##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section B. It has been peer reviewed under the auspices  #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary may be obtained from        #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#           Copyright International Union of Crystallography                 #
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##############################################################################

data_global
_audit_creation_method     'form.cif (version 2.0)'
_journal_data_validation_number     ?
_journal_date_recd_electronic     2005-08-19
_journal_date_accepted     2006-05-16
_journal_name_full     'Acta Crystallographica, Section B'
_journal_year     2006
_journal_volume     62
_journal_issue      4
_journal_page_first     719
_journal_page_last     728
_journal_paper_category     FA
_journal_coeditor_code     LC5039
_publ_contact_author_name     'Dr. Michael Merz'
_publ_contact_author_address
;
Institut fr̈ Kristallographie
RWTH Aachen
Jg̈er Strasse 17-19
D-52066, Aachen
Germany
;
_publ_contact_author_email     merz@xtal.rwth-aachen.de
_publ_contact_author_fax     ' 49(241)8092184'
_publ_contact_author_phone     '49(241)8096988'
_publ_section_title
;
Structural phase transition and hydrogen ordering of
TlH₂PO₄ at low temperature
;
_publ_section_title_footnote
; ?
;
loop_
    _publ_author_name
    _publ_author_address
    'Oh, I.H.'
;Institut fur̈ Kristallographie
RWTH Aachen
Jag̈erstrasse 17-19
D-52056, Aachen
Germany
;
    'Merz, M.'
;Institut fur̈ Kristallographie
RWTH Aachen
Jag̈erstrasse 17-19
D-52056, Aachen
Germany
;
    'Mattauch, S.'
;Institut fur̈ Festkor̈perforschung
Forschungszentrum Jul̈ich
D-52425, Jul̈ich
Germany
;
    'Heger, G.'
;Institut fur̈ Kristallographie
RWTH Aachen
Jag̈erstrasse 17-19
D-52056, Aachen
Germany
;
data_TDP298K
_audit_creation_method     enCIFer
_chemical_formula_sum     ' H2 O4 P Tl'
_chemical_formula_weight     301.6
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/a'
_symmetry_space_group_name_Hall     '-P 2yab'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x+1/2, y+1/2, -z'
    '-x, -y, -z'
    'x+1/2, -y-1/2, z'
_cell_length_a     14.331(7)
_cell_length_b     4.535(2)
_cell_length_c     6.514(3)
_cell_angle_alpha     90
_cell_angle_beta     91.67(2)
_cell_angle_gamma     90
_cell_volume     423.2(3)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     20
_cell_measurement_theta_min     17.5
_cell_measurement_theta_max     22.5
_cell_measurement_temperature     298
_exptl_crystal_description     platelet
_exptl_crystal_colour     colourless
_exptl_crystal_size_max     5
_exptl_crystal_size_mid     3
_exptl_crystal_size_min     3
_exptl_crystal_density_diffrn     4.753
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_F_000     119
_exptl_absorpt_coefficient_mu     0.04
_exptl_absorpt_correction_type     none
_diffrn_ambient_temperature     '298K '
_diffrn_radiation_type     neutron
_diffrn_radiation_wavelength     1.2413
_diffrn_radiation_monochromator     'Cu (200)'
_diffrn_measurement_device_type     'four circle diffractometer'
_diffrn_measurement_method     'ω'
_diffrn_reflns_number     2766
_diffrn_reflns_av_R_equivalents     0.0218
_diffrn_reflns_theta_min     1.5
_diffrn_reflns_theta_max     50.992
_diffrn_measured_fraction_theta_max     0.6207
_diffrn_reflns_limit_h_min     -17
_diffrn_reflns_limit_h_max     17
_diffrn_reflns_limit_k_min     -5
_diffrn_reflns_limit_k_max     4
_diffrn_reflns_limit_l_min     -8
_diffrn_reflns_limit_l_max     6
_diffrn_standards_number     3
_diffrn_standards_interval_time     360
_diffrn_standards_decay_%     0.7
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
    -2 2 2
    4 2 0
    6 0 2
_reflns_number_total     814
_reflns_number_gt     699
_reflns_threshold_expression     >3sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_gt     0.051
_refine_ls_wR_factor_ref     0.0603
_refine_ls_goodness_of_fit_ref     3.90
_refine_ls_number_reflns     699
_refine_ls_number_parameters     73
_refine_ls_hydrogen_treatment     refall
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details     'w=1/σ²(Fo²)'
_refine_ls_shift/su_max     0
_refine_ls_shift/su_mean     0
_refine_diff_density_max     0.65
_refine_diff_density_min     -0.42
_refine_ls_extinction_method
                     'secondary Type I, isotropic, Gaussian (Zachariasen, 1967)'
_refine_ls_extinction_coef     0.05425
loop_
    _atom_type_symbol
    'H'
    'TL'
    'P'
    'O'
_atom_type_scat_source     International_Tables_Vol_C
_computing_data_collection     'pron'
_computing_cell_refinement     'pron'
_computing_data_reduction     'pron'
_computing_structure_refinement     'prometheus(Zucker et al.,1983)'
_computing_molecular_graphics     'drawxtal(Finger and Kroeker, 2004)'
loop_
    _atom_site_type_symbol
    _atom_site_label
    _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
    Tl Tl 0.12833(5) -0.0049(2) 0.25850(10)
                                          0.0389(3) Uani 1.00
    P P 0.12455(8) 0.5207(3) 0.7608(2) 0.0237(4) Uani 1.00
    O O1 0.07470(10) 0.3996(4) 0.9468(2) 0.0526(7) Uani 1.00
    O O2 0.05391(10) 0.6547(3) 0.6063(2) 0.0417(6) Uani 1.00
    O O3 0.19149(10) 0.7704(3) 0.8299(2) 0.0353(6) Uani 1.00
    O O4 0.18173(10) 0.2726(3) 0.6680(2) 0.0340(5) Uani 1.00
    H H1 -0.0088(5) 0.5245(18) 0.0161(11) 0.0419(7) Uiso 0.50
    H H2 0.0078(4) 0.5308(15) 0.5232(9) 0.0382(6) Uiso 0.50
    H H3 0.1845(2) 0.0052(7) 0.7544(4) 0.0516(7) Uani 1.00
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Tl 0.0392(2) 0.0397(3) 0.0379(3) . . 0.0083(2)
    P 0.0230(3) 0.0219(5) 0.0265(4) . . 0.0051(3)
    O1 0.0402(6) 0.0623(7) 0.0553(6) 0.0244(5) 0.0259(4) 0.0359(5)
    O2 0.0410(5) 0.0359(5) 0.0469(5) -0.0097(4) -0.0200(4) 0.0139(4)
    O3 0.0391(5) 0.0239(5) 0.0423(5) -0.0148(3) 0.0024(3) -0.0037(4)
    O4 0.0421(5) 0.0240(5) 0.0366(5) -0.0028(3) 0.0113(3) -0.0044(4)
    H3 0.0408(7) 0.0680(10)
                          0.0460(9) -0.0062(8) . -0.0150(10)
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_1
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    P O1 . . 1.527(2) ?
    P O2 . . 1.532(2) ?
    P O3 . . 1.543(2) ?
    P O4 . . 1.527(2) ?
    Tl O1 . 9 2.828(5) ?
    Tl O4 . 13 2.931(2) ?
    Tl O3 . 13 2.939(7) ?
    Tl O2 . 10 2.965(3) ?
    Tl O4 . . 3.028(5) ?
    Tl O3 . 12 3.133(5) ?
    Tl O2 . 7 3.201(5) ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_2
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1 P O2 . . . 110.39(3) ?
    O1 P O3 . . . 109.50(2) ?
    O1 P O4 . . . 108.55(2) ?
    O2 P O3 . . . 107.08(2) ?
    O2 P O4 . . . 112.60(4) ?
    O3 P O4 . . . 108.67(3) ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_D
    _geom_hbond_site_symmetry_H
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    O1 H1 O1 9 . 7 1.040(7) 1.409(7) 2.445(7) 172.8(4) ?
    O2 H2 O2 . . 7 1.012(6) 1.469(6) 2.480(6) 176.2(5) ?
    O3 H3 O4 10 . . 1.176(3) 1.337(3) 2.512(3) 176.9(5) ?
data_TDP240K
_audit_creation_method     enCIFer
_chemical_formula_sum     ' H2 O4 P Tl'
_chemical_formula_weight     301.6
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/a'
_symmetry_space_group_name_Hall     '-P 2yab'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x+1/2, y+1/2, -z'
    '-x, -y, -z'
    'x+1/2, -y-1/2, z'
_cell_length_a     14.26(2)
_cell_length_b     4.517(9)
_cell_length_c     6.497(10)
_cell_angle_alpha     90
_cell_angle_beta     92.19(13)
_cell_angle_gamma     90
_cell_volume     418.2(11)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     12
_cell_measurement_theta_min     17.5
_cell_measurement_theta_max     22.5
_cell_measurement_temperature     240
_exptl_crystal_description     platelet
_exptl_crystal_colour     colourless
_exptl_crystal_size_max     5
_exptl_crystal_size_mid     3
_exptl_crystal_size_min     3
_exptl_crystal_density_diffrn     4.753
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_F_000     118.6
_exptl_absorpt_coefficient_mu     0.04
_exptl_absorpt_correction_type     none
_diffrn_ambient_temperature     '240K '
_diffrn_radiation_type     neutron
_diffrn_radiation_wavelength     0.8724
_diffrn_radiation_monochromator     'Cu (220)'
_diffrn_measurement_device_type     'four circle diffractometer'
_diffrn_measurement_method     'ω'
_diffrn_reflns_number     1695
_diffrn_reflns_av_R_equivalents     0.0207
_diffrn_reflns_theta_min     3.51
_diffrn_reflns_theta_max     37.47
_diffrn_measured_fraction_theta_max     0.6974
_diffrn_reflns_limit_h_min     -19
_diffrn_reflns_limit_h_max     19
_diffrn_reflns_limit_k_min     -6
_diffrn_reflns_limit_k_max     4
_diffrn_reflns_limit_l_min     -9
_diffrn_reflns_limit_l_max     8
_diffrn_standards_number     2
_diffrn_standards_interval_time     540
_diffrn_standards_decay_%     0.7
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
    8 2 0
    8 0 2
_reflns_number_total     845
_reflns_number_gt     630
_reflns_threshold_expression     >3sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_gt     0.0458
_refine_ls_wR_factor_ref     0.0544
_refine_ls_goodness_of_fit_ref     2.21
_refine_ls_number_reflns     699
_refine_ls_number_parameters     73
_refine_ls_hydrogen_treatment     refall
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details     'w=1/σ²(Fo²)'
_refine_ls_shift/su_max     0
_refine_ls_shift/su_mean     0
_refine_diff_density_max     0.51
_refine_diff_density_min     -0.48
_refine_ls_extinction_method
                     'secondary Type I, isotropic, Gaussian (Zachariasen, 1967)'
_refine_ls_extinction_coef     0.05425
loop_
    _atom_type_symbol
    'H'
    'TL'
    'P'
    'O'
_atom_type_scat_source     International_Tables_Vol_C
_computing_data_collection     'pron'
_computing_cell_refinement     'pron'
_computing_data_reduction     'pron'
_computing_structure_refinement     'prometheus(Zucker et al.,1983)'
_computing_molecular_graphics     'drawxtal(Finger and Kroeker, 2004)'
loop_
    _atom_site_type_symbol
    _atom_site_label
    _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
    Tl Tl 0.12833(7) -0.0075(4) 0.2603(2) 0.0309(3) Uani 1.00
    P P 0.12432(10) 0.5238(5) 0.7633(2) 0.0178(5) Uani 1.00
    O O1 0.07640(10)
                   0.4034(6) 0.9526(3) 0.0392(7) Uani 1.00
    O O2 0.05160(10)
                   0.6604(5) 0.6104(3) 0.0304(7) Uani 1.00
    O O3 0.19250(10)
                   0.7757(6) 0.8310(3) 0.0284(7) Uani 1.00
    O O4 0.18020(10)
                   0.2764(5) 0.6662(3) 0.0262(7) Uani 1.00
    H H1 -0.0097(5) 0.526(2)   0.0162(11) 0.0310(10)
                                                   Uiso 0.50
    H H2 0.0067(5) 0.534(2)   0.5249(9) 0.0320(10)
                                                 Uiso 0.50
    H H3 0.1847(2) 0.0057(13) 0.7562(5) 0.042(3) Uani 1.00
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Tl 0.0314(4) 0.0283(12) 0.0334(5) . . 0.0066(6)
    P 0.0179(5) 0.0141(15) 0.0216(6) . 0.0011(4) 0.0031(7)
    O1 0.0292(7) 0.050(2)   0.0403(8) 0.0175(7) 0.0179(6) 0.0268(8)
    O2 0.0289(7) 0.0270(19) 0.0339(8) -0.0046(7) -0.0120(5) 0.0093(8)
    O3 0.0307(8) 0.018(2)   0.0355(8) . -0.0122(5) -0.0034(7)
    O4 0.0313(7) 0.0169(18) 0.0307(7) . 0.0083(5) -0.0036(7)
    H3 0.0340(10)
                0.048(4) 0.0420(10)
                                  . . -0.0130(10)
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_1
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    P O1 . . 1.529(3) ?
    P O2 . . 1.538(3) ?
    P O3 . . 1.549(3) ?
    P O4 . . 1.523(3) ?
    Tl O1 . 9 2.806(7) ?
    Tl O4 . 13 2.920(4) ?
    Tl O3 . 13 2.936(2) ?
    Tl O2 . 10 2.970(7) ?
    Tl O4 . . 2.999(5) ?
    Tl O3 . 12 3.127(8) ?
    Tl O2 . 7 3.146(2) ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_2
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1 P O2 . . . 110.55(5) ?
    O1 P O3 . . . 109.13(3) ?
    O1 P O4 . . . 109.21(3) ?
    O2 P O3 . . . 106.79(3) ?
    O2 P O4 . . . 112.18(5) ?
    O3 P O4 . . . 108.88(4) ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_D
    _geom_hbond_site_symmetry_H
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    O1 H1 O1 9 . 7 1.032(7) 1.422(7) 2.448(7) 172.3(4) ?
    O2 H2 O2 . . 7 1.010(8) 1.475(9) 2.483(8) 174.9(6) ?
    O3 H3 O4 10 . . 1.150(6) 1.356(6) 2.506(6) 177.2(4) ?
data_TDP210K
_audit_creation_method     enCIFer
_chemical_formula_sum     ' H8 O16 P4 Tl4'
_chemical_formula_weight     1206.4
_symmetry_cell_setting     triclinic
_symmetry_space_group_name_H-M     'C-1'
_symmetry_space_group_name_Hall     '-C 1'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, -y, -z'
    'x+1/2, y+1/2, z'
    '-x+1/2, -y+1/2, -z'
_cell_length_a     28.483(12)
_cell_length_b     9.016(5)
_cell_length_c     6.502(3)
_cell_angle_alpha     90.09(5)
_cell_angle_beta     92.21(3)
_cell_angle_gamma     90.49(3)
_cell_volume     1668.4(14)
_cell_formula_units_Z     16
_cell_measurement_reflns_used     12
_cell_measurement_theta_min     17.5
_cell_measurement_theta_max     22.5
_cell_measurement_temperature     210
_exptl_crystal_description     platelet
_exptl_crystal_colour     colourless
_exptl_crystal_size_max     5
_exptl_crystal_size_mid     3
_exptl_crystal_size_min     3
_exptl_crystal_density_diffrn     4.820
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_F_000     474.3
_exptl_absorpt_coefficient_mu     0.04
_exptl_absorpt_correction_type     none
_diffrn_ambient_temperature     '210K '
_diffrn_radiation_type     neutron
_diffrn_radiation_wavelength     0.8724
_diffrn_radiation_monochromator     'Cu (220)'
_diffrn_measurement_device_type     'four circle diffractometer'
_diffrn_measurement_method     'ω'
_diffrn_reflns_number     3170
_diffrn_reflns_av_R_equivalents     0.0621
_diffrn_reflns_theta_min     3.51
_diffrn_reflns_theta_max     37.80
_diffrn_measured_fraction_theta_max     0.7025
_diffrn_reflns_limit_h_min     -40
_diffrn_reflns_limit_h_max     38
_diffrn_reflns_limit_k_min     -12
_diffrn_reflns_limit_k_max     8
_diffrn_reflns_limit_l_min     -8
_diffrn_reflns_limit_l_max     9
_diffrn_standards_number     2
_diffrn_standards_interval_time     540
_diffrn_standards_decay_%     2.5
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
    0 0 2
    12 0 -1
_reflns_number_total     2982
_reflns_number_gt     1428
_reflns_threshold_expression     >2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_gt     0.0458
_refine_ls_wR_factor_ref     0.0544
_refine_ls_goodness_of_fit_ref     1.933
_refine_ls_number_reflns     2982
_refine_ls_number_parameters     131
_refine_ls_hydrogen_treatment     refall
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details     'w=1/σ²(Fo²)'
_refine_ls_shift/su_max     0
_refine_ls_shift/su_mean     0
_refine_diff_density_max     3.03
_refine_diff_density_min     -2.28
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef     0.00300(15)
loop_
    _atom_type_symbol
    'H'
    'TL'
    'P'
    'O'
_atom_type_scat_source     International_Tables_Vol_C
_computing_data_collection     'pron'
_computing_cell_refinement     'pron'
_computing_data_reduction     'pron'
_computing_structure_refinement     'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'drawxtal(Finger and Kroeker, 2004)'
loop_
    _atom_site_type_symbol
    _atom_site_label
    _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
    Tl Tl1 0.0644(3) 0.4990(10)
                              0.2650(10)
                                       0.027(2) Uiso 1
    Tl Tl2 0.1883(2) 0.2490(10)
                              0.7270(10)
                                       0.029(2) Uiso 1
    Tl Tl3 0.0639(3) 0.9950(10)
                              0.2530(10)
                                       0.027(2) Uiso 1
    Tl Tl4 0.1838(2) 0.7440(10)
                              0.749(2) 0.029(2) Uiso 1
    P P1 0.0620(4) 0.261(2) 0.762(2) 0.016(2) Uiso 1
    P P2 0.1881(4) 0.013(2) 0.231(2) 0.020(3) Uiso 1
    P P3 0.0625(3) 0.761(2) 0.756(2) 0.013(2) Uiso 1
    P P4 0.1876(4) 0.512(2) 0.231(2) 0.015(2) Uiso 1
    O O1 0.0410(3) 0.2160(10)
                            0.9730(10)
                                     0.019(2) Uiso 1
    O O2 0.2148(4) 0.438(2) 0.064(2) 0.025(2) Uiso 1
    O O3 0.0348(3) 0.686(2) 0.934(2) 0.020(2) Uiso 1
    O O4 0.2092(3) 0.961(2) 0.032(2) 0.018(2) Uiso 1
    O O5 0.0290(4) 0.323(2) 0.594(2) 0.022(2) Uiso 1
    O O6 0.2263(4) 0.085(2)  374(2) 0.021(2) Uiso 1
    O O7 0.0266(4) 0.828(2) 0.603(2) 0.023(3) Uiso 1
    O O8 0.2266(4) 0.589(2) 0.375(2) 0.017(2) Uiso 1
    O O9 0.0999(3) 0.388(2) 0.812(2) 0.021(2) Uiso 1
    O O10 0.1509(4) 0.138(2) 0.181(2) 0.014(2) Uiso 1
    O O11 0.0936(4) 0.886(2) 0.845(2) 0.024(2) Uiso 1
    O O12 0.1571(3) 0.6360(10)
                             0.1540(10)
                                      0.014(2) Uiso 1
    O O13 0.0890(4) 0.138(2) 0.658(2) 0.014(2) Uiso 1
    O O14 0.1591(4) 0.389(2) 0.332(2) 0.022(3) Uiso 1
    O O15 0.0878(4) 0.640(2) 0.657(2) 0.019(2) Uiso 1
    O O16 0.1559(3) 0.888(2) 0.317(2) 0.025(2) Uiso 1
    H H1 0.9920(6) 0.267(3) 0.018(3) 0.048(4) Uiso 1
    H H2 0.2509(9) 1.001(4) -0.010(3) 0.010(3) Uiso 1
    H H3 0.9992(6) 0.254(3) 0.516(3) 0.023(2) Uiso 1
    H H4 0.2567(5) -0.018(2) 0.538(2) 0.037(4) Uiso 1
    H H5 0.1585(6) 0.775(2) 0.258(2) 0.030(4) Uiso 1
    H H6 0.4065(7) 0.507(3) 0.223(3) 0.038(5) Uiso 1
    H H7 0.3413(8) 0.243(4) 0.755(3) 0.038(4) Uiso 1
    H H8 0.4066(6) 0.012(3) 0.243(3) 0.029(4) Uiso 1
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_1
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    P1 O1 . . 1.57(2) ?
    P1 O5 . . 1.53(2) ?
    P1 O9 . . 1.59(2) ?
    P1 O13 . . 1.52(2) ?
    P2 O4 . 11 1.53(2) ?
    P2 O6 . . 1.54(2) ?
    P2 O10 . . 1.58(2) ?
    P2 O16 . 11 1.57(2) ?
    P3 O3 . . 1.58(2) ?
    P3 O7 . . 1.53(2) ?
    P3 O11 . . 1.53(2) ?
    P3 O15 . . 1.47(2) ?
    P4 O2 . . 1.52(2) ?
    P4 O8 . . 1.58(2) ?
    P4 O12 . . 1.50(2) ?
    P4 O14 . . 1.53(2) ?
    Tl1 O3 . 9 2.850(10)
                       ?
    Tl1 O5 . . 2.870(10)
                       ?
    Tl1 O14 . . 2.90(2) ?
    Tl1 O15 . . 2.90(2) ?
    Tl1 O12 . . 3.020(10)
                        ?
    Tl1 O1 . 9 3.23(2) ?
    Tl2 O2 9 . 2.85(2) ?
    Tl2 O9 . . 2.900(10)
                       ?
    Tl2 O6 . 7 2.94(2) ?
    Tl2 O14 . . 2.96(2) ?
    Tl2 O6 . . 2.97(2) ?
    Tl2 O13 . . 3.010(10)
                        ?
    Tl3 O1 . 10 2.76(3) ?
    Tl3 O16 . . 2.820(10)
                        ?
    Tl3 O10 . 17 2.840(10)
                         ?
    Tl3 O7 . . 2.96(2) ?
    Tl3 O11 . 9 2.99(2) ?
    Tl3 O13 . 17 2.99(2) ?
    Tl3 O7 . 14 3.21(2) ?
    Tl4 O4 9 . 2.75(2) ?
    Tl4 O15 . . 2.930(10)
                        ?
    Tl4 O12 9 . 2.940(10)
                        ?
    Tl4 O11 . . 2.97(2) ?
    Tl4 O8 . 8 3.090(10)
                       ?
    Tl4 O8 . . 3.100(10)
                       ?
    Tl4 O16 . . 3.170(10)
                        ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_2
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1 P1 O9 . . . 105.7(9) ?
    O1 P1 O5 . . . 118.3(9) ?
    O1 P1 O13 . . . 114.7(9) ?
    O5 P1 O9 . . . 106.5(9) ?
    O5 P1 O13 . . . 105.1(9) ?
    O4 P2 O6 11 . . 104.4(9) ?
    O4 P2 O10 11 . . 111.70(10)
                              ?
    O4 P2 O16 11 . 11 106.60(10)
                               ?
    O3 P3 O7 . . . 107.8(9) ?
    O3 P3 O11 . . . 109.4(9) ?
    O3 P3 O15 . . . 106.0(9) ?
    O7 P3 O11 . . . 107.9(9) ?
    O7 P3 O15 . . . 109.9(9) ?
    O11 P3 O15 . . . 115.2(9) ?
    O2 P4 O8 . . . 104.5(9) ?
    O2 P4 O12 . . . 113.8(9)
                            ?
    O2 P4 O14 . . . 106.3(9) ?
    O8 P4 O12 . . . 105.9(9) ?
    O8 P4 O14 . . . 115.2(9) ?
    O12 P4 O14 . . . 111.8(9) ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_D
    _geom_hbond_site_symmetry_H
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    O3 H1 O1 5 . 15 0.94(2) 1.51(2) 2.44(3) 167.5(2) ?
    O2 H2 O4 6 . . 1.18(3) 1.28(3) 2.450(10)
                                           167.4(9) ?
    O5 H3 O7 5 . 5 1.12(2) 1.30(3) 2.410(10)
                                           169.3(9) ?
    O8 H4 O6 7 . . 0.97(2) 1.64(2) 2.606(9) 173.1(9) ?
    O16 H5 O12 . . . 1.09(3) 1.42(3) 2.50(2) 170.9(9) ?
    O11 H6 O13 8 . 7 1.06(3) 1.52(3) 2.58(2) 172.6(3) ?
    O10 H7 O14 7 . 7 1.17(3) 1.32(2) 2.48(2) 168.8(6) ?
    O9 H8 O15 8 . 8 0.99(3) 1.53(3) 2.51(2) 173.9(2) ?
