#------------------------------------------------------------------------------
#$Date: 2026-04-05 14:01:25 +0200 (Sun 05 de Apr de 2026) $
#$Revision: 305357 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/02/7720243.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7720243
loop_
_publ_author_name
'Zhao, Zong-Jie'
'Yan, Yu-Zheng'
'Fu, Jia-Jian'
'Wu, Hong-Yan'
'Zhang, Jian-Han'
_publ_section_title
;
 Crystal structures and optical properties of two layered lead halide
 phosphites
 Pb₃(HPO₃)Cl₄·H₂O and
 Pb₃(HPO₃)₂Cl₂·H₂O.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4169
_journal_page_last               4180
_journal_paper_doi               10.1039/d5dt03075g
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'Cl2 H2 O6 P2 Pb3, 0.5(H4 O2)'
_chemical_formula_sum            'Cl2 H4 O7 P2 Pb3'
_chemical_formula_weight         870.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2026-01-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2026-01-28 deposited with the CCDC.	2026-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.808(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0370(3)
_cell_length_b                   5.4777(2)
_cell_length_c                   14.1283(5)
_cell_measurement_reflns_used    2275
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.1120
_cell_measurement_theta_min      2.8760
_cell_volume                     542.68(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -23.00   3.00   0.50    6.12    --   20.00  54.00 -90.00   52
  2  ω     12.00 110.00   0.50    6.12    --   20.00  54.00 -90.00  196
  3  ω    -71.00 110.00   0.50    6.12    --   20.00  54.00  30.00  362
  4  ω    -16.00   9.00   0.50    6.12    --   20.00  54.00-180.00   50
  5  ω     41.00  66.00   0.50    6.12    --   20.00  54.00-180.00   50
  6  ω     73.00 109.00   0.50    6.12    --   20.00  54.00-180.00   72
  7  ω    -35.00 -10.00   0.50    6.12    --   20.00  54.00 -30.00   50
  8  ω     43.00  68.00   0.50    6.12    --   20.00  54.00 -30.00   50
  9  ω    -17.00   8.00   0.50    6.12    --   20.00  54.00-120.00   50
 10  ω    -69.00 -40.00   0.50    6.12    --   20.00  54.00 -90.00   58
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3525
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.989
_diffrn_reflns_theta_max         24.989
_diffrn_reflns_theta_min         2.894
_exptl_absorpt_coefficient_mu    47.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    5.327
_exptl_crystal_description       needle
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.079
_refine_diff_density_min         -1.858
_refine_diff_density_rms         0.340
_refine_ls_extinction_coef       0.0034(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1059
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0247P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                957
_reflns_number_total             1059
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt03075g2.cif
_cod_data_source_block           20250624-g2-2
_cod_depositor_comments
'Adding full bibliography for 7720243--7720244.cif.'
_cod_database_code               7720243
_shelx_shelxl_version_number     2019/3
_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.
;
_shelx_estimated_absorpt_t_max   0.452
_shelx_estimated_absorpt_t_min   0.164
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All H(H) groups, All O(H) groups
2. Restrained distances
 P1-H1 = P2-H2
 1.3 with sigma of 0.02
 O5-H5B = O5-H5A
 0.85 with sigma of 0.02
 H5B-H5A
 1.4 with sigma of 0.02
3. Others
 Fixed Sof: H5A(0.5)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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
Pb3 Pb 0.09996(7) 1.250000 0.87235(4) 0.01557(19) Uani 1 2 d S T P . .
Pb1 Pb 0.64326(7) 0.750000 0.38987(4) 0.01726(19) Uani 1 2 d S T P . .
Pb2 Pb 0.81113(7) 0.750000 0.67663(4) 0.01627(19) Uani 1 2 d S T P . .
P1 P 0.8338(5) 0.250000 0.5295(2) 0.0091(7) Uani 1 2 d DS T P . .
Cl2 Cl -0.2747(5) 1.250000 0.7713(2) 0.0204(8) Uani 1 2 d S T P . .
P2 P 0.3510(5) 0.750000 0.7570(2) 0.0135(8) Uani 1 2 d DS T P . .
Cl1 Cl -0.0591(7) 0.750000 0.9125(3) 0.0372(11) Uani 1 2 d S T P . .
O2 O 0.7166(9) 0.4814(11) 0.5422(4) 0.0150(15) Uani 1 1 d . . . . .
O4 O 0.2285(9) 0.9821(12) 0.7520(4) 0.0221(17) Uani 1 1 d . . . . .
O3 O 0.4807(13) 0.750000 0.6780(6) 0.017(2) Uani 1 2 d S T P . .
O1 O 1.0152(13) 0.250000 0.5934(7) 0.021(2) Uani 1 2 d S T P . .
H1 H 0.879(18) 0.250000 0.442(3) 0.032 Uiso 1 2 d DS U P . .
H2 H 0.451(15) 0.750000 0.839(4) 0.02(3) Uiso 1 2 d DS . P . .
O5 O 0.473(2) 1.250000 0.9514(9) 0.055(4) Uani 1 2 d DS T P . .
H5A H 0.568(14) 1.33(3) 0.978(8) 0.03(7) Uiso 0.5 1 d D . P . .
H5B H 0.48(2) 1.250000 0.8914(18) 0.040 Uiso 1 2 d DS U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Cl2 Pb3 Cl2 0.00(7) . 4_585 ?
Cl2 Pb3 Cl1 75.92(9) 4_585 . ?
Cl2 Pb3 Cl1 75.92(9) . . ?
Cl2 Pb3 Cl1 75.92(9) 4_585 1_565 ?
Cl2 Pb3 Cl1 109.34(11) . 3_577 ?
Cl2 Pb3 Cl1 75.92(9) . 1_565 ?
Cl2 Pb3 Cl1 109.34(11) 4_585 3_577 ?
Cl1 Pb3 Cl1 75.43(8) . 3_577 ?
Cl1 Pb3 Cl1 129.33(15) . 1_565 ?
Cl1 Pb3 Cl1 75.43(8) 1_565 3_577 ?
O4 Pb3 Cl2 91.79(17) . . ?
O4 Pb3 Cl2 91.79(17) 4_585 4_585 ?
O4 Pb3 Cl2 91.79(17) 4_585 . ?
O4 Pb3 Cl2 91.79(17) . 4_585 ?
O4 Pb3 Cl1 138.48(16) . 3_577 ?
O4 Pb3 Cl1 138.48(16) 4_585 3_577 ?
O4 Pb3 Cl1 145.78(17) 4_585 . ?
O4 Pb3 Cl1 145.78(17) . 1_565 ?
O4 Pb3 Cl1 75.80(16) 4_585 1_565 ?
O4 Pb3 Cl1 75.80(16) . . ?
O4 Pb3 O4 72.8(3) 4_585 . ?
O2 Pb1 O2 68.2(3) . 4_575 ?
O2 Pb1 O4 104.44(19) . 2_646 ?
O2 Pb1 O4 104.44(19) 4_575 3_676 ?
O2 Pb1 O4 149.2(2) . 3_676 ?
O2 Pb1 O4 149.2(2) 4_575 2_646 ?
O4 Pb1 O4 65.9(3) 2_646 3_676 ?
O1 Pb1 O2 78.0(2) 3_766 4_575 ?
O1 Pb1 O2 78.0(2) 3_766 . ?
O1 Pb1 O4 71.2(2) 3_766 2_646 ?
O1 Pb1 O4 71.2(2) 3_766 3_676 ?
O2 Pb2 Cl2 143.84(15) 4_575 4_675 ?
O2 Pb2 Cl2 75.88(15) . 4_675 ?
O2 Pb2 O2 73.8(3) 4_575 . ?
O3 Pb2 Cl2 76.56(12) . 4_675 ?
O3 Pb2 O2 78.5(2) . . ?
O3 Pb2 O2 78.5(2) . 4_575 ?
O2 P1 O2 111.8(5) 4_565 . ?
O2 P1 H1 107(3) . . ?
O2 P1 H1 107(3) 4_565 . ?
O1 P1 O2 111.6(3) . . ?
O1 P1 O2 111.6(3) . 4_565 ?
O1 P1 H1 108(6) . . ?
Cl2 Cl2 Pb3 0(10) 4_585 . ?
O4 P2 O4 111.9(5) . 4_575 ?
O4 P2 H2 107(3) 4_575 . ?
O4 P2 H2 107(3) . . ?
O3 P2 O4 109.9(3) . 4_575 ?
O3 P2 O4 109.9(3) . . ?
O3 P2 H2 110(5) . . ?
Pb3 Cl1 Pb3 104.57(8) 1_545 3_577 ?
Pb3 Cl1 Pb3 104.57(8) . 3_577 ?
Pb3 Cl1 Pb3 129.33(15) 1_545 . ?
Pb2 O2 Pb1 108.7(2) . . ?
P1 O2 Pb1 116.0(3) . . ?
P1 O2 Pb2 118.3(3) . . ?
Pb3 O4 Pb1 110.6(2) . 3_676 ?
P2 O4 Pb3 134.1(4) . . ?
P2 O4 Pb1 105.3(3) . 3_676 ?
P2 O3 Pb2 132.6(6) . . ?
P1 O1 Pb1 148.8(6) . 3_766 ?
H5A O5 H5A 59(10) . 4_585 ?
H5A O5 H5B 111(4) . . ?
H5B O5 H5A 111(4) . 4_585 ?
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
Pb3 Cl2 2.891(4) . ?
Pb3 Cl2 2.891(4) 4_585 ?
Pb3 Cl1 3.0303(19) 1_565 ?
Pb3 Cl1 3.077(4) 3_577 ?
Pb3 Cl1 3.0303(19) . ?
Pb3 O4 2.474(6) . ?
Pb3 O4 2.474(6) 4_585 ?
Pb1 O2 2.622(6) . ?
Pb1 O2 2.622(6) 4_575 ?
Pb1 O4 2.700(6) 2_646 ?
Pb1 O4 2.700(6) 3_676 ?
Pb1 O1 2.395(9) 3_766 ?
Pb2 Cl2 3.1287(17) 4_675 ?
Pb2 O2 2.450(6) 4_575 ?
Pb2 O2 2.450(6) . ?
Pb2 O3 2.327(9) . ?
P1 O2 1.531(6) 4_565 ?
P1 O2 1.531(6) . ?
P1 O1 1.500(9) . ?
P1 H1 1.30(2) . ?
Cl2 Cl2 0.000(7) 4_585 ?
P2 O4 1.534(7) . ?
P2 O4 1.534(7) 4_575 ?
P2 O3 1.499(9) . ?
P2 H2 1.30(2) . ?
O5 H5A 0.85(2) . ?
O5 H5A 0.85(2) 4_585 ?
O5 H5B 0.85(2) . ?
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
O2 P1 O2 Pb1 -113.1(4) 4_565 . . . ?
O2 P1 O2 Pb2 114.9(4) 4_565 . . . ?
O2 P1 O1 Pb1 -117.0(3) . . . 3_766 ?
O2 P1 O1 Pb1 117.0(3) 4_565 . . 3_766 ?
O4 P2 O4 Pb3 92.3(6) 4_575 . . . ?
O4 P2 O4 Pb1 -127.1(3) 4_575 . . 3_676 ?
O4 P2 O3 Pb2 -118.2(3) 4_575 . . . ?
O4 P2 O3 Pb2 118.2(3) . . . . ?
O3 P2 O4 Pb3 -145.3(5) . . . . ?
O3 P2 O4 Pb1 -4.7(5) . . . 3_676 ?
O1 P1 O2 Pb1 121.1(4) . . . . ?
O1 P1 O2 Pb2 -11.0(5) . . . . ?
