010   0.0008
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.0083   0.0108
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ca'  'Ca'   0.0425   0.0513
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            62
_space_group_name_H-M_alt         'P n a m'
_space_group_name_Hall            '-P 2c 2n'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 '-x+1/2, y+1/2, -z'
 'x+1/2, -y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, y, -z-1/2'
 'x-1/2, -y-1/2, z'
 '-x-1/2, y-1/2, z-1/2'
 
_cell_length_a                    6.3537(5)
_cell_length_b                    7.9518(3)
_cell_length_c                    8.0112(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      404.75(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_pressure        25400000
_cell_measurement_reflns_used     977
_cell_measurement_theta_min       1.6750
_cell_measurement_theta_max       16.6370
 
 
_exptl_crystal_description        'plate crystal'
_exptl_crystal_colour             colorless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     4.035          
_exptl_crystal_F_000              488
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.020
_exptl_crystal_size_mid           0.015
_exptl_crystal_size_min           0.010
_exptl_absorpt_coefficient_mu     0.215
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_ambient_pressure          25400000
_diffrn_radiation_wavelength      0.29056
_diffrn_radiation_type            synchrotron
_diffrn_source                    synchrotron
_diffrn_source_type              'PETRA III, Beamline P02.2'
_diffrn_measurement_device_type   'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             2163
_diffrn_reflns_av_unetI/netI      0.0291
_diffrn_reflns_av_R_equivalents   0.0239
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          1.677
_diffrn_reflns_theta_max          16.730
_diffrn_reflns_theta_full         10.500
_diffrn_measured_fraction_theta_max   0.515
_diffrn_measured_fraction_theta_full  0.796
_diffrn_reflns_Laue_measured_fraction_max    0.515
_diffrn_reflns_Laue_measured_fraction_full   0.796
_diffrn_reflns_point_group_measured_fraction_max   0.515
_diffrn_reflns_point_group_measured_fraction_full  0.796
_reflns_number_total              891
_reflns_number_gt                 742
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction         
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0923P)²+0.4473P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.18(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          891
_refine_ls_number_parameters      65
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0596
_refine_ls_R_factor_gt            0.0423
_refine_ls_wR_factor_ref          0.1783
_refine_ls_wR_factor_gt           0.1256
_refine_ls_goodness_of_fit_ref    1.321
_refine_ls_restrained_S_all       1.321
_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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ca1 Ca 0.25404(13) 0.10929(9) 0.2500 0.0112(2) Uani 1 2 d S T P . .
Si1 Si -0.00581(14) 0.23537(9) -0.07365(10) 0.0103(3) Uani 1 1 d . . . . .
O1 O 0.2513(3) 0.1368(2) -0.0738(3) 0.0111(4) Uani 1 1 d . . . . .
O2 O 0.1243(4) 0.4068(2) -0.0572(2) 0.0099(4) Uani 1 1 d . . . . .
O3 O 0.4325(4) 0.3664(2) 0.0939(2) 0.0110(4) Uani 1 1 d . . . . .
O4 O 0.5630(5) 0.6518(3) 0.2500 0.0114(5) Uani 1 2 d S T P . .
O5 O 0.1238(5) 0.4081(3) 0.2500 0.0111(5) Uani 1 2 d S T P . .
B1 B 0.2292(5) 0.4549(3) 0.4046(3) 0.0093(5) Uani 1 1 d . . . . .
 
 
_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
Ca1 O5 2.354(3) 7_665 ?
Ca1 O2 2.3614(19) 3_545 ?
Ca1 O2 2.3614(19) 8_656 ?
Ca1 O3 2.403(2) 7_565 ?
Ca1 O3 2.403(2) 4_455 ?
Ca1 O4 2.405(3) 7_565 ?
Ca1 O5 2.516(3) . ?
Ca1 O1 2.603(2) . ?
Ca1 O1 2.603(2) 6_556 ?
Ca1 O3 2.651(2) 6_556 ?
Ca1 O3 2.651(2) . ?
Ca1 B1 3.019(3) . ?
Si1 O2 1.600(2) . ?
Si1 O4 1.6030(15) 3_545 ?
Si1 O3 1.6157(19) 7_565 ?
Si1 O1 1.812(2) . ?
Si1 O1 1.848(2) 7_565 ?
Si1 Si1 2.8256(15) 6 ?
Si1 Ca1 3.2522(9) 7_565 ?
Si1 Ca1 3.4633(10) 5 ?
O1 B1 1.461(3) 8_655 ?
O1 Si1 1.848(2) 7_665 ?
O2 B1 1.444(3) 6_556 ?
O2 Ca1 2.3614(19) 3 ?
O3 B1 1.471(4) 6_556 ?
O3 Si1 1.6157(19) 7_665 ?
O3 Ca1 2.403(2) 7_665 ?
O4 Si1 1.6030(15) 8_666 ?
O4 Si1 1.6030(15) 3 ?
O4 Ca1 2.405(3) 7_665 ?
O5 B1 1.456(3) . ?
O5 B1 1.456(3) 6_556 ?
O5 Ca1 2.354(3) 7_565 ?
B1 O2 1.444(3) 6_556 ?
B1 O1 1.461(3) 8_666 ?
B1 O3 1.471(4) 6_556 ?
B1 Ca1 3.029(3) 3_556 ?
 
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
O5 Ca1 O2 68.48(7) 7_665 3_545 ?
O5 Ca1 O2 68.48(7) 7_665 8_656 ?
O2 Ca1 O2 81.70(9) 3_545 8_656 ?
O5 Ca1 O3 148.59(5) 7_665 7_565 ?
O2 Ca1 O3 89.58(7) 3_545 7_565 ?
O2 Ca1 O3 132.34(8) 8_656 7_565 ?
O5 Ca1 O3 148.59(5) 7_665 4_455 ?
O2 Ca1 O3 132.34(8) 3_545 4_455 ?
O2 Ca1 O3 89.58(7) 8_656 4_455 ?
O3 Ca1 O3 62.71(10) 7_565 4_455 ?
O5 Ca1 O4 116.94(10) 7_665 7_565 ?
O2 Ca1 O4 64.95(7) 3_545 7_565 ?
O2 Ca1 O4 64.95(7) 8_656 7_565 ?
O3 Ca1 O4 68.92(8) 7_565 7_565 ?
O3 Ca1 O4 68.92(8) 4_455 7_565 ?
O5 Ca1 O5 112.57(9) 7_665 . ?
O2 Ca1 O5 138.73(5) 3_545 . ?
O2 Ca1 O5 138.73(5) 8_656 . ?
O3 Ca1 O5 69.18(8) 7_565 . ?
O3 Ca1 O5 69.18(8) 4_455 . ?
O4 Ca1 O5 130.49(11) 7_565 . ?
O5 Ca1 O1 90.67(5) 7_665 . ?
O2 Ca1 O1 53.68(6) 3_545 . ?
O2 Ca1 O1 135.34(7) 8_656 . ?
O3 Ca1 O1 57.92(6) 7_565 . ?
O3 Ca1 O1 120.40(7) 4_455 . ?
O4 Ca1 O1 93.96(5) 7_565 . ?
O5 Ca1 O1 85.33(5) . . ?
O5 Ca1 O1 90.67(5) 7_665 6_556 ?
O2 Ca1 O1 135.34(7) 3_545 6_556 ?
O2 Ca1 O1 53.68(6) 8_656 6_556 ?
O3 Ca1 O1 120.40(7) 7_565 6_556 ?
O3 Ca1 O1 57.92(6) 4_455 6_556 ?
O4 Ca1 O1 93.96(5) 7_565 6_556 ?
O5 Ca1 O1 85.33(5) . 6_556 ?
O1 Ca1 O1 170.34(9) . 6_556 ?
O5 Ca1 O3 67.57(7) 7_665 6_556 ?
O2 Ca1 O3 133.98(8) 3_545 6_556 ?
O2 Ca1 O3 94.44(6) 8_656 6_556 ?
O3 Ca1 O3 123.16(6) 7_565 6_556 ?
O3 Ca1 O3 93.22(6) 4_455 6_556 ?
O4 Ca1 O3 151.83(4) 7_565 6_556 ?
O5 Ca1 O3 54.01(8) . 6_556 ?
O1 Ca1 O3 114.09(7) . 6_556 ?
O1 Ca1 O3 57.87(6) 6_556 6_556 ?
O5 Ca1 O3 67.57(7) 7_665 . ?
O2 Ca1 O3 94.44(6) 3_545 . ?
O2 Ca1 O3 133.98(8) 8_656 . ?
O3 Ca1 O3 93.22(6) 7_565 . ?
O3 Ca1 O3 123.16(6) 4_455 . ?
O4 Ca1 O3 151.83(4) 7_565 . ?
O5 Ca1 O3 54.01(8) . . ?
O1 Ca1 O3 57.88(6) . . ?
O1 Ca1 O3 114.09(7) 6_556 . ?
O3 Ca1 O3 56.28(8) 6_556 . ?
O5 Ca1 B1 96.08(9) 7_665 . ?
O2 Ca1 B1 155.01(8) 3_545 . ?
O2 Ca1 B1 111.69(7) 8_656 . ?
O3 Ca1 B1 95.50(8) 7_565 . ?
O3 Ca1 B1 70.66(8) 4_455 . ?
O4 Ca1 B1 139.42(9) 7_565 . ?
O5 Ca1 B1 28.71(7) . . ?
O1 Ca1 B1 109.40(7) . . ?
O1 Ca1 B1 60.95(7) 6_556 . ?
O3 Ca1 B1 29.17(8) 6_556 . ?
O3 Ca1 B1 60.91(7) . . ?
O2 Si1 O4 122.89(12) . 3_545 ?
O2 Si1 O3 118.93(11) . 7_565 ?
O4 Si1 O3 118.01(13) 3_545 7_565 ?
O2 Si1 O1 84.42(11) . . ?
O4 Si1 O1 91.39(14) 3_545 . ?
O3 Si1 O1 90.14(11) 7_565 . ?
O2 Si1 O1 87.88(10) . 7_565 ?
O4 Si1 O1 92.20(14) 3_545 7_565 ?
O3 Si1 O1 94.22(12) 7_565 7_565 ?
O1 Si1 O1 172.27(8) . 7_565 ?
O2 Si1 Si1 94.73(7) . 6 ?
O4 Si1 Si1 28.20(9) 3_545 6 ?
O3 Si1 Si1 146.19(7) 7_565 6 ?
O1 Si1 Si1 89.96(7) . 6 ?
O1 Si1 Si1 89.96(7) 7_565 6 ?
O2 Si1 Ca1 86.23(8) . . ?
O4 Si1 Ca1 133.94(11) 3_545 . ?
O3 Si1 Ca1 45.75(9) 7_565 . ?
O1 Si1 Ca1 53.56(7) . . ?
O1 Si1 Ca1 126.69(7) 7_565 . ?
Si1 Si1 Ca1 143.315(18) 6 . ?
O2 Si1 Ca1 81.56(8) . 7_565 ?
O4 Si1 Ca1 138.93(13) 3_545 7_565 ?
O3 Si1 Ca1 54.13(8) 7_565 7_565 ?
O1 Si1 Ca1 126.01(8) . 7_565 ?
O1 Si1 Ca1 53.11(7) 7_565 7_565 ?
Si1 Si1 Ca1 142.869(18) 6 7_565 ?
Ca1 Si1 Ca1 73.62(2) . 7_565 ?
O2 Si1 Ca1 160.61(8) . 5 ?
O4 Si1 Ca1 37.74(9) 3_545 5 ?
O3 Si1 Ca1 80.34(8) 7_565 5 ?
O1 Si1 Ca1 93.89(7) . 5 ?
O1 Si1 Ca1 93.14(7) 7_565 5 ?
Si1 Si1 Ca1 65.925(14) 6 5 ?
Ca1 Si1 Ca1 108.32(2) . 5 ?
Ca1 Si1 Ca1 114.34(3) 7_565 5 ?
B1 O1 Si1 120.32(18) 8_655 . ?
B1 O1 Si1 118.25(18) 8_655 7_665 ?
Si1 O1 Si1 120.98(11) . 7_665 ?
B1 O1 Ca1 91.96(14) 8_655 . ?
Si1 O1 Ca1 92.39(9) . . ?
Si1 O1 Ca1 92.28(9) 7_665 . ?
B1 O2 Si1 122.29(16) 6_556 . ?
B1 O2 Ca1 102.82(15) 6_556 3 ?
Si1 O2 Ca1 134.13(11) . 3 ?
B1 O3 Si1 117.34(17) 6_556 7_665 ?
B1 O3 Ca1 134.73(15) 6_556 7_665 ?
Si1 O3 Ca1 105.45(12) 7_665 7_665 ?
B1 O3 Ca1 89.41(14) 6_556 . ?
Si1 O3 Ca1 96.28(9) 7_665 . ?
Ca1 O3 Ca1 100.38(7) 7_665 . ?
Si1 O4 Si1 123.61(18) 8_666 3 ?
Si1 O4 Ca1 118.18(9) 8_666 7_665 ?
Si1 O4 Ca1 118.18(9) 3 7_665 ?
B1 O5 B1 116.5(3) . 6_556 ?
B1 O5 Ca1 118.29(17) . 7_565 ?
B1 O5 Ca1 118.29(17) 6_556 7_565 ?
B1 O5 Ca1 95.17(17) . . ?
B1 O5 Ca1 95.17(17) 6_556 . ?
Ca1 O5 Ca1 105.81(11) 7_565 . ?
O2 B1 O5 116.1(3) 6_556 . ?
O2 B1 O1 101.6(2) 6_556 8_666 ?
O5 B1 O1 113.1(2) . 8_666 ?
O2 B1 O3 105.8(2) 6_556 6_556 ?
O5 B1 O3 106.7(2) . 6_556 ?
O1 B1 O3 113.4(2) 8_666 6_556 ?
O2 B1 Ca1 97.47(14) 6_556 . ?
O5 B1 Ca1 56.11(14) . . ?
O1 B1 Ca1 160.88(18) 8_666 . ?
O3 B1 Ca1 61.42(12) 6_556 . ?
O2 B1 Ca1 49.48(12) 6_556 3_556 ?
O5 B1 Ca1 153.7(2) . 3_556 ?
O1 B1 Ca1 59.20(12) 8_666 3_556 ?
O3 B1 Ca1 98.96(15) 6_556 3_556 ?
Ca1 B1 Ca1 137.90(10) . 3_556 ?
 
_refine_diff_density_max    1.049
_refine_diff_density_min   -1.441
_refine_diff_density_rms    0.280




 
data_danburite-III_25.4GPa
_database_code_depnum_ccdc_archive 'CCDC 1562975'


_publ_requested_journal          'International Union of Crystallography' 

_publ_contact_author_name        'Anna Pakhomova'
_publ_contact_author_address     
;Deutsches Elektronen-Synchrotron (DESY)
Notkestrasse 85
22607 Hamburg
Germany
;
_publ_contact_author_email       anna.pakhomova@desy.de
_publ_contact_author_phone       00494089985457
loop_
_publ_author_name
_publ_author_address
'Pakhomova, Anna'
;Deutsches Elektronen-Synchrotron (DESY)
Notkestrasse 85
22607 Hamburg
Germany
;
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         danburite
_chemical_name_common             danburite
_chemical_melting_point           ?
_chemical_formula_moiety          'B2 Ca O8 Si2' 
_chemical_formula_sum
 'B2 Ca O8 Si2' 
_chemical_formula_weight          245.88

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'B'  'B'  -0.0005   0.0001
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'  -0.0010   0.0008
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.0083   0.0108
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ca'  'Ca'   0.0425   0.0513
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    5.479(5)
_cell_length_b                    5.532(2)
_cell_length_c                    6.681(6)
_cell_angle_alpha                 91.74(5)
_cell_angle_beta                  104.57(8)
_cell_angle_gamma                 95.59(5)
_cell_volume                      194.7(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     296(2)
_cell_measurement_pressure        25400000
_cell_measurement_reflns_used     150
_cell_measurement_theta_min       2.0780
_cell_measurement_theta_max       12.7910
 
_exptl_crystal_description        'plate crystal'
_exptl_crystal_colour             colorless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_density_diffrn     4.193          
_exptl_crystal_F_000              244
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.020
_exptl_crystal_size_mid           0.015
_exptl_crystal_size_min           0.010
_exptl_absorpt_coefficient_mu     0.223
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       296(2)
_diffrn_ambient_pressure          25400000
_diffrn_radiation_wavelength      0.29024
_diffrn_radiation_type            synchrotron
_diffrn_source                    synchrotron
_diffrn_source_type              'PETRA III, Beamline P02.2'
_diffrn_measurement_device_type   'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             1042
_diffrn_reflns_av_unetI/netI      0.0934
_diffrn_reflns_av_R_equivalents   0.0545
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -7
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -8
_diffrn_reflns_limit_l_max        7
_diffrn_reflns_theta_min          1.765
_diffrn_reflns_theta_max          11.151
_diffrn_reflns_theta_full         10.500
_diffrn_measured_fraction_theta_max   0.616
_diffrn_measured_fraction_theta_full  0.664
_diffrn_reflns_Laue_measured_fraction_max    0.616
_diffrn_reflns_Laue_measured_fraction_full   0.664
_diffrn_reflns_point_group_measured_fraction_max   0.616
_diffrn_reflns_point_group_measured_fraction_full  0.664
_reflns_number_total              591
_reflns_number_gt                 397
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction         
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1393P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          591
_refine_ls_number_parameters      68
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1154
_refine_ls_R_factor_gt            0.0887
_refine_ls_wR_factor_ref          0.2714
_refine_ls_wR_factor_gt           0.2368
_refine_ls_goodness_of_fit_ref    1.120
_refine_ls_restrained_S_all       1.120
_refine_ls_shift/su_max           0.488
_refine_ls_shift/su_mean          0.053
 
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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ca1 Ca 0.1796(4) 0.9158(4) 0.7626(4) 0.0238(9) Uani 1 1 d . . . . .
Si1 Si 0.3213(5) 0.3165(5) 0.5071(5) 0.0203(10) Uani 1 1 d . . . . .
Si2 Si 0.5902(5) 0.5701(5) 0.8447(5) 0.0202(10) Uani 1 1 d . . . . .
O1 O 0.2648(12) 0.0351(12) 0.4132(11) 0.0160(15) Uiso 1 1 d . . . . .
O2 O 0.5163(13) 0.2513(12) 0.7444(12) 0.0166(16) Uiso 1 1 d . . . . .
O3 O 0.0664(13) 0.3002(13) 0.5906(12) 0.0199(17) Uiso 1 1 d . . . . .
O4 O 0.4153(13) 0.6186(13) 0.5989(12) 0.0205(17) Uiso 1 1 d . . . . .
O5 O 0.0598(12) 0.8038(12) 0.1066(12) 0.0176(16) Uiso 1 1 d . . . . .
O6 O 0.3841(13) 0.1260(13) 0.0992(12) 0.0208(17) Uiso 1 1 d . . . . .
O7 O 0.7126(13) 0.4847(13) 0.0838(13) 0.0235(18) Uiso 1 1 d . . . . .
O8 O -0.1464(13) 0.5792(12) 0.7461(12) 0.0193(16) Uiso 1 1 d . . . . .
B1 B -0.027(2) 0.612(2) 0.223(2) 0.022(2) Uiso 1 1 d . . . . .
B2 B 0.702(2) 0.063(2) 0.777(2) 0.023(2) Uiso 1 1 d . . . . .
 
 
_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
Ca1 O6 2.373(7) 2_666 ?
Ca1 O5 2.404(7) 2_576 ?
Ca1 O8 2.431(7) . ?
Ca1 O6 2.446(8) 1_566 ?
Ca1 O1 2.468(7) 2_566 ?
Ca1 O3 2.505(8) 1_565 ?
Ca1 O2 2.515(7) 1_565 ?
Ca1 O7 2.530(8) 2_666 ?
Ca1 O4 2.566(8) . ?
Ca1 O1 2.585(8) 1_565 ?
Ca1 O3 2.594(7) 2_566 ?
Ca1 O5 2.620(9) 1_556 ?
Si1 O3 1.625(9) . ?
Si1 O1 1.631(7) . ?
Si1 O2 1.744(9) . ?
Si1 O4 1.745(7) . ?
Si1 O4 1.773(8) 2_666 ?
Si1 O8 1.861(9) 2_566 ?
Si1 Si2 2.599(6) 2_666 ?
Si1 Si2 2.639(5) . ?
Si1 Si1 2.702(6) 2_666 ?
Si1 Ca1 2.998(5) 1_545 ?
Si1 Ca1 3.019(5) 2_566 ?
Si2 O7 1.671(9) 1_556 ?
Si2 O6 1.696(8) 2_666 ?
Si2 O4 1.724(9) . ?
Si2 O8 1.728(8) 1_655 ?
Si2 O2 1.837(7) . ?
Si2 O7 1.839(9) 2_666 ?
Si2 Si1 2.599(6) 2_666 ?
Si2 Si2 2.620(7) 2_667 ?
O1 B2 1.427(15) 2_656 ?
O1 Ca1 2.468(7) 2_566 ?
O1 Ca1 2.585(8) 1_545 ?
O2 B2 1.509(14) . ?
O2 Ca1 2.514(7) 1_545 ?
O3 B1 1.398(16) 2_566 ?
O3 Ca1 2.505(8) 1_545 ?
O3 Ca1 2.594(7) 2_566 ?
O4 Si1 1.773(8) 2_666 ?
O5 B1 1.446(16) . ?
O5 B2 1.455(13) 2_666 ?
O5 Ca1 2.404(7) 2_576 ?
O5 Ca1 2.620(9) 1_554 ?
O6 B2 1.468(17) 2_656 ?
O6 Si2 1.696(8) 2_666 ?
O6 Ca1 2.373(7) 2_666 ?
O6 Ca1 2.446(8) 1_544 ?
O7 B1 1.577(13) 1_655 ?
O7 Si2 1.671(9) 1_554 ?
O7 Si2 1.839(9) 2_666 ?
O7 Ca1 2.530(8) 2_666 ?
O8 B1 1.477(13) 2_566 ?
O8 Si2 1.728(8) 1_455 ?
O8 Si1 1.861(9) 2_566 ?
B1 O3 1.398(16) 2_566 ?
B1 O8 1.477(13) 2_566 ?
B1 O7 1.577(13) 1_455 ?
B1 Ca1 2.824(12) 2_576 ?
B1 Ca1 2.970(12) 2_566 ?
B2 O1 1.427(15) 2_656 ?
B2 O5 1.455(13) 2_666 ?
B2 O6 1.468(17) 2_656 ?
B2 Ca1 2.838(13) 1_645 ?
B2 Ca1 2.876(13) 1_545 ?
B2 Ca1 2.977(14) 2_667 ?
 
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
O6 Ca1 O5 125.8(3) 2_666 2_576 ?
O6 Ca1 O8 121.5(3) 2_666 . ?
O5 Ca1 O8 91.9(3) 2_576 . ?
O6 Ca1 O6 63.3(3) 2_666 1_566 ?
O5 Ca1 O6 63.4(2) 2_576 1_566 ?
O8 Ca1 O6 118.5(3) . 1_566 ?
O6 Ca1 O1 174.5(3) 2_666 2_566 ?
O5 Ca1 O1 57.5(2) 2_576 2_566 ?
O8 Ca1 O1 60.9(2) . 2_566 ?
O6 Ca1 O1 120.6(2) 1_566 2_566 ?
O6 Ca1 O3 117.9(3) 2_666 1_565 ?
O5 Ca1 O3 57.6(3) 2_576 1_565 ?
O8 Ca1 O3 120.2(2) . 1_565 ?
O6 Ca1 O3 93.7(3) 1_566 1_565 ?
O1 Ca1 O3 59.3(2) 2_566 1_565 ?
O6 Ca1 O2 59.0(3) 2_666 1_565 ?
O5 Ca1 O2 91.7(2) 2_576 1_565 ?
O8 Ca1 O2 174.5(3) . 1_565 ?
O6 Ca1 O2 66.9(3) 1_566 1_565 ?
O1 Ca1 O2 118.0(3) 2_566 1_565 ?
O3 Ca1 O2 58.8(2) 1_565 1_565 ?
O6 Ca1 O7 63.1(3) 2_666 2_666 ?
O5 Ca1 O7 124.8(3) 2_576 2_666 ?
O8 Ca1 O7 58.6(2) . 2_666 ?
O6 Ca1 O7 89.4(3) 1_566 2_666 ?
O1 Ca1 O7 119.5(3) 2_566 2_666 ?
O3 Ca1 O7 176.8(3) 1_565 2_666 ?
O2 Ca1 O7 122.1(2) 1_565 2_666 ?
O6 Ca1 O4 57.6(2) 2_666 . ?
O5 Ca1 O4 176.2(3) 2_576 . ?
O8 Ca1 O4 87.2(3) . . ?
O6 Ca1 O4 120.3(2) 1_566 . ?
O1 Ca1 O4 119.0(2) 2_566 . ?
O3 Ca1 O4 119.8(3) 1_565 . ?
O2 Ca1 O4 88.9(2) 1_565 . ?
O7 Ca1 O4 57.7(3) 2_666 . ?
O6 Ca1 O1 90.7(3) 2_666 1_565 ?
O5 Ca1 O1 112.7(3) 2_576 1_565 ?
O8 Ca1 O1 116.2(2) . 1_565 ?
O6 Ca1 O1 125.3(3) 1_566 1_565 ?
O1 Ca1 O1 83.9(3) 2_566 1_565 ?
O3 Ca1 O1 55.3(2) 1_565 1_565 ?
O2 Ca1 O1 58.5(2) 1_565 1_565 ?
O7 Ca1 O1 122.1(3) 2_666 1_565 ?
O4 Ca1 O1 64.5(3) . 1_565 ?
O6 Ca1 O3 120.5(3) 2_666 2_566 ?
O5 Ca1 O3 113.0(2) 2_576 2_566 ?
O8 Ca1 O3 59.5(3) . 2_566 ?
O6 Ca1 O3 176.1(2) 1_566 2_566 ?
O1 Ca1 O3 55.6(2) 2_566 2_566 ?
O3 Ca1 O3 85.0(2) 1_565 2_566 ?
O2 Ca1 O3 115.2(3) 1_565 2_566 ?
O7 Ca1 O3 91.9(2) 2_666 2_566 ?
O4 Ca1 O3 63.4(2) . 2_566 ?
O1 Ca1 O3 56.7(2) 1_565 2_566 ?
O6 Ca1 O5 93.4(3) 2_666 1_556 ?
O5 Ca1 O5 64.2(3) 2_576 1_556 ?
O8 Ca1 O5 62.0(2) . 1_556 ?
O6 Ca1 O5 56.5(2) 1_566 1_556 ?
O1 Ca1 O5 92.0(3) 2_566 1_556 ?
O3 Ca1 O5 121.8(2) 1_565 1_556 ?
O2 Ca1 O5 123.4(2) 1_565 1_556 ?
O7 Ca1 O5 60.7(3) 2_666 1_556 ?
O4 Ca1 O5 118.5(3) . 1_556 ?
O1 Ca1 O5 175.8(2) 1_565 1_556 ?
O3 Ca1 O5 121.3(3) 2_566 1_556 ?
O3 Si1 O1 93.1(4) . . ?
O3 Si1 O2 94.0(4) . . ?
O1 Si1 O2 95.1(4) . . ?
O3 Si1 O4 93.6(4) . . ?
O1 Si1 O4 173.3(4) . . ?
O2 Si1 O4 83.9(4) . . ?
O3 Si1 O4 170.5(4) . 2_666 ?
O1 Si1 O4 93.7(4) . 2_666 ?
O2 Si1 O4 92.0(4) . 2_666 ?
O4 Si1 O4 79.7(4) . 2_666 ?
O3 Si1 O8 91.2(4) . 2_566 ?
O1 Si1 O8 90.4(4) . 2_566 ?
O2 Si1 O8 172.2(4) . 2_566 ?
O4 Si1 O8 90.0(4) . 2_566 ?
O4 Si1 O8 82.2(4) 2_666 2_566 ?
O3 Si1 Si2 132.7(3) . 2_666 ?
O1 Si1 Si2 86.8(3) . 2_666 ?
O2 Si1 Si2 133.1(3) . 2_666 ?
O4 Si1 Si2 89.0(3) . 2_666 ?
O4 Si1 Si2 41.3(3) 2_666 2_666 ?
O8 Si1 Si2 41.6(3) 2_566 2_666 ?
O3 Si1 Si2 92.0(3) . . ?
O1 Si1 Si2 139.0(3) . . ?
O2 Si1 Si2 43.9(2) . . ?
O4 Si1 Si2 40.2(3) . . ?
O4 Si1 Si2 87.1(3) 2_666 . ?
O8 Si1 Si2 130.2(3) 2_566 . ?
Si2 Si1 Si2 117.91(15) 2_666 . ?
O3 Si1 Si1 133.5(3) . 2_666 ?
O1 Si1 Si1 133.2(4) . 2_666 ?
O2 Si1 Si1 87.4(3) . 2_666 ?
O4 Si1 Si1 40.2(3) . 2_666 ?
O4 Si1 Si1 39.5(2) 2_666 2_666 ?
O8 Si1 Si1 84.9(3) 2_566 2_666 ?
Si2 Si1 Si1 59.67(15) 2_666 2_666 ?
Si2 Si1 Si1 58.24(14) . 2_666 ?
O3 Si1 Ca1 56.7(3) . 1_545 ?
O1 Si1 Ca1 59.5(3) . 1_545 ?
O2 Si1 Ca1 56.9(3) . 1_545 ?
O4 Si1 Ca1 124.5(3) . 1_545 ?
O4 Si1 Ca1 132.8(3) 2_666 1_545 ?
O8 Si1 Ca1 130.8(3) 2_566 1_545 ?
Si2 Si1 Ca1 146.31(13) 2_666 1_545 ?
Si2 Si1 Ca1 90.67(14) . 1_545 ?
Si1 Si1 Ca1 144.29(19) 2_666 1_545 ?
O3 Si1 Ca1 59.2(3) . 2_566 ?
O1 Si1 Ca1 54.8(3) . 2_566 ?
O2 Si1 Ca1 134.1(3) . 2_566 ?
O4 Si1 Ca1 130.0(3) . 2_566 ?
O4 Si1 Ca1 120.5(3) 2_666 2_566 ?
O8 Si1 Ca1 53.6(2) 2_566 2_566 ?
Si2 Si1 Ca1 83.67(14) 2_666 2_566 ?
Si2 Si1 Ca1 150.93(15) . 2_566 ?
Si1 Si1 Ca1 138.4(2) 2_666 2_566 ?
Ca1 Si1 Ca1 77.32(12) 1_545 2_566 ?
O7 Si2 O6 98.1(4) 1_556 2_666 ?
O7 Si2 O4 169.0(4) 1_556 . ?
O6 Si2 O4 88.4(4) 2_666 . ?
O7 Si2 O8 100.5(4) 1_556 1_655 ?
O6 Si2 O8 95.4(4) 2_666 1_655 ?
O4 Si2 O8 87.6(4) . 1_655 ?
O7 Si2 O2 91.1(4) 1_556 . ?
O6 Si2 O2 169.8(4) 2_666 . ?
O4 Si2 O2 81.8(4) . . ?
O8 Si2 O2 87.1(3) 1_655 . ?
O7 Si2 O7 83.5(4) 1_556 2_666 ?
O6 Si2 O7 93.1(4) 2_666 2_666 ?
O4 Si2 O7 87.3(4) . 2_666 ?
O8 Si2 O7 169.9(3) 1_655 2_666 ?
O2 Si2 O7 83.6(3) . 2_666 ?
O7 Si2 Si1 146.1(3) 1_556 2_666 ?
O6 Si2 Si1 86.0(3) 2_666 2_666 ?
O4 Si2 Si1 42.7(3) . 2_666 ?
O8 Si2 Si1 45.7(3) 1_655 2_666 ?
O2 Si2 Si1 88.7(3) . 2_666 ?
O7 Si2 Si1 130.0(3) 2_666 2_666 ?
O7 Si2 Si2 44.2(3) 1_556 2_667 ?
O6 Si2 Si2 97.4(4) 2_666 2_667 ?
O4 Si2 Si2 126.4(3) . 2_667 ?
O8 Si2 Si2 143.8(3) 1_655 2_667 ?
O2 Si2 Si2 86.2(3) . 2_667 ?
O7 Si2 Si2 39.3(3) 2_666 2_667 ?
Si1 Si2 Si2 168.69(19) 2_666 2_667 ?
O7 Si2 Si1 131.1(3) 1_556 . ?
O6 Si2 Si1 128.8(3) 2_666 . ?
O4 Si2 Si1 40.8(3) . . ?
O8 Si2 Si1 89.5(3) 1_655 . ?
O2 Si2 Si1 41.2(3) . . ?
O7 Si2 Si1 81.0(3) 2_666 . ?
Si1 Si2 Si1 62.09(15) 2_666 . ?
Si2 Si2 Si1 108.01(18) 2_667 . ?
O7 Si2 Ca1 120.9(3) 1_556 . ?
O6 Si2 Ca1 50.7(2) 2_666 . ?
O4 Si2 Ca1 57.2(3) . . ?
O8 Si2 Ca1 127.1(3) 1_655 . ?
O2 Si2 Ca1 120.3(2) . . ?
O7 Si2 Ca1 55.9(3) 2_666 . ?
Si1 Si2 Ca1 87.62(14) 2_666 . ?
Si2 Si2 Ca1 86.26(14) 2_667 . ?
Si1 Si2 Ca1 86.70(13) . . ?
B2 O1 Si1 128.7(8) 2_656 . ?
B2 O1 Ca1 89.4(6) 2_656 2_566 ?
Si1 O1 Ca1 92.6(3) . 2_566 ?
B2 O1 Ca1 143.0(7) 2_656 1_545 ?
Si1 O1 Ca1 87.6(3) . 1_545 ?
Ca1 O1 Ca1 96.1(3) 2_566 1_545 ?
B2 O2 Si1 125.8(7) . . ?
B2 O2 Si2 125.2(6) . . ?
Si1 O2 Si2 94.9(4) . . ?
B2 O2 Ca1 87.5(6) . 1_545 ?
Si1 O2 Ca1 87.5(3) . 1_545 ?
Si2 O2 Ca1 134.2(4) . 1_545 ?
B1 O3 Si1 130.6(7) 2_566 . ?
B1 O3 Ca1 87.9(6) 2_566 1_545 ?
Si1 O3 Ca1 90.5(3) . 1_545 ?
B1 O3 Ca1 141.1(7) 2_566 2_566 ?
Si1 O3 Ca1 88.3(3) . 2_566 ?
Ca1 O3 Ca1 95.0(2) 1_545 2_566 ?
Si2 O4 Si1 99.0(4) . . ?
Si2 O4 Si1 96.0(4) . 2_666 ?
Si1 O4 Si1 100.3(4) . 2_666 ?
Si2 O4 Ca1 88.4(3) . . ?
Si1 O4 Ca1 129.6(4) . . ?
Si1 O4 Ca1 128.6(4) 2_666 . ?
B1 O5 B2 111.9(9) . 2_666 ?
B1 O5 Ca1 90.8(6) . 2_576 ?
B2 O5 Ca1 91.3(6) 2_666 2_576 ?
B1 O5 Ca1 146.2(6) . 1_554 ?
B2 O5 Ca1 89.1(7) 2_666 1_554 ?
Ca1 O5 Ca1 115.8(3) 2_576 1_554 ?
B2 O6 Si2 125.3(7) 2_656 2_666 ?
B2 O6 Ca1 94.0(6) 2_656 2_666 ?
Si2 O6 Ca1 95.7(3) 2_666 2_666 ?
B2 O6 Ca1 95.8(6) 2_656 1_544 ?
Si2 O6 Ca1 126.1(4) 2_666 1_544 ?
Ca1 O6 Ca1 116.7(3) 2_666 1_544 ?
B1 O7 Si2 121.4(8) 1_655 1_554 ?
B1 O7 Si2 127.5(7) 1_655 2_666 ?
Si2 O7 Si2 96.5(4) 1_554 2_666 ?
B1 O7 Ca1 89.5(6) 1_655 2_666 ?
Si2 O7 Ca1 134.5(4) 1_554 2_666 ?
Si2 O7 Ca1 87.0(3) 2_666 2_666 ?
B1 O8 Si2 123.0(7) 2_566 1_455 ?
B1 O8 Si1 126.4(7) 2_566 2_566 ?
Si2 O8 Si1 92.7(4) 1_455 2_566 ?
B1 O8 Ca1 95.8(6) 2_566 . ?
Si2 O8 Ca1 128.6(4) 1_455 . ?
Si1 O8 Ca1 88.3(3) 2_566 . ?
O3 B1 O5 112.6(9) 2_566 . ?
O3 B1 O8 112.0(9) 2_566 2_566 ?
O5 B1 O8 110.5(10) . 2_566 ?
O3 B1 O7 108.6(10) 2_566 1_455 ?
O5 B1 O7 107.4(9) . 1_455 ?
O8 B1 O7 105.3(7) 2_566 1_455 ?
O3 B1 Ca1 62.4(5) 2_566 2_576 ?
O5 B1 Ca1 58.4(5) . 2_576 ?
O8 B1 Ca1 157.8(7) 2_566 2_576 ?
O7 B1 Ca1 96.7(6) 1_455 2_576 ?
O3 B1 Ca1 100.6(7) 2_566 2_566 ?
O5 B1 Ca1 146.8(8) . 2_566 ?
O8 B1 Ca1 54.5(5) 2_566 2_566 ?
O7 B1 Ca1 58.4(5) 1_455 2_566 ?
Ca1 B1 Ca1 145.4(5) 2_576 2_566 ?
O1 B2 O5 108.9(9) 2_656 2_666 ?
O1 B2 O6 112.2(9) 2_656 2_656 ?
O5 B2 O6 110.5(10) 2_666 2_656 ?
O1 B2 O2 112.6(9) 2_656 . ?
O5 B2 O2 104.2(8) 2_666 . ?
O6 B2 O2 108.2(9) 2_656 . ?
O1 B2 Ca1 60.4(5) 2_656 1_645 ?
O5 B2 Ca1 57.9(5) 2_666 1_645 ?
O6 B2 Ca1 100.7(7) 2_656 1_645 ?
O2 B2 Ca1 150.3(8) . 1_645 ?
O1 B2 Ca1 104.6(6) 2_656 1_545 ?
O5 B2 Ca1 146.4(8) 2_666 1_545 ?
O6 B2 Ca1 55.4(5) 2_656 1_545 ?
O2 B2 Ca1 60.9(5) . 1_545 ?
Ca1 B2 Ca1 147.0(5) 1_645 1_545 ?
O1 B2 Ca1 150.6(8) 2_656 2_667 ?
O5 B2 Ca1 61.6(6) 2_666 2_667 ?
O6 B2 Ca1 54.9(5) 2_656 2_667 ?
O2 B2 Ca1 96.8(6) . 2_667 ?
Ca1 B2 Ca1 94.1(4) 1_645 2_667 ?
Ca1 B2 Ca1 89.0(4) 1_545 2_667 ?
 
_refine_diff_density_max    0.763
_refine_diff_density_min   -0.809
_refine_diff_density_rms    0.228



 
data_danburite-IV_32.3GPa
_database_code_depnum_ccdc_archive 'CCDC 1562976'
 

_publ_requested_journal           'International Union of Crystallography' 

_publ_contact_author_name        'Anna Pakhomova'
_publ_contact_author_address     
;Deutsches Elektronen-Synchrotron (DESY)
Notkestrasse 85
22607 Hamburg
Germany
;
_publ_contact_author_email       anna.pakhomova@desy.de
_publ_contact_author_phone       00494089985457
loop_
_publ_author_name
_publ_author_address
'Pakhomova, Anna'
;Deutsches Elektronen-Synchrotron (DESY)
Notkestrasse 85
22607 Hamburg
Germany
;
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         danburite
_chemical_name_common             danburite
_chemical_melting_point           ?
_chemical_formula_moiety          'B2 Ca1 O8 Si2' 
_chemical_formula_sum
 'B4 Ca2 O16 Si4' 
_chemical_formula_weight          491.76

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'B'  'B'  -0.0005   0.0001
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'  -0.0010   0.0008
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Si'  'Si'   0.0083   0.0108
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ca'  'Ca'   0.0425   0.0513
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    7.9989(17)
_cell_length_b                    7.8697(14)
_cell_length_c                    6.249(3)
_cell_angle_alpha                 90
_cell_angle_beta                  89.75(3)
_cell_angle_gamma                 90
_cell_volume                      393.4(2)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_pressure        32300000
_cell_measurement_reflns_used     326
_cell_measurement_theta_min       1.6950
_cell_measurement_theta_max       10.4260
 
_exptl_crystal_description        'plate crystal'
_exptl_crystal_colour             colorless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     4.152          
_exptl_crystal_F_000              488
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.020
_exptl_crystal_size_mid           0.015
_exptl_crystal_size_min           0.010
_exptl_absorpt_coefficient_mu     0.221
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_ambient_pressure          32300000
_diffrn_radiation_wavelength      0.29024
_diffrn_radiation_type            synchrotron
_diffrn_source                    synchrotron
_diffrn_source_type              'PETRA III, Beamline P02.2'
_diffrn_measurement_device_type   'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             940
_diffrn_reflns_av_unetI/netI      0.0587
_diffrn_reflns_av_R_equivalents   0.0536
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -6
_diffrn_reflns_limit_l_max        6
_diffrn_reflns_theta_min          1.701
_diffrn_reflns_theta_max          10.458
_diffrn_reflns_theta_full         10.040
_diffrn_measured_fraction_theta_max   0.657
_diffrn_measured_fraction_theta_full  0.663
_diffrn_reflns_Laue_measured_fraction_max    0.657
_diffrn_reflns_Laue_measured_fraction_full   0.663
_diffrn_reflns_point_group_measured_fraction_max   0.657
_diffrn_reflns_point_group_measured_fraction_full  0.663
_reflns_number_total              524
_reflns_number_gt                 408
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction         
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution     'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1924P)²+3.6413P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          524
_refine_ls_number_parameters      68
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1252
_refine_ls_R_factor_gt            0.0979
_refine_ls_wR_factor_ref          0.3095
_refine_ls_wR_factor_gt           0.2941
_refine_ls_goodness_of_fit_ref    1.175
_refine_ls_restrained_S_all       1.175
_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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ca1 Ca 0.7504(3) 0.1112(3) 0.7465(4) 0.0245(11) Uani 1 1 d . . . . .
Si1 Si 0.0746(4) 0.2356(4) 0.0072(6) 0.0231(12) Uani 1 1 d . . . . .
Si2 Si 0.4261(4) 0.2350(4) 0.0072(6) 0.0232(12) Uani 1 1 d . . . . .
O1 O 0.5962(11) 0.1336(10) 0.0670(16) 0.0249(19) Uiso 1 1 d . . . . .
O2 O -0.0958(11) 0.1343(10) 0.0663(16) 0.026(2) Uiso 1 1 d . . . . .
O3 O 0.7492(12) 0.0931(10) 0.3777(17) 0.029(2) Uiso 1 1 d . . . . .
O4 O 0.2490(11) 0.1500(10) 0.0633(16) 0.0246(18) Uiso 1 1 d . . . . .
O5 O 0.4245(11) 0.3625(11) 0.2490(17) 0.027(2) Uiso 1 1 d . . . . .
O6 O 0.0746(11) 0.1369(11) -0.2515(17) 0.0258(19) Uiso 1 1 d . . . . .
O7 O 0.4417(10) 0.4091(10) -0.1258(16) 0.024(2) Uiso 1 1 d . . . . .
O8 O 0.0587(10) 0.4087(10) -0.1263(16) 0.025(2) Uiso 1 1 d . . . . .
B1 B 0.5951(16) 0.0457(17) 0.269(2) 0.026(3) Uiso 1 1 d . . . . .
B2 B -0.0939(16) 0.0468(18) 0.272(3) 0.029(3) Uiso 1 1 d . . . . .
 
 
_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
Ca1 O3 2.309(11) . ?
Ca1 O8 2.329(8) 2_645 ?
Ca1 O7 2.339(9) 2_645 ?
Ca1 O1 2.354(9) 1_556 ?
Ca1 O2 2.358(11) 1_656 ?
Ca1 O4 2.375(9) 3_656 ?
Ca1 O3 2.468(9) 4_566 ?
Ca1 O6 2.601(9) 1_656 ?
Ca1 O2 2.604(8) 4_666 ?
Ca1 O1 2.613(9) 4_566 ?
Ca1 O5 2.615(9) 4_566 ?
Ca1 B2 2.971(14) 4_666 ?
Si1 O4 1.590(10) . ?
Si1 O8 1.603(9) . ?
Si1 O2 1.621(8) . ?
Si1 O6 1.794(11) . ?
Si1 O6 1.811(11) 4_566 ?
Si1 Si2 2.811(5) . ?
Si1 Ca1 3.221(5) 1_454 ?
Si1 Ca1 3.222(4) 4_465 ?
Si1 Ca1 3.435(4) 3_656 ?
Si1 Ca1 3.631(4) 2_655 ?
Si2 O4 1.603(9) . ?
Si2 O7 1.607(9) . ?
Si2 O1 1.623(9) . ?
Si2 O5 1.787(11) 4_565 ?
Si2 O5 1.813(11) . ?
Si2 Ca1 3.209(4) 1_554 ?
Si2 Ca1 3.235(4) 4_565 ?
Si2 Ca1 3.430(4) 3_656 ?
O1 B1 1.438(17) . ?
O1 Ca1 2.354(9) 1_554 ?
O1 Ca1 2.613(9) 4_565 ?
O2 B2 1.457(18) . ?
O2 Ca1 2.358(11) 1_454 ?
O2 Ca1 2.604(8) 4_465 ?
O3 B1 1.459(18) . ?
O3 B2 1.463(15) 1_655 ?
O3 Ca1 2.468(9) 4_565 ?
O4 Ca1 2.375(9) 3_656 ?
O5 B1 1.454(15) 2_655 ?
O5 Si2 1.787(11) 4_566 ?
O5 Ca1 2.615(9) 4_565 ?
O6 B2 1.459(16) 3 ?
O6 Si1 1.811(11) 4_565 ?
O6 Ca1 2.601(9) 1_454 ?
O7 B1 1.435(14) 4_565 ?
O7 Ca1 2.339(9) 2_655 ?
O8 B2 1.423(18) 4_565 ?
O8 Ca1 2.329(8) 2_655 ?
B1 O7 1.435(14) 4_566 ?
B1 O5 1.454(15) 2_645 ?
B1 Ca1 2.976(14) 4_565 ?
B1 Ca1 3.029(13) 3_656 ?
B2 O8 1.423(18) 4_566 ?
B2 O6 1.459(16) 3 ?
B2 O3 1.463(15) 1_455 ?
B2 Ca1 2.971(14) 4_465 ?
B2 Ca1 3.017(14) 3_656 ?
B2 Ca1 3.253(15) 1_455 ?
 
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
O3 Ca1 O8 69.0(3) . 2_645 ?
O3 Ca1 O7 68.3(3) . 2_645 ?
O8 Ca1 O7 82.0(3) 2_645 2_645 ?
O3 Ca1 O1 148.1(3) . 1_556 ?
O8 Ca1 O1 131.7(3) 2_645 1_556 ?
O7 Ca1 O1 89.0(3) 2_645 1_556 ?
O3 Ca1 O2 148.8(3) . 1_656 ?
O8 Ca1 O2 89.0(3) 2_645 1_656 ?
O7 Ca1 O2 132.2(3) 2_645 1_656 ?
O1 Ca1 O2 63.0(3) 1_556 1_656 ?
O3 Ca1 O4 116.5(3) . 3_656 ?
O8 Ca1 O4 64.3(3) 2_645 3_656 ?
O7 Ca1 O4 64.9(3) 2_645 3_656 ?
O1 Ca1 O4 69.0(3) 1_556 3_656 ?
O2 Ca1 O4 68.9(3) 1_656 3_656 ?
O3 Ca1 O3 112.9(3) . 4_566 ?
O8 Ca1 O3 138.9(3) 2_645 4_566 ?
O7 Ca1 O3 138.3(3) 2_645 4_566 ?
O1 Ca1 O3 69.2(3) 1_556 4_566 ?
O2 Ca1 O3 69.3(3) 1_656 4_566 ?
O4 Ca1 O3 130.5(4) 3_656 4_566 ?
O3 Ca1 O6 91.0(3) . 1_656 ?
O8 Ca1 O6 53.3(3) 2_645 1_656 ?
O7 Ca1 O6 135.3(3) 2_645 1_656 ?
O1 Ca1 O6 120.6(3) 1_556 1_656 ?
O2 Ca1 O6 57.7(3) 1_656 1_656 ?
O4 Ca1 O6 93.5(3) 3_656 1_656 ?
O3 Ca1 O6 85.8(3) 4_566 1_656 ?
O3 Ca1 O2 67.7(3) . 4_666 ?
O8 Ca1 O2 94.5(3) 2_645 4_666 ?
O7 Ca1 O2 133.9(4) 2_645 4_666 ?
O1 Ca1 O2 123.7(3) 1_556 4_666 ?
O2 Ca1 O2 93.4(3) 1_656 4_666 ?
O4 Ca1 O2 151.7(3) 3_656 4_666 ?
O3 Ca1 O2 54.5(3) 4_566 4_666 ?
O6 Ca1 O2 58.2(3) 1_656 4_666 ?
O3 Ca1 O1 67.4(3) . 4_566 ?
O8 Ca1 O1 134.2(3) 2_645 4_566 ?
O7 Ca1 O1 94.2(3) 2_645 4_566 ?
O1 Ca1 O1 93.5(2) 1_556 4_566 ?
O2 Ca1 O1 123.6(3) 1_656 4_566 ?
O4 Ca1 O1 151.9(3) 3_656 4_566 ?
O3 Ca1 O1 54.3(3) 4_566 4_566 ?
O6 Ca1 O1 114.5(3) 1_656 4_566 ?
O2 Ca1 O1 56.4(2) 4_666 4_566 ?
O3 Ca1 O5 90.1(3) . 4_566 ?
O8 Ca1 O5 135.1(3) 2_645 4_566 ?
O7 Ca1 O5 53.1(3) 2_645 4_566 ?
O1 Ca1 O5 58.0(3) 1_556 4_566 ?
O2 Ca1 O5 120.8(3) 1_656 4_566 ?
O4 Ca1 O5 94.0(3) 3_656 4_566 ?
O3 Ca1 O5 85.4(3) 4_566 4_566 ?
O6 Ca1 O5 171.0(3) 1_656 4_566 ?
O2 Ca1 O5 114.2(3) 4_666 4_566 ?
O1 Ca1 O5 57.9(3) 4_566 4_566 ?
O3 Ca1 B2 96.5(4) . 4_666 ?
O8 Ca1 B2 111.3(3) 2_645 4_666 ?
O7 Ca1 B2 155.4(4) 2_645 4_666 ?
O1 Ca1 B2 96.0(3) 1_556 4_666 ?
O2 Ca1 B2 70.4(4) 1_656 4_666 ?
O4 Ca1 B2 139.1(4) 3_656 4_666 ?
O3 Ca1 B2 29.4(3) 4_566 4_666 ?
O6 Ca1 B2 60.7(3) 1_656 4_666 ?
O2 Ca1 B2 29.4(4) 4_666 4_666 ?
O1 Ca1 B2 61.6(4) 4_566 4_666 ?
O5 Ca1 B2 110.3(3) 4_566 4_666 ?
O4 Si1 O8 123.1(5) . . ?
O4 Si1 O2 118.6(5) . . ?
O8 Si1 O2 117.9(5) . . ?
O4 Si1 O6 91.1(5) . . ?
O8 Si1 O6 84.2(5) . . ?
O2 Si1 O6 89.4(5) . . ?
O4 Si1 O6 92.8(5) . 4_566 ?
O8 Si1 O6 87.9(5) . 4_566 ?
O2 Si1 O6 94.9(5) . 4_566 ?
O6 Si1 O6 172.0(4) . 4_566 ?
O4 Si1 Si2 28.4(3) . . ?
O8 Si1 Si2 94.8(3) . . ?
O2 Si1 Si2 147.1(4) . . ?
O6 Si1 Si2 90.2(3) . . ?
O6 Si1 Si2 89.8(3) 4_566 . ?
O4 Si1 Ca1 133.8(4) . 1_454 ?
O8 Si1 Ca1 85.9(4) . 1_454 ?
O2 Si1 Ca1 44.5(4) . 1_454 ?
O6 Si1 Ca1 53.8(3) . 1_454 ?
O6 Si1 Ca1 126.3(3) 4_566 1_454 ?
Si2 Si1 Ca1 143.79(15) . 1_454 ?
O4 Si1 Ca1 139.6(4) . 4_465 ?
O8 Si1 Ca1 81.8(3) . 4_465 ?
O2 Si1 Ca1 53.4(3) . 4_465 ?
O6 Si1 Ca1 125.3(3) . 4_465 ?
O6 Si1 Ca1 53.8(3) 4_566 4_465 ?
Si2 Si1 Ca1 143.46(15) . 4_465 ?
Ca1 Si1 Ca1 72.56(10) 1_454 4_465 ?
O4 Si1 Ca1 37.3(3) . 3_656 ?
O8 Si1 Ca1 160.4(3) . 3_656 ?
O2 Si1 Ca1 81.4(3) . 3_656 ?
O6 Si1 Ca1 93.5(3) . 3_656 ?
O6 Si1 Ca1 93.8(3) 4_566 3_656 ?
Si2 Si1 Ca1 65.74(11) . 3_656 ?
Ca1 Si1 Ca1 108.40(10) 1_454 3_656 ?
Ca1 Si1 Ca1 114.71(11) 4_465 3_656 ?
O4 Si1 Ca1 96.0(3) . 2_655 ?
O8 Si1 Ca1 27.4(3) . 2_655 ?
O2 Si1 Ca1 145.3(4) . 2_655 ?
O6 Si1 Ca1 87.7(3) . 2_655 ?
O6 Si1 Ca1 84.9(3) 4_566 2_655 ?
Si2 Si1 Ca1 67.53(10) . 2_655 ?
Ca1 Si1 Ca1 109.65(12) 1_454 2_655 ?
Ca1 Si1 Ca1 101.89(9) 4_465 2_655 ?
Ca1 Si1 Ca1 133.26(14) 3_656 2_655 ?
O4 Si2 O7 122.4(5) . . ?
O4 Si2 O1 119.0(5) . . ?
O7 Si2 O1 118.4(4) . . ?
O4 Si2 O5 90.5(5) . 4_565 ?
O7 Si2 O5 84.3(5) . 4_565 ?
O1 Si2 O5 90.3(5) . 4_565 ?
O4 Si2 O5 92.6(5) . . ?
O7 Si2 O5 87.7(5) . . ?
O1 Si2 O5 94.8(5) . . ?
O5 Si2 O5 171.8(4) 4_565 . ?
O4 Si2 Si1 28.2(3) . . ?
O7 Si2 Si1 94.3(3) . . ?
O1 Si2 Si1 147.2(3) . . ?
O5 Si2 Si1 89.4(3) 4_565 . ?
O5 Si2 Si1 89.8(3) . . ?
O4 Si2 Ca1 134.0(3) . 1_554 ?
O7 Si2 Ca1 86.3(3) . 1_554 ?
O1 Si2 Ca1 44.8(3) . 1_554 ?
O5 Si2 Ca1 54.5(3) 4_565 1_554 ?
O5 Si2 Ca1 126.4(3) . 1_554 ?
Si1 Si2 Ca1 143.77(16) . 1_554 ?
O4 Si2 Ca1 139.9(4) . 4_565 ?
O7 Si2 Ca1 81.9(4) . 4_565 ?
O1 Si2 Ca1 53.3(3) . 4_565 ?
O5 Si2 Ca1 125.9(3) 4_565 4_565 ?
O5 Si2 Ca1 53.9(3) . 4_565 ?
Si1 Si2 Ca1 143.46(15) . 4_565 ?
Ca1 Si2 Ca1 72.55(10) 1_554 4_565 ?
O4 Si2 Ca1 37.7(3) . 3_656 ?
O7 Si2 Ca1 160.1(3) . 3_656 ?
O1 Si2 Ca1 81.4(3) . 3_656 ?
O5 Si2 Ca1 93.4(3) 4_565 3_656 ?
O5 Si2 Ca1 93.7(3) . 3_656 ?
Si1 Si2 Ca1 65.91(10) . 3_656 ?
Ca1 Si2 Ca1 108.47(10) 1_554 3_656 ?
Ca1 Si2 Ca1 114.78(12) 4_565 3_656 ?
B1 O1 Si2 115.9(7) . . ?
B1 O1 Ca1 135.3(7) . 1_554 ?
Si2 O1 Ca1 106.1(5) . 1_554 ?
B1 O1 Ca1 89.7(7) . 4_565 ?
Si2 O1 Ca1 96.8(4) . 4_565 ?
Ca1 O1 Ca1 100.2(3) 1_554 4_565 ?
B2 O2 Si1 114.9(9) . . ?
B2 O2 Ca1 135.9(8) . 1_454 ?
Si1 O2 Ca1 106.6(5) . 1_454 ?
B2 O2 Ca1 89.4(7) . 4_465 ?
Si1 O2 Ca1 96.6(4) . 4_465 ?
Ca1 O2 Ca1 100.3(3) 1_454 4_465 ?
B1 O3 B2 116.8(11) . 1_655 ?
B1 O3 Ca1 119.2(8) . . ?
B2 O3 Ca1 117.4(9) 1_655 . ?
B1 O3 Ca1 95.1(7) . 4_565 ?
B2 O3 Ca1 94.7(7) 1_655 4_565 ?
Ca1 O3 Ca1 105.9(3) . 4_565 ?
Si1 O4 Si2 123.4(6) . . ?
Si1 O4 Ca1 118.7(4) . 3_656 ?
Si2 O4 Ca1 117.8(5) . 3_656 ?
B1 O5 Si2 119.7(9) 2_655 4_566 ?
B1 O5 Si2 119.0(9) 2_655 . ?
Si2 O5 Si2 121.0(5) 4_566 . ?
B1 O5 Ca1 91.7(6) 2_655 4_565 ?
Si2 O5 Ca1 91.6(4) 4_566 4_565 ?
Si2 O5 Ca1 92.0(3) . 4_565 ?
B2 O6 Si1 120.4(9) 3 . ?
B2 O6 Si1 118.5(9) 3 4_565 ?
Si1 O6 Si1 120.7(5) . 4_565 ?
B2 O6 Ca1 91.6(7) 3 1_454 ?
Si1 O6 Ca1 92.4(3) . 1_454 ?
Si1 O6 Ca1 92.0(4) 4_565 1_454 ?
B1 O7 Si2 120.9(8) 4_565 . ?
B1 O7 Ca1 104.2(7) 4_565 2_655 ?
Si2 O7 Ca1 134.2(4) . 2_655 ?
B2 O8 Si1 120.8(8) 4_565 . ?
B2 O8 Ca1 104.4(7) 4_565 2_655 ?
Si1 O8 Ca1 134.1(5) . 2_655 ?
O7 B1 O1 106.6(11) 4_566 . ?
O7 B1 O5 100.9(9) 4_566 2_645 ?
O1 B1 O5 114.2(12) . 2_645 ?
O7 B1 O3 116.4(12) 4_566 . ?
O1 B1 O3 106.5(10) . . ?
O5 B1 O3 112.4(11) 2_645 . ?
O7 B1 Ca1 98.8(7) 4_566 4_565 ?
O1 B1 Ca1 61.4(6) . 4_565 ?
O5 B1 Ca1 160.2(8) 2_645 4_565 ?
O3 B1 Ca1 55.7(6) . 4_565 ?
O7 B1 Ca1 48.5(6) 4_566 3_656 ?
O1 B1 Ca1 99.8(8) . 3_656 ?
O5 B1 Ca1 59.7(6) 2_645 3_656 ?
O3 B1 Ca1 153.1(9) . 3_656 ?
Ca1 B1 Ca1 138.5(5) 4_565 3_656 ?
O7 B1 Ca1 82.5(8) 4_566 . ?
O1 B1 Ca1 136.2(8) . . ?
O5 B1 Ca1 105.5(9) 2_645 . ?
O3 B1 Ca1 37.9(6) . . ?
Ca1 B1 Ca1 75.0(3) 4_565 . ?
Ca1 B1 Ca1 116.2(4) 3_656 . ?
O8 B2 O2 106.9(10) 4_566 . ?
O8 B2 O6 101.1(11) 4_566 3 ?
O2 B2 O6 113.2(12) . 3 ?
O8 B2 O3 118.1(12) 4_566 1_455 ?
O2 B2 O3 105.6(11) . 1_455 ?
O6 B2 O3 112.1(10) 3 1_455 ?
O8 B2 Ca1 99.3(8) 4_566 4_465 ?
O2 B2 Ca1 61.2(6) . 4_465 ?
O6 B2 Ca1 159.6(10) 3 4_465 ?
O3 B2 Ca1 55.9(6) 1_455 4_465 ?
O8 B2 Ca1 48.4(5) 4_566 3_656 ?
O2 B2 Ca1 100.1(7) . 3_656 ?
O6 B2 Ca1 59.5(6) 3 3_656 ?
O3 B2 Ca1 154.0(10) 1_455 3_656 ?
Ca1 B2 Ca1 138.9(5) 4_465 3_656 ?
O8 B2 Ca1 83.0(8) 4_566 1_455 ?
O2 B2 Ca1 136.4(8) . 1_455 ?
O6 B2 Ca1 105.8(8) 3 1_455 ?
O3 B2 Ca1 39.1(6) 1_455 1_455 ?
Ca1 B2 Ca1 75.4(3) 4_465 1_455 ?
Ca1 B2 Ca1 116.3(5) 3_656 1_455 ?
 
_refine_diff_density_max    1.185
_refine_diff_density_min   -0.983
_refine_diff_density_rms    0.296




