Crystal structures and optical properties of two layered lead halide phosphites Pb<sub>3</sub>(HPO<sub>3</sub>)Cl<sub>4</sub>·H<sub>2</sub>O and Pb<sub>3</sub>(HPO<sub>3</sub>)<sub>2</sub>Cl<sub>2</sub>·H<sub>2</sub>O.
Zhao, Zong-Jie; Yan, Yu-Zheng; Fu, Jia-Jian; Wu, Hong-Yan; Zhang, Jian-Han; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4169–4180; doi:10.1039/d5dt03075g

data_7720244
_publ_section_title
;
 Crystal structures and optical properties of two layered lead halide
 phosphites
 Pb<sub>3</sub>(HPO<sub>3</sub>)Cl<sub>4</sub>&#xb7;H<sub>2</sub>O and
 Pb<sub>3</sub>(HPO<sub>3</sub>)<sub>2</sub>Cl<sub>2</sub>&#xb7;H<sub>2</sub>O.
;
_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         'Cl4 H3 O4 P Pb3'
_chemical_formula_sum            'Cl4 H3 O4 P Pb3'
_chemical_formula_weight         861.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 102.742(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.7896(3)
_cell_length_b                   8.4224(2)
_cell_length_c                   16.4621(4)
_cell_measurement_reflns_used    8684
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.3660
_cell_measurement_theta_min      2.5150
_cell_volume                     2135.32(8)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -35.00  15.00   0.50   38.35    --   20.00  54.00 -90.00  100
  2  \w     39.00 105.00   0.50   38.35    --   20.00  54.00 -90.00  132
  3  \w    -70.00  63.00   0.50   38.35    --   20.00  54.00-180.00  266
  4  \w     71.00 107.00   0.50   38.35    --   20.00  54.00-180.00   72
  5  \w    -74.00 -17.00   0.50   38.35    --   20.00  54.00  30.00  114
  6  \w     41.00  66.00   0.50   38.35    --   20.00  54.00  30.00   50
  7  \w    -72.00  40.00   0.50   38.35    --   20.00  54.00 150.00  224
  8  \w     83.00 108.00   0.50   38.35    --   20.00  54.00 150.00   50
  9  \w    -45.00   5.00   0.50   38.35    --   20.00  54.00 -30.00  100
 10  \w     55.00  80.00   0.50   38.35    --   20.00  54.00-120.00   50
 11  \w    -61.00 -36.00   0.50   38.35    --   20.00  54.00 -90.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15996
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.618
_exptl_absorpt_coefficient_mu    48.313
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11861
_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    5.359
_exptl_crystal_description       needle
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.141
_refine_diff_density_min         -1.865
_refine_diff_density_rms         0.376
_refine_ls_extinction_coef       0.00082(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3674
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0331
_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/[\s^2^(Fo^2^)+(0.0443P)^2^+2.0635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3068
_reflns_number_total             3674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03075g2.cif
_cod_data_source_block           20250625-g5-1
_cod_depositor_comments
'Adding full bibliography for 7720243--7720244.cif.'
_cod_database_code               7720244
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.248
_shelx_estimated_absorpt_t_min   0.133
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.3 times of:
  All O(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 P2-H2 = P1-H1
 1.3 with sigma of 0.02
3.a Free rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
;
_shelx_res_checksum              36493
_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
;