# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_(h3o)2-xpbxi2(2-2x)h2o
_database_code_depnum_ccdc_archive 'CCDC 2071140'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2021-06-24 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT971_h3o2-xpbxi22-2xh2o  
;
PROBLEM: Check Calcd Resid. Dens.  0.95A   From I1              2.64 eA-3  
RESPONSE: This alert arises because we kept the occupation of I an O 
atoms non-fixed, to align with the model published by Daub 
& Hillebrecht (10.1002/zaac.201800267)
;
# Added during the CSD deposition process: Wednesday 17 March 2021 05:01 PM
# end Validation Reply Form



_audit_creation_date             2021-03-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
loop_
_audit_author_email
szymon.sobczak@amu.edu.pl
_chemical_name_common            '[H3O]2x[Pb1-xI2] x (2-2x)H2O'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I1 Pb0.4, H1.817 O0.932'
_chemical_formula_sum            'H1.82 I O0.93 Pb0.40'
_chemical_formula_weight         226.53
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   7.8946(10)
_cell_length_b                   4.5598(3)
_cell_length_c                   11.1985(18)
_cell_angle_alpha                90
_cell_angle_beta                 118.023(19)
_cell_angle_gamma                90
_cell_volume                     355.86(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    959
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.6960
_cell_measurement_theta_min      2.0400
_shelx_estimated_absorpt_T_max   0.339
_shelx_estimated_absorpt_T_min   0.169
_exptl_absorpt_coefficient_mu    27.563
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dull yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.228
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3208
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.692
_diffrn_reflns_theta_min         4.123
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                419
_reflns_number_total             523
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.750
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.295
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         523
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0360
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0433P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0869
_refine_special_details          ?
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Pb1 Pb 1.000000 0.500000 0.500000 0.0437(3) Uani 0.80(3) 4 d S T . . .
I1 I 0.70736(11) 1.000000 0.31094(9) 0.0431(3) Uani 1.00(4) 2 d S T . . .
O1 O 0.3498(18) 0.500000 0.0273(18) 0.069(6) Uani 0.93(6) 2 d GS T . A 1
H1A H 0.462407 0.568104 0.055517 0.104 Uiso 0.4(2) 1 d G U . A 1
H1B H 0.278045 0.630912 0.033225 0.104 Uiso 0.5(2) 1 d G U . A 1


_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
Pb1 I1 3.2278(9) 7_666 ?
Pb1 I1 3.2283(8) 5_766 ?
Pb1 I1 3.2278(9) 3_545 ?
Pb1 I1 3.2283(8) . ?
Pb1 I1 3.2283(8) 1_545 ?
Pb1 I1 3.2283(8) 5_776 ?
O1 H1A 0.8498 . ?
O1 H1A 0.85(13) 6_565 ?
O1 H1B 0.85(18) 6_565 ?
O1 H1B 0.8468 . ?

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
I1 Pb1 I1 180.0 7_666 3_545 ?
I1 Pb1 I1 90.14(3) 1_545 5_766 ?
I1 Pb1 I1 89.83(2) 7_666 5_766 ?
I1 Pb1 I1 89.86(3) 5_776 5_766 ?
I1 Pb1 I1 90.14(3) 5_776 . ?
I1 Pb1 I1 89.86(3) 1_545 . ?
I1 Pb1 I1 90.17(2) 7_666 1_545 ?
I1 Pb1 I1 89.83(2) 7_666 5_776 ?
I1 Pb1 I1 89.83(2) 3_545 1_545 ?
I1 Pb1 I1 90.17(2) 7_666 . ?
I1 Pb1 I1 180.0 5_766 . ?
I1 Pb1 I1 90.17(2) 3_545 5_776 ?
I1 Pb1 I1 89.83(2) 3_545 . ?
I1 Pb1 I1 90.17(2) 3_545 5_766 ?
I1 Pb1 I1 180.0 5_776 1_545 ?
Pb1 I1 Pb1 89.83(2) 3_455 1_565 ?
Pb1 I1 Pb1 89.86(3) 1_565 . ?
Pb1 I1 Pb1 89.83(2) 3_455 . ?
H1A O1 H1A 42.9 . 6_565 ?
H1A O1 H1B 148.2 . 6_565 ?
H1A O1 H1B 109.6 . . ?
H1A O1 H1B 109.6 6_565 6_565 ?
H1B O1 H1A 148.2 . 6_565 ?
H1B O1 H1B 89.7 . 6_565 ?


_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pbi3_oh3_4h2o_1_20gpa
_database_code_depnum_ccdc_archive 'CCDC 2071142'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2021-03-17 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_pbi3_oh3_4h2o_1_20gpa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.273 Why?
RESPONSE: These date comes from high-pressure experiment and part of the reflection can not be collected, due to the DAC opening angle and crystal low symmetry.
;
_vrf_PLAT088_pbi3_oh3_4h2o_1_20gpa 
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.59 Note
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC, particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT149_pbi3_oh3_4h2o_1_20gpa 
;
PROBLEM: s.u. on the   beta    Angle is Too Large .......       0.17 Degree
RESPONSE: This higher than usual s.u. on the beta angle parabobly is affected by the used method and the nature of sample.
;
_vrf_PLAT306_pbi3_oh3_4h2o_1_20gpa 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O1 Check
RESPONSE: Due to the highly absorbing sample and the limitation of the used method, assigning of the hydrogen atoms was impossible.
;
_vrf_PLAT911_pbi3_oh3_4h2o_1_20gpa 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        344 Report
RESPONSE: These reflections were probably affected by unexpected deviations in their intensities for symmetry equivalent measurements and omitted during initial data reduction.
;
# Added during the CSD deposition process: Wednesday 17 March 2021 05:01 PM
# end Validation Reply Form

_audit_creation_date             2021-03-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
loop_
_audit_author_email
szymon.sobczak@amu.edu.pl
_chemical_name_common            (H3O)PbI3x4H2O
_chemical_name_systematic        (H3O)PbI3.4H2O
_chemical_formula_moiety         '0.5(I6 Pb2), 5(O)'
_chemical_formula_sum            'I3 O5 Pb'
_chemical_formula_weight         667.89
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'I 1 2/m 1'
_space_group_name_Hall           '-I 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   16.119(13)
_cell_length_b                   4.5261(9)
_cell_length_c                   16.88(4)
_cell_angle_alpha                90
_cell_angle_beta                 111.25(17)
_cell_angle_gamma                90
_cell_volume                     1147(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    257
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      24.8010
_cell_measurement_theta_min      2.1570
_shelx_estimated_absorpt_T_max   0.342
_shelx_estimated_absorpt_T_min   0.056
_exptl_absorpt_coefficient_mu    22.746
_exptl_absorpt_correction_T_max  0.046
_exptl_absorpt_correction_T_min  0.007
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.866
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1124
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 1.20(2) GPa
 (1200000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the
 shift of the ruby R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_av_unetI/netI     0.1186
_diffrn_reflns_Laue_measured_fraction_full 0.366
_diffrn_reflns_Laue_measured_fraction_max 0.259
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1043
_diffrn_reflns_point_group_measured_fraction_full 0.273
_diffrn_reflns_point_group_measured_fraction_max 0.265
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.647
_diffrn_reflns_theta_min         2.188
_diffrn_ambient_temperature      300(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0593
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.273
_diffrn_measured_fraction_theta_max 0.265
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00   3.00   1.00   20.00    --   25.28  81.00 -29.00   23
  2  ω     -9.00  19.00   1.00   20.00    --   25.28  39.00 -12.00   28
  3  ω    -29.00  -4.00   1.00   20.00    --   25.28   0.00-150.00   25
  4  ω     11.00  37.00   1.00   20.00    --   25.28 -99.00-150.00   26
  5  ω     -6.00  29.00   1.00   20.00    --   25.28 -26.00   7.00   35
  6  ω     71.00  99.00   1.00   20.00    --   25.28-178.00 -90.00   28
  7  ω     12.00  65.00   1.00   20.00    --   25.28 -97.00  35.00   53
  8  ω    -28.00  -2.00   1.00   20.00    --  -26.22   0.00   0.00   26
  9  ω    -44.00 -19.00   1.00   20.00    --  -26.22  19.00  30.00   25
 10  ω     -3.00  19.00   1.00   20.00    --  -26.22 -81.00  29.00   22
 11  ω     26.00  50.00   1.00   20.00    --  -26.22-135.00-123.00   24
 12  ω     -7.00  25.00   1.00   20.00    --  -26.22 -39.00-167.00   32
 13  ω    -14.00  11.00   1.00   20.00    --  -26.22 -53.00  17.00   25
 14  ω    -57.00 -26.00   1.00   20.00    --  -26.22  97.00 -35.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0138848000
_diffrn_orient_matrix_UB_12      -0.0146053000
_diffrn_orient_matrix_UB_13      -0.0346808000
_diffrn_orient_matrix_UB_21      0.0452569000
_diffrn_orient_matrix_UB_22      -0.0073850000
_diffrn_orient_matrix_UB_23      0.0283613000
_diffrn_orient_matrix_UB_31      -0.0033853000
_diffrn_orient_matrix_UB_32      -0.1566577000
_diffrn_orient_matrix_UB_33      0.0020584000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                236
_reflns_number_total             331
_reflns_odcompleteness_completeness 27.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.249
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         331
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0799
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          .
_refine_ls_shift/su_mean         .
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0817P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1853
_refine_special_details          ?
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Pb1 Pb 0.1501(2) 1.000000 0.3022(4) 0.058(7) Uani 1 2 d S T P . .
I2 I 0.3705(4) 1.000000 0.3406(7) 0.068(10) Uani 1 2 d S T P . .
I3 I 0.1877(4) 0.500000 0.4427(7) 0.061(11) Uani 1 2 d S T P . .
I1 I -0.0500(4) 1.000000 0.2612(7) 0.052(8) Uani 1 2 d S TU P . .
O3 O 0.230(4) 1.000000 0.627(6) 0.051(11) Uiso 1 2 d S . P . .
O2 O 0.164(4) 0.500000 0.663(6) 0.089(17) Uiso 1 2 d S . P . .
O5 O 0.433(4) 0.500000 0.529(7) 0.070(14) Uiso 1 2 d S . P . .
O1 O 0.000000 0.500000 0.500000 0.128 Uiso 1 4 d S U P . .
O4 O 0.388(4) 1.000000 0.600(7) 0.069(13) Uiso 1 2 d S . P . .
O1H O -0.021(10) 1.000000 0.498(19) 0.07(3) Uiso 0.5 2 d S . P . .


_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
Pb1 I2 3.235(10) 7_575 ?
Pb1 I2 3.235(10) 7_565 ?
Pb1 I2 3.372(10) . ?
Pb1 I3 3.173(10) 1_565 ?
Pb1 I3 3.173(10) . ?
Pb1 I1 3.044(9) . ?
O1H O1H 0.7(4) 5_576 ?

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
I2 Pb1 I2 87.7(2) 7_565 . ?
I2 Pb1 I2 87.7(2) 7_575 . ?
I2 Pb1 I2 88.8(4) 7_565 7_575 ?
I3 Pb1 I2 174.9(3) 1_565 7_565 ?
I3 Pb1 I2 87.3(2) 1_565 . ?
I3 Pb1 I2 174.9(3) . 7_575 ?
I3 Pb1 I2 89.9(3) . 7_565 ?
I3 Pb1 I2 87.3(2) . . ?
I3 Pb1 I2 89.9(3) 1_565 7_575 ?
I3 Pb1 I3 91.0(4) 1_565 . ?
I1 Pb1 I2 91.0(2) . 7_575 ?
I1 Pb1 I2 178.1(4) . . ?
I1 Pb1 I2 91.0(2) . 7_565 ?
I1 Pb1 I3 94.0(3) . 1_565 ?
I1 Pb1 I3 94.0(3) . . ?
Pb1 I2 Pb1 92.3(2) 7_565 . ?
Pb1 I2 Pb1 88.8(4) 7_565 7_575 ?
Pb1 I2 Pb1 92.3(2) 7_575 . ?
Pb1 I3 Pb1 91.0(4) 1_545 . ?


_exptl_crystal_recrystallization_method 
'Obtained in the high-pressure reaction of PbI2 in conc. HI at 1.2 GPa'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pbi3_oh3_4h2o_0_50gpa
# Added during the CSD deposition process: Monday 19 April 2021 06:18 PM
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 2071141'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2021-04-19 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT027_pbi3_oh3_4h2o_0_50gpa 
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: These date comes from high-pressure experiment and part of the reflect
;
_vrf_PLAT029_pbi3_oh3_4h2o_0_50gpa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.395 Why?
RESPONSE: A full set of data was collected, however the very high angle data was
;
_vrf_PLAT088_pbi3_oh3_4h2o_0_50gpa 
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.98 Note
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC,
;
_vrf_PLAT306_pbi3_oh3_4h2o_0_50gpa 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O1 Check
RESPONSE: Due to the highly absorbing sample and the limitation of the used meth
;
_vrf_PLAT306_pbi3_oh3_4h2o_0_50gpa_2 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O2 Check
RESPONSE: Due to the highly absorbing sample and the limitation of the used meth
;
_vrf_PLAT306_pbi3_oh3_4h2o_0_50gpa_3 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O3 Check
RESPONSE: Due to the highly absorbing sample and the limitation of the used meth
;
_vrf_PLAT306_pbi3_oh3_4h2o_0_50gpa_4 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O4 Check
RESPONSE: Due to the highly absorbing sample and the limitation of the used meth
;
_vrf_PLAT306_pbi3_oh3_4h2o_0_50gpa_5 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O5 Check
RESPONSE: Due to the highly absorbing sample and the limitation of the used meth
;
_vrf_PLAT911_pbi3_oh3_4h2o_0_50gpa 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        149 Report
RESPONSE: These reflections were probably affected by unexpected deviations in their intensities for symmetry equivalent measurements and omitted during initial data reduction.
;
_audit_creation_date             2021-03-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
loop_
_audit_author_email
szymon.sobczak@amu.edu.pl
_chemical_name_common            (H3O)PbI3x4H2O
_chemical_name_systematic        (H3O)PbI3.4H2O
_chemical_formula_moiety         '0.5(I6 Pb2), 5(O)'
_chemical_formula_sum            'I3 O5 Pb'
_chemical_formula_weight         667.89
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'I 1 2/m 1'
_space_group_name_Hall           '-I 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   16.205(2)
_cell_length_b                   4.51695(14)
_cell_length_c                   17.184(14)
_cell_angle_alpha                90
_cell_angle_beta                 111.50(4)
_cell_angle_gamma                90
_cell_volume                     1170.3(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2890
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      26.9830
_cell_measurement_theta_min      2.6920
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.303
_exptl_absorpt_correction_T_max  0.043
_exptl_absorpt_correction_T_min  0.015
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.791
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1124
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
20 0 3 0.0473
-7 6 2 0.1180
-10 -1 23 0.0323
-21 0 -3 0.0469
10 1 -24 0.0323
8 -6 -4 0.1652

_exptl_crystal_preparation       'mounted in a diamond-anvil cell'
_exptl_crystal_recrystallization_method 
'Obtained from the high-pressure reaction of the PbI2 dissolved in conc. HI at pressure of 0.5 GPa'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.065
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.393     0.454
         range of gasket transmission (min-max)           0.828     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 258.0 microns
    Gasket absorption coeff =        21.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 0.50(2) GPa
 (500000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the 
 shift of the ruby R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.395
_diffrn_reflns_Laue_measured_fraction_max 0.252
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            6503
_diffrn_reflns_point_group_measured_fraction_full 0.395
_diffrn_reflns_point_group_measured_fraction_max 0.252
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         26.191
_diffrn_reflns_theta_min         2.702
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean 16.0593
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.395
_diffrn_measured_fraction_theta_max 0.252
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  30.00   0.75   30.00    --   24.72  13.00  -3.00   80
  2  ω    -15.00   9.00   0.75   30.00    --   24.72  77.00 150.00   32
  3  ω    -35.00 -11.00   0.75   30.00    --   24.72 114.00 -45.00   32
  4  ω     -6.50  52.00   0.75   30.00    --   24.72 -53.00-162.00   78
  5  ω    -21.00  21.00   0.75   30.00    --   24.72  39.00 167.00   56
  6  ω    -22.00  20.00   0.75   30.00    --  -25.90 -39.00-167.00   56
  7  ω    -79.00 -10.00   0.75   30.00    --  -25.90 114.00 -45.00   92
  8  ω      1.00  25.00   0.75   30.00    --  -25.90 -97.00-143.00   32
  9  ω     -9.00  13.50   0.75   30.00    --  -25.90 -77.00  30.00   30
 10  ω    -35.00  34.00   0.75   30.00    --  -25.90   0.00   0.00   92
 11  ω    -58.00  11.00   0.75   30.00    --  -25.90  67.00 157.00   92
 12  ω    -21.00  10.50   0.75   30.00    --   24.72  38.00 150.00   42
 13  ω    -35.00 -11.00   0.75   30.00    --   24.72 114.00 135.00   32
 14  ω    -10.00  11.00   0.75   30.00    --   24.72  67.00 -23.00   28
 15  ω     -8.00  22.00   0.75   30.00    --   24.72  57.00 -30.00   40
 16  ω    -47.00  22.00   0.75   30.00    --  -25.90  19.00-180.00   92
 17  ω    -17.00   7.00   0.75   30.00    --  -25.90 -53.00-162.00   32
 18  ω   -111.00 -78.00   0.75   30.00    --  -25.90 178.00 -90.00   44
 19  ω   -102.00 -75.00   0.75   30.00    --  -25.90-178.00  90.00   36
 20  ω   -105.00 -78.00   0.75   30.00    --  -25.90 178.00  90.00   36
 21  ω     -9.50  52.00   0.75   30.00    --   24.72 -53.00  17.00   82
 22  ω     33.50  92.00   0.75   30.00    --   24.72-135.00  57.00   78
 23  ω    -47.00  -8.00   0.75   30.00    --   24.72  19.00-150.00   52
 24  ω    -22.00  47.00   0.75   30.00    --  -25.90 -19.00-180.00   92
 25  ω    -35.00  34.00   0.75   30.00    --  -25.90   0.00-180.00   92
 26  ω    -30.00  39.00   0.75   30.00    --  -25.90 -13.00   3.00   92
 27  ω    -39.00  30.00   0.75   30.00    --  -25.90  13.00  -3.00   92
 28  ω    -35.00  34.00   0.75   30.00    --  -25.90   0.00   0.00   92
 29  ω    -26.00  43.00   0.75   30.00    --  -25.90 -26.00   7.00   92
 30  ω    -47.00  22.00   0.75   30.00    --  -25.90  39.00 -12.00   92
 31  ω    -43.00  26.00   0.75   30.00    --  -25.90  26.00  -7.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                317
_reflns_number_total             335
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.00118(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         335
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.232
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0344P)²+26.3231P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0843
_refine_special_details          ?
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Pb1 Pb 0.15064(6) 1.000000 0.3016(2) 0.048(4) Uani 1 2 d S T P . .
I2 I 0.36987(11) 1.000000 0.3403(4) 0.045(6) Uani 1 2 d S T P . .
I3 I 0.18849(12) 0.500000 0.4401(4) 0.055(6) Uani 1 2 d S T P . .
I1 I -0.04838(11) 1.000000 0.2634(4) 0.070(7) Uani 1 2 d S T P . .
O3 O 0.2393(16) 1.000000 0.627(5) 0.082(8) Uiso 1 2 d S . P . .
O2 O 0.175(2) 0.500000 0.657(6) 0.118(12) Uiso 1 2 d S . P . .
O5 O 0.4332(15) 0.500000 0.527(5) 0.061(6) Uiso 1 2 d S . P . .
O1 O 0.000000 0.500000 0.500000 0.128 Uiso 1 4 d S U P . .
O4 O 0.3918(16) 1.000000 0.599(5) 0.077(8) Uiso 1 2 d S . P . .
O1H O -0.019(4) 1.000000 0.534(15) 0.10(2) Uiso 0.5 2 d S . P . .


_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
Pb1 I2 3.250(6) 7_575 ?
Pb1 I2 3.3662(19) . ?
Pb1 I2 3.250(6) 7_565 ?
Pb1 I3 3.174(6) 1_565 ?
Pb1 I3 3.174(6) . ?
Pb1 I1 3.0463(19) . ?
O1H O1H 1.5(4) 5_576 ?

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
I2 Pb1 I2 87.63(10) 7_565 . ?
I2 Pb1 I2 87.63(10) 7_575 . ?
I2 Pb1 I2 88.04(19) 7_565 7_575 ?
I3 Pb1 I2 90.39(14) . 7_565 ?
I3 Pb1 I2 87.24(11) . . ?
I3 Pb1 I2 90.39(14) 1_565 7_575 ?
I3 Pb1 I2 174.70(8) 1_565 7_565 ?
I3 Pb1 I2 87.24(11) 1_565 . ?
I3 Pb1 I2 174.70(8) . 7_575 ?
I3 Pb1 I3 90.7(2) . 1_565 ?
I1 Pb1 I2 91.68(12) . 7_575 ?
I1 Pb1 I2 91.68(12) . 7_565 ?
I1 Pb1 I2 179.0(2) . . ?
I1 Pb1 I3 93.44(12) . . ?
I1 Pb1 I3 93.43(12) . 1_565 ?
Pb1 I2 Pb1 92.37(10) 7_565 . ?
Pb1 I2 Pb1 92.37(10) 7_575 . ?
Pb1 I2 Pb1 88.04(19) 7_565 7_575 ?
Pb1 I3 Pb1 90.7(2) 1_545 . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pbi3_oh3_3h2o_2_63gpa
_database_code_depnum_ccdc_archive 'CCDC 2071143'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2021-03-17 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT027_pbi3_oh3_3h2o_2_63gpa 
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however the very high angle data was dominated by noise and was omitted.
;
_vrf_PLAT029_pbi3_oh3_3h2o_2_63gpa 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.370 Why?
RESPONSE: These date comes from high-pressure experiment and part of the reflection can not be collected, due to the DAC opening angle and crystal low symmetry.
;
_vrf_PLAT088_pbi3_oh3_3h2o_2_63gpa 
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.76 Note
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC, particularly disadvantageous for low-symmetry crystals.
;
_vrf_PLAT149_pbi3_oh3_3h2o_2_63gpa 
;
PROBLEM: s.u. on the   beta    Angle is Too Large .......       0.60 Degree
RESPONSE: This higher than usual s.u. on the beta angle parabobly is affected by the used method and the nature of sample.
;
_vrf_PLAT306_pbi3_oh3_3h2o_2_63gpa 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O1 Check
RESPONSE: Due to the highly absorbing sample and the limitation of the used method, assigning of the hydrogen atoms was impossible.
;
_vrf_PLAT911_pbi3_oh3_3h2o_2_63gpa 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        555 Report
RESPONSE: These reflections were probably affected by unexpected deviations in their intensities for symmetry equivalent measurements and omitted during initial data reduction.
;
# Added during the CSD deposition process: Wednesday 17 March 2021 05:01 PM
# end Validation Reply Form

_audit_creation_date             2021-03-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
loop_
_audit_author_email
szymon.sobczak@amu.edu.pl
_chemical_name_common            ?
_chemical_name_systematic        (H3O)PbI3.3H2O
_chemical_formula_moiety         '0.5(I6 Pb2), 4(O)'
_chemical_formula_sum            'I3 O4 Pb'
_chemical_formula_weight         651.89
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   9.57(3)
_cell_length_b                   4.513(3)
_cell_length_c                   12.98(11)
_cell_angle_alpha                90
_cell_angle_beta                 95.9(6)
_cell_angle_gamma                90
_cell_volume                     558(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    211
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      23.6820
_cell_measurement_theta_min      2.1140
_shelx_estimated_absorpt_T_max   0.127
_shelx_estimated_absorpt_T_min   0.054
_exptl_absorpt_coefficient_mu    23.395
_exptl_absorpt_correction_T_max  0.309
_exptl_absorpt_correction_T_min  0.183
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.883
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             546
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
9 4 6 0.0230
-8 -5 -5 0.0157
4 6 5 0.0202
-7 0 17 0.0092
-5 -6 0 0.0111
6 -1 -17 0.0223

_exptl_crystal_preparation       'mounted in a diamond-anvil cell'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 Data were collected at room temperature and pressure of 2.63(2) GPa
 (2630000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the 
 shift of the ruby R1-fluorescence line.
;

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1665
_diffrn_reflns_av_unetI/netI     0.1750
_diffrn_reflns_Laue_measured_fraction_full 0.370
_diffrn_reflns_Laue_measured_fraction_max 0.199
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            788
_diffrn_reflns_point_group_measured_fraction_full 0.370
_diffrn_reflns_point_group_measured_fraction_max 0.199
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         27.558
_diffrn_reflns_theta_min         2.140
_diffrn_ambient_temperature      300
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0593
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.370
_diffrn_measured_fraction_theta_max 0.199
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -40.00  17.00   0.75    5.00    --   -0.47  53.00 162.00   76
  2  ω    -15.25  47.00   0.75   17.50    --   26.66 -19.00-180.00   83
  3  ω    -19.00   5.00   0.75   17.50    --   26.66  81.00 -29.00   32
  4  ω     32.75  92.00   0.75   17.50    --   26.66-135.00-123.00   79
  5  ω    -22.00  26.00   0.75   17.50    --  -27.60 -39.00  12.00   64
  6  ω    -95.00 -75.50   0.75    5.00    --   -0.47-178.00 -90.00   26
  7  ω    -11.50  35.00   0.75   17.50    --   26.66 -39.00  12.00   62
  8  ω     23.00  47.00   0.75   17.50    --  -27.60-135.00-123.00   32
  9  ω    -11.00  28.00   0.75   17.50    --  -27.60 -38.00-180.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0337641000
_diffrn_orient_matrix_UB_12      0.0029414000
_diffrn_orient_matrix_UB_13      0.0456417000
_diffrn_orient_matrix_UB_21      0.0609867000
_diffrn_orient_matrix_UB_22      -0.0614535000
_diffrn_orient_matrix_UB_23      0.0280818000
_diffrn_orient_matrix_UB_31      0.0264822000
_diffrn_orient_matrix_UB_32      0.1455689000
_diffrn_orient_matrix_UB_33      0.0107440000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                110
_reflns_number_total             287
_reflns_odcompleteness_completeness 22.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.955
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.280
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         287
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.2014
_refine_ls_R_factor_gt           0.0860
_refine_ls_restrained_S_all      0.902
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1202P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2143
_refine_ls_wR_factor_ref         0.2865
_refine_special_details          ?
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Pb1 Pb 0.9198(7) 0.250000 0.8477(9) 0.056(3) Uani 1 2 d S TU P . .
I2 I 0.8442(14) 0.250000 1.0924(16) 0.060(4) Uani 1 2 d S TU P . .
I3 I 0.9747(16) 0.250000 0.6401(19) 0.071(5) Uani 1 2 d S TU P . .
I4 I 0.6858(16) -0.250000 0.8040(19) 0.068(4) Uani 1 2 d S TU P . .
O1 O 0.726(10) -0.250000 0.564(11) 0.028(15) Uiso 1 2 d S . P . .
O2 O 0.560(13) -0.250000 1.037(15) 0.06(2) Uiso 1 2 d S . P . .
O3 O 0.715(9) 0.250000 1.362(10) 0.015(12) Uiso 1 2 d S . P . .
O4 O 0.409(10) -0.750000 0.726(11) 0.034(17) Uiso 1 2 d S . P . .


_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
Pb1 I2 3.231(11) 3_757 ?
Pb1 I2 3.231(11) 3_767 ?
Pb1 I2 3.33(4) . ?
Pb1 I3 2.80(4) . ?
Pb1 I4 3.188(12) 1_565 ?
Pb1 I4 3.188(12) . ?

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
I2 Pb1 I2 89.1(7) 3_767 . ?
I2 Pb1 I2 89.1(7) 3_757 . ?
I2 Pb1 I2 88.6(4) 3_767 3_757 ?
I3 Pb1 I2 92.1(7) . 3_757 ?
I3 Pb1 I2 178.3(3) . . ?
I3 Pb1 I2 92.1(7) . 3_767 ?
I3 Pb1 I4 91.5(7) . . ?
I3 Pb1 I4 91.5(7) . 1_565 ?
I4 Pb1 I2 90.5(3) 1_565 3_767 ?
I4 Pb1 I2 87.3(7) 1_565 . ?
I4 Pb1 I2 87.3(7) . . ?
I4 Pb1 I2 176.3(7) . 3_767 ?
I4 Pb1 I2 176.3(7) 1_565 3_757 ?
I4 Pb1 I2 90.5(3) . 3_757 ?
I4 Pb1 I4 90.1(4) . 1_565 ?
Pb1 I2 Pb1 90.9(7) 3_767 . ?
Pb1 I2 Pb1 90.9(7) 3_757 . ?
Pb1 I2 Pb1 88.6(4) 3_767 3_757 ?
Pb1 I4 Pb1 90.1(4) . 1_545 ?

_oxdiff_exptl_absorpt_empirical_full_max 3.051
_oxdiff_exptl_absorpt_empirical_full_min 0.268
_oxdiff_exptl_absorpt_spherical_max 0.152
_oxdiff_exptl_absorpt_spherical_min 0.129
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pbi2_pol_b
_database_code_depnum_ccdc_archive 'CCDC 2071144'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2021-03-17 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_pbi2_pol_b          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.348 Why?
RESPONSE: These date comes from high-pressure experiment and part of the reflection can not be collected, due to the DAC opening angle and crystal low symmetry.
;
_vrf_RINTA01_pbi2_pol_b          
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: High factor is a result from the weak diffraction and the inclusion of reflections that are essentially unobserved. Additionally, due to the high pressure DAC used in this experiment, part of diffraction data is omitted.
;
_vrf_PLAT020_pbi2_pol_b          
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.246 Report
RESPONSE: RESPONSE: Please see comment to RINTA01
;
_vrf_PLAT149_pbi2_pol_b          
;
PROBLEM: s.u. on the   beta    Angle is Too Large .......       0.12 Degree
RESPONSE: This higher than usual s.u. on the beta angle parabobly is affected by the used method and the nature of sample.
;
_vrf_PLAT911_pbi2_pol_b          
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        239 Report
RESPONSE: A full set of data was collected, however the very high angle data was dominated by noise [I/sigma(I) < 1.0] and was omitted.
;
# Added during the CSD deposition process: Wednesday 17 March 2021 05:01 PM
# end Validation Reply Form

_audit_creation_date             2021-03-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
loop_
_audit_author_email
szymon.sobczak@amu.edu.pl
_chemical_name_common            'phase B of lead(II) iodide'
_chemical_name_systematic        'Lead(II) iodide polymorph B'
_chemical_formula_moiety         'I3 Pb1.5'
_chemical_formula_sum            'I3 Pb1.50'
_chemical_formula_weight         691.48
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   14.06(4)
_cell_length_b                   4.4260(12)
_cell_length_c                   10.540(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.08(12)
_cell_angle_gamma                90
_cell_volume                     654.9(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    501
_cell_measurement_temperature    320(2)
_cell_measurement_theta_max      25.0230
_cell_measurement_theta_min      2.0730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    52.550
_exptl_absorpt_correction_T_max  0.150
_exptl_absorpt_correction_T_min  0.056
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    7.013
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 Data were collected at 320K and pressure of 2.05(2) GPa
 (2050000 kPa) with the crystal obtained by the in-situ high-pressure
 crystallization technique.
 Pressure was determined by monitoring the shift of the ruby
 R1-fluorescence line.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2461
_diffrn_reflns_av_unetI/netI     0.1212
_diffrn_reflns_Laue_measured_fraction_full 0.419
_diffrn_reflns_Laue_measured_fraction_max 0.329
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1977
_diffrn_reflns_point_group_measured_fraction_full 0.419
_diffrn_reflns_point_group_measured_fraction_max 0.329
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         1.935
_diffrn_ambient_temperature      320(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0593
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.348
_diffrn_measured_fraction_theta_max 0.336
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00   5.00   1.00   22.50    --   26.82   0.00-150.00   40
  2  ω    -27.00  -1.00   1.00   22.50    --   26.82  97.00 -35.00   26
  3  ω     15.00  79.00   1.00   22.50    --   26.82-114.00  45.00   64
  4  ω    -28.00  22.00   1.00   22.50    --   26.82  39.00 -12.00   50
  5  ω     15.00  79.00   1.00   22.50    --   26.82-114.00-135.00   64
  6  ω    -21.00  39.00   1.00   22.50    --   26.82 -13.00   3.00   60
  7  ω    -19.00   6.00   1.00   22.50    --   26.82  81.00 151.00   25
  8  ω    -47.00  22.00   1.00   22.50    --  -27.75  39.00 -12.00   69
  9  ω    -58.00  11.00   1.00   22.50    --  -27.75  67.00 157.00   69
 10  ω    -22.00  27.00   1.00   22.50    --  -27.75 -39.00  12.00   49
 11  ω     10.00  35.00   1.00   22.50    --  -27.75-114.00-135.00   25
 12  ω    -22.00  47.00   1.00   22.50    --  -27.75 -19.00-180.00   69
 13  ω      1.00  26.00   1.00   22.50    --  -27.75 -97.00  35.00   25
 14  ω    -11.00  10.00   1.00   22.50    --  -27.75 -67.00-157.00   21
 15  ω    -28.00  22.00   1.00   22.50    --   26.82  39.00 167.00   50
 16  ω    -18.00  47.00   1.00   22.50    --   26.82 -39.00-167.00   65
 17  ω     -5.00  58.00   1.00   22.50    --   26.82 -67.00-157.00   63
 18  ω    -27.00  -1.00   1.00   22.50    --   26.82  97.00 143.00   26
 19  ω    -11.00  11.00   1.00   22.50    --   26.82  67.00 -23.00   22
 20  ω      0.00  63.00   1.00   22.50    --   26.82 -81.00  29.00   63
 21  ω    -47.00 -13.00   1.00   22.50    --  -27.75  19.00-180.00   34
 22  ω     10.00  35.00   1.00   22.50    --  -27.75-114.00  45.00   25
 23  ω    -11.00  28.00   1.00   22.50    --  -27.75 -38.00   0.00   39
 24  ω    -11.00  28.00   1.00   22.50    --  -27.75 -38.00-180.00   39
 25  ω    -63.00   6.00   1.00   22.50    --  -27.75  81.00 -29.00   69
 26  ω     23.00  48.00   1.00   22.50    --  -27.75-135.00-123.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0458554000
_diffrn_orient_matrix_UB_12      -0.0284733000
_diffrn_orient_matrix_UB_13      0.0228618000
_diffrn_orient_matrix_UB_21      0.0020945000
_diffrn_orient_matrix_UB_22      -0.1504498000
_diffrn_orient_matrix_UB_23      -0.0225260000
_diffrn_orient_matrix_UB_31      0.0213637000
_diffrn_orient_matrix_UB_32      -0.0463999000
_diffrn_orient_matrix_UB_33      0.0592068000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                169
_reflns_number_total             258
_reflns_odcompleteness_completeness 35.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.763
_refine_diff_density_min         -1.644
_refine_diff_density_rms         0.625
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         252
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0809
_refine_ls_restrained_S_all      0.973
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1093P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.2161
_refine_special_details          ?
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Pb1 Pb 0.000000 0.500000 0.000000 0.055(7) Uani 1 4 d S TU P . .
Pb2 Pb -0.2359(7) 0.000000 0.2975(5) 0.067(6) Uani 1 2 d S TU P . .
I1 I 0.1547(11) 1.000000 0.0680(8) 0.070(8) Uani 1 2 d S TU P . .
I3 I -0.3633(11) 0.500000 0.4335(7) 0.063(7) Uani 1 2 d S TU P . .
I2 I -0.0738(11) 0.500000 0.2811(8) 0.071(7) Uani 1 2 d S TU P . .


_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
Pb1 I1 3.158(10) . ?
Pb1 I1 3.158(10) 1_545 ?
Pb1 I1 3.158(10) 5_565 ?
Pb1 I1 3.158(10) 5_575 ?
Pb1 I2 3.192(12) . ?
Pb1 I2 3.192(12) 5_565 ?
Pb2 I3 3.092(8) 7_456 ?
Pb2 I3 3.230(13) 1_545 ?
Pb2 I3 3.230(13) . ?
Pb2 I2 3.188(14) 1_545 ?
Pb2 I2 3.188(14) . ?

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
I1 Pb1 I1 180.0 . 5_565 ?
I1 Pb1 I1 89.0(4) . 1_545 ?
I1 Pb1 I1 91.0(4) 5_565 1_545 ?
I1 Pb1 I1 89.0(4) 5_565 5_575 ?
I1 Pb1 I1 91.0(4) . 5_575 ?
I1 Pb1 I1 180.0(3) 5_575 1_545 ?
I1 Pb1 I2 92.5(3) 1_545 . ?
I1 Pb1 I2 92.5(3) 5_565 5_565 ?
I1 Pb1 I2 92.5(3) 5_575 5_565 ?
I1 Pb1 I2 87.5(3) 5_565 . ?
I1 Pb1 I2 92.5(3) . . ?
I1 Pb1 I2 87.5(3) 5_575 . ?
I1 Pb1 I2 87.5(3) 1_545 5_565 ?
I1 Pb1 I2 87.5(3) . 5_565 ?
I2 Pb1 I2 180.0 . 5_565 ?
I3 Pb2 I3 80.0(3) 7_456 1_545 ?
I3 Pb2 I3 86.5(4) . 1_545 ?
I3 Pb2 I3 80.0(3) 7_456 . ?
I3 Pb2 I2 76.2(3) 7_456 . ?
I3 Pb2 I2 76.2(3) 7_456 1_545 ?
I2 Pb2 I3 87.9(3) . . ?
I2 Pb2 I3 156.2(2) . 1_545 ?
I2 Pb2 I3 156.2(2) 1_545 . ?
I2 Pb2 I3 87.9(3) 1_545 1_545 ?
I2 Pb2 I2 87.9(5) 1_545 . ?
Pb1 I1 Pb1 89.0(4) . 1_565 ?
Pb2 I3 Pb2 100.0(3) 7_456 . ?
Pb2 I3 Pb2 100.0(3) 7_456 1_565 ?
Pb2 I3 Pb2 86.5(4) . 1_565 ?
Pb2 I2 Pb1 108.6(2) . . ?
Pb2 I2 Pb1 108.6(2) 1_565 . ?
Pb2 I2 Pb2 87.9(5) 1_565 . ?

