# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 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. 
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data_191025b_a
_database_code_depnum_ccdc_archive 'CCDC 2294271'
loop_
_audit_author_name
_audit_author_address
'Yilin Jiang'
;Tongji University
China
;
_audit_update_record             
;
2023-09-11 deposited with the CCDC.	2024-01-11 downloaded from the CCDC.
;
_audit_creation_date             2023-03-30
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H12 Cl2 O10 Pb3, H2 O'
_chemical_formula_sum            'C10 H14 Cl2 O11 Pb3'
_chemical_formula_weight         1002.68
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cl Cl 0.1484 0.1585 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.450(8)
_cell_length_b                   14.206(7)
_cell_length_c                   9.152(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.28(2)
_cell_angle_gamma                90
_cell_volume                     1748.6(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5646
_cell_measurement_temperature    287.0
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.65
_shelx_estimated_absorpt_T_max   0.179
_shelx_estimated_absorpt_T_min   0.041
_exptl_absorpt_coefficient_mu    29.175
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1483 before and 0.0727 after correction.
The Ratio of minimum to maximum transmission is 0.3971.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_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    3.809
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.608
_diffrn_reflns_theta_min         2.648
_diffrn_ambient_temperature      287.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3594
_reflns_number_total             3997
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         6.314
_refine_diff_density_min         -5.051
_refine_diff_density_rms         0.741
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3997
_refine_ls_number_restraints     172
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0592
_refine_ls_restrained_S_all      1.082
_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)+(0.1400P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1821
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Pb03-H00A \\sim Pb03-H00B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Free rotating group:
 O006(H00A,H00B), O00B(H00G,H00H), O00D(H00K,H00L)
4.b Ternary CH refined with riding coordinates:
 C1(H1), C00I(H00I), C00J(H00J), C00N(H00N)
4.c Secondary CH2 refined with riding coordinates:
 C00O(H00C,H00D), C00P(H00E,H00F)
;
_atom_sites_solution_hydrogens   mixed
_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
Pb01 Pb 0.41537(4) 0.29225(3) 0.66396(5) 0.0195(2) Uani 1 1 d . . . . .
O1 O 0.8869(8) 0.5241(6) 0.4149(10) 0.029(2) Uani 1 1 d . . . . .
C1 C 0.8550(9) 0.3255(8) 0.3447(12) 0.0152(19) Uani 1 1 d . . . . .
H1 H 0.848129 0.265870 0.291816 0.018 Uiso 1 1 calc R U . . .
Pb02 Pb 1.10397(4) 0.30037(3) 0.65388(5) 0.0206(2) Uani 1 1 d . . . . .
O2 O 0.9322(7) 0.3179(7) 0.5827(10) 0.0267(19) Uani 1 1 d . . . . .
Pb03 Pb 0.37485(4) 0.48216(3) 0.32639(5) 0.0221(2) Uani 1 1 d D . . . .
Cl04 Cl 0.2704(2) 0.3105(2) 0.4092(3) 0.0231(6) Uani 1 1 d . . . . .
Cl05 Cl 0.5282(3) 0.3801(2) 0.8848(3) 0.0287(7) Uani 1 1 d . . . . .
O006 O 0.3316(8) 0.4003(8) 0.0932(11) 0.034(2) Uani 1 1 d G . . . .
H00A H 0.273564 0.391567 0.058454 0.051 Uiso 1 1 d DG U . . .
H00B H 0.370113 0.391150 0.021219 0.051 Uiso 1 1 d DG U . . .
O007 O 0.7098(8) 0.5922(6) 0.2179(10) 0.0257(19) Uani 1 1 d . . . . .
O008 O 0.6073(8) 0.5302(6) 0.3837(10) 0.0252(19) Uani 1 1 d . . . . .
O009 O 0.4935(7) 0.3573(6) 0.3153(11) 0.0257(19) Uani 1 1 d . . . . .
O00A O 0.5676(7) 0.3464(7) 0.5341(10) 0.030(2) Uani 1 1 d . . . . .
O00B O 0.8771(9) 0.6138(7) 0.9251(11) 0.033(2) Uani 1 1 d G . . . .
H00G H 0.891094 0.598721 1.012690 0.050 Uiso 1 1 d G U . . .
H00H H 0.875731 0.561761 0.879268 0.050 Uiso 1 1 d G U . . .
O00D O 0.8338(9) 0.4875(8) 0.7015(13) 0.036(2) Uani 1 1 d G . . . .
H00K H 0.817494 0.490388 0.611804 0.054 Uiso 1 1 d G U . . .
H00L H 0.852802 0.542928 0.722649 0.054 Uiso 1 1 d G U . . .
O00E O 1.0268(8) 0.2937(8) 0.3897(12) 0.037(3) Uani 1 1 d . . . . .
O00G O 0.9420(8) 0.5565(7) 0.1925(10) 0.032(2) Uani 1 1 d . . . . .
C00H C 0.5696(8) 0.3504(8) 0.3970(14) 0.0179(19) Uani 1 1 d . . . . .
C00I C 0.6837(10) 0.4249(8) 0.2069(13) 0.020(2) Uani 1 1 d . . . . .
H00I H 0.631212 0.417180 0.133154 0.024 Uiso 1 1 calc R U . . .
C00J C 0.6712(8) 0.3440(8) 0.3199(12) 0.0150(19) Uani 1 1 d . . . . .
H00J H 0.671418 0.284857 0.264760 0.018 Uiso 1 1 calc R U . . .
C00K C 0.9424(9) 0.3137(8) 0.4457(13) 0.0164(19) Uani 1 1 d . . . . .
C00L C 0.6680(9) 0.5210(7) 0.2787(13) 0.0159(19) Uani 1 1 d . . . . .
C00M C 0.9035(9) 0.4993(9) 0.2841(14) 0.019(2) Uani 1 1 d . . . . .
C00N C 0.8743(9) 0.4025(8) 0.2265(12) 0.0165(19) Uani 1 1 d . . . . .
H00N H 0.929304 0.380111 0.165765 0.020 Uiso 1 1 calc R U . . .
C00O C 0.7582(8) 0.3396(8) 0.4265(12) 0.016(2) Uani 1 1 d . . . . .
H00C H 0.761453 0.397646 0.482266 0.019 Uiso 1 1 calc R U . . .
H00D H 0.748433 0.288051 0.494379 0.019 Uiso 1 1 calc R U . . .
C00P C 0.7844(9) 0.4121(8) 0.1281(12) 0.0155(19) Uani 1 1 d . . . . .
H00E H 0.780189 0.356421 0.066928 0.019 Uiso 1 1 calc R U . . .
H00F H 0.794649 0.465640 0.064158 0.019 Uiso 1 1 calc R U . . .


_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
Pb01 Cl04 3.043(3) . ?
Pb01 Cl05 2.813(3) . ?
Pb01 O007 2.591(10) 3_666 ?
Pb01 O008 2.577(8) 3_666 ?
Pb01 O009 2.743(9) 4_566 ?
Pb01 O00A 2.494(9) . ?
O1 Pb02 2.574(9) 3_766 ?
O1 C00M 1.269(16) . ?
C1 H1 0.9800 . ?
C1 C00K 1.501(15) . ?
C1 C00N 1.561(15) . ?
C1 C00O 1.518(16) . ?
Pb02 O2 2.410(10) . ?
Pb02 O00B 2.759(10) 2_746 ?
Pb02 O00E 2.628(11) . ?
Pb02 O00E 2.747(10) 4_566 ?
Pb02 O00G 2.550(10) 3_766 ?
O2 C00K 1.263(15) . ?
Pb03 Cl04 2.916(3) . ?
Pb03 Cl05 3.048(4) 3_666 ?
Pb03 O006 2.497(10) . ?
Pb03 O008 2.668(9) 3_666 ?
Pb03 O009 2.389(9) . ?
O006 H00A 0.8500 . ?
O006 H00B 0.8500 . ?
O007 C00L 1.285(14) . ?
O008 C00L 1.272(16) . ?
O009 C00H 1.267(15) . ?
O00A C00H 1.257(15) . ?
O00B H00G 0.8500 . ?
O00B H00H 0.8500 . ?
O00D H00K 0.8500 . ?
O00D H00L 0.8502 . ?
O00E C00K 1.280(16) . ?
O00G C00M 1.280(15) . ?
C00H C00J 1.544(16) . ?
C00I H00I 0.9800 . ?
C00I C00J 1.556(15) . ?
C00I C00L 1.530(16) . ?
C00I C00P 1.549(17) . ?
C00J H00J 0.9800 . ?
C00J C00O 1.522(15) . ?
C00M C00N 1.524(16) . ?
C00N H00N 0.9800 . ?
C00N C00P 1.510(17) . ?
C00O H00C 0.9700 . ?
C00O H00D 0.9700 . ?
C00P H00E 0.9700 . ?
C00P H00F 0.9700 . ?

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
Cl05 Pb01 Cl04 148.63(9) . . ?
O007 Pb01 Cl04 81.4(2) 3_666 . ?
O007 Pb01 Cl05 76.6(2) 3_666 . ?
O007 Pb01 O009 121.9(3) 3_666 4_566 ?
O008 Pb01 Cl04 73.3(2) 3_666 . ?
O008 Pb01 Cl05 75.5(2) 3_666 . ?
O008 Pb01 O007 51.3(3) 3_666 3_666 ?
O008 Pb01 O009 152.6(3) 3_666 4_566 ?
O009 Pb01 Cl04 134.1(2) 4_566 . ?
O009 Pb01 Cl05 77.1(2) 4_566 . ?
O00A Pb01 Cl04 97.6(2) . . ?
O00A Pb01 Cl05 76.4(2) . . ?
O00A Pb01 O007 122.7(3) . 3_666 ?
O00A Pb01 O008 73.4(3) . 3_666 ?
O00A Pb01 O009 99.6(3) . 4_566 ?
C00M O1 Pb02 91.7(7) . 3_766 ?
C00K C1 H1 106.2 . . ?
C00K C1 C00N 111.9(10) . . ?
C00K C1 C00O 112.4(9) . . ?
C00N C1 H1 106.2 . . ?
C00O C1 H1 106.2 . . ?
C00O C1 C00N 113.3(9) . . ?
O1 Pb02 O00B 149.5(3) 3_766 2_746 ?
O1 Pb02 O00E 133.0(3) 3_766 4_566 ?
O1 Pb02 O00E 80.2(3) 3_766 . ?
O2 Pb02 O1 83.2(3) . 3_766 ?
O2 Pb02 O00B 96.8(3) . 2_746 ?
O2 Pb02 O00E 84.1(3) . 4_566 ?
O2 Pb02 O00E 51.8(3) . . ?
O2 Pb02 O00G 80.3(3) . 3_766 ?
O00E Pb02 O00B 77.0(3) 4_566 2_746 ?
O00E Pb02 O00B 76.2(3) . 2_746 ?
O00E Pb02 O00E 123.8(3) . 4_566 ?
O00G Pb02 O1 51.3(3) 3_766 3_766 ?
O00G Pb02 O00B 159.0(3) 3_766 2_746 ?
O00G Pb02 O00E 116.1(3) 3_766 . ?
O00G Pb02 O00E 82.0(3) 3_766 4_566 ?
C00K O2 Pb02 99.0(8) . . ?
Cl04 Pb03 Cl05 155.48(9) . 3_666 ?
O006 Pb03 Cl04 73.9(3) . . ?
O006 Pb03 Cl05 81.7(3) . 3_666 ?
O006 Pb03 O008 147.0(3) . 3_666 ?
O008 Pb03 Cl04 74.2(2) 3_666 . ?
O008 Pb03 Cl05 129.5(2) 3_666 3_666 ?
O009 Pb03 Cl04 73.3(2) . . ?
O009 Pb03 Cl05 99.3(2) . 3_666 ?
O009 Pb03 O006 76.8(3) . . ?
O009 Pb03 O008 86.3(3) . 3_666 ?
Pb03 Cl04 Pb01 87.86(9) . . ?
Pb01 Cl05 Pb03 93.46(10) . 3_666 ?
Pb03 O006 H00A 126.7 . . ?
Pb03 O006 H00B 126.4 . . ?
H00A O006 H00B 104.5 . . ?
C00L O007 Pb01 91.8(8) . 3_666 ?
Pb01 O008 Pb03 104.1(3) 3_666 3_666 ?
C00L O008 Pb01 92.8(6) . 3_666 ?
C00L O008 Pb03 133.6(8) . 3_666 ?
Pb03 O009 Pb01 110.0(3) . 4_565 ?
C00H O009 Pb01 123.0(7) . 4_565 ?
C00H O009 Pb03 124.7(8) . . ?
C00H O00A Pb01 120.8(8) . . ?
Pb02 O00B H00G 117.9 2_756 . ?
Pb02 O00B H00H 135.1 2_756 . ?
H00G O00B H00H 104.5 . . ?
H00K O00D H00L 104.5 . . ?
Pb02 O00E Pb02 126.3(4) . 4_565 ?
C00K O00E Pb02 139.6(9) . 4_565 ?
C00K O00E Pb02 88.3(8) . . ?
C00M O00G Pb02 92.6(7) . 3_766 ?
O009 C00H C00J 116.7(11) . . ?
O00A C00H O009 124.8(11) . . ?
O00A C00H C00J 118.5(10) . . ?
C00J C00I H00I 107.2 . . ?
C00L C00I H00I 107.2 . . ?
C00L C00I C00J 111.0(9) . . ?
C00L C00I C00P 115.3(10) . . ?
C00P C00I H00I 107.2 . . ?
C00P C00I C00J 108.7(10) . . ?
C00H C00J C00I 111.1(9) . . ?
C00H C00J H00J 106.9 . . ?
C00I C00J H00J 106.9 . . ?
C00O C00J C00H 112.9(9) . . ?
C00O C00J C00I 111.8(9) . . ?
C00O C00J H00J 106.9 . . ?
O2 C00K C1 121.2(11) . . ?
O2 C00K O00E 120.5(12) . . ?
O00E C00K C1 118.1(11) . . ?
O007 C00L C00I 117.1(11) . . ?
O008 C00L O007 122.0(10) . . ?
O008 C00L C00I 120.5(10) . . ?
O1 C00M O00G 121.0(11) . . ?
O1 C00M C00N 122.1(11) . . ?
O00G C00M C00N 116.8(11) . . ?
C1 C00N H00N 107.2 . . ?
C00M C00N C1 115.8(9) . . ?
C00M C00N H00N 107.2 . . ?
C00P C00N C1 109.9(9) . . ?
C00P C00N C00M 109.2(9) . . ?
C00P C00N H00N 107.2 . . ?
C1 C00O C00J 110.3(9) . . ?
C1 C00O H00C 109.6 . . ?
C1 C00O H00D 109.6 . . ?
C00J C00O H00C 109.6 . . ?
C00J C00O H00D 109.6 . . ?
H00C C00O H00D 108.1 . . ?
C00I C00P H00E 108.4 . . ?
C00I C00P H00F 108.4 . . ?
C00N C00P C00I 115.6(9) . . ?
C00N C00P H00E 108.4 . . ?
C00N C00P H00F 108.4 . . ?
H00E C00P H00F 107.4 . . ?

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
Pb01 O007 C00L O008 -15.0(12) 3_666 . . . ?
Pb01 O007 C00L C00I 157.3(9) 3_666 . . . ?
Pb01 O008 C00L O007 15.0(12) 3_666 . . . ?
Pb01 O008 C00L C00I -156.9(9) 3_666 . . . ?
Pb01 O009 C00H O00A -102.5(12) 4_565 . . . ?
Pb01 O009 C00H C00J 75.9(12) 4_565 . . . ?
Pb01 O00A C00H O009 23.1(16) . . . . ?
Pb01 O00A C00H C00J -155.3(8) . . . . ?
O1 C00M C00N C1 -18.9(17) . . . . ?
O1 C00M C00N C00P 105.8(13) . . . . ?
C1 C00N C00P C00I 50.7(12) . . . . ?
Pb02 O1 C00M O00G 18.7(13) 3_766 . . . ?
Pb02 O1 C00M C00N -158.2(10) 3_766 . . . ?
Pb02 O2 C00K C1 -177.3(9) . . . . ?
Pb02 O2 C00K O00E 6.9(13) . . . . ?
Pb02 O00E C00K C1 -30.7(19) 4_565 . . . ?
Pb02 O00E C00K C1 177.8(9) . . . . ?
Pb02 O00E C00K O2 145.3(11) 4_565 . . . ?
Pb02 O00E C00K O2 -6.2(12) . . . . ?
Pb02 O00G C00M O1 -18.9(13) 3_766 . . . ?
Pb02 O00G C00M C00N 158.1(9) 3_766 . . . ?
Pb03 O008 C00L O007 -97.4(13) 3_666 . . . ?
Pb03 O008 C00L C00I 90.6(13) 3_666 . . . ?
Pb03 O009 C00H O00A 58.5(15) . . . . ?
Pb03 O009 C00H C00J -123.1(9) . . . . ?
O009 C00H C00J C00I 51.4(13) . . . . ?
O009 C00H C00J C00O 177.8(10) . . . . ?
O00A C00H C00J C00I -130.1(11) . . . . ?
O00A C00H C00J C00O -3.7(15) . . . . ?
O00G C00M C00N C1 164.1(11) . . . . ?
O00G C00M C00N C00P -71.2(13) . . . . ?
C00H C00J C00O C1 175.4(9) . . . . ?
C00I C00J C00O C1 -58.5(12) . . . . ?
C00J C00I C00L O007 155.3(11) . . . . ?
C00J C00I C00L O008 -32.3(15) . . . . ?
C00J C00I C00P C00N -53.1(12) . . . . ?
C00K C1 C00N C00M -55.4(14) . . . . ?
C00K C1 C00N C00P -179.8(9) . . . . ?
C00K C1 C00O C00J -175.8(9) . . . . ?
C00L C00I C00J C00H 54.9(13) . . . . ?
C00L C00I C00J C00O -72.2(12) . . . . ?
C00L C00I C00P C00N 72.2(13) . . . . ?
C00M C00N C00P C00I -77.4(12) . . . . ?
C00N C1 C00K O2 127.3(12) . . . . ?
C00N C1 C00K O00E -56.7(14) . . . . ?
C00N C1 C00O C00J 56.1(12) . . . . ?
C00O C1 C00K O2 -1.5(16) . . . . ?
C00O C1 C00K O00E 174.5(11) . . . . ?
C00O C1 C00N C00M 73.0(13) . . . . ?
C00O C1 C00N C00P -51.4(12) . . . . ?
C00P C00I C00J C00H -177.3(9) . . . . ?
C00P C00I C00J C00O 55.6(12) . . . . ?
C00P C00I C00L O007 31.2(15) . . . . ?
C00P C00I C00L O008 -156.4(11) . . . . ?

_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_191102c_a
_database_code_depnum_ccdc_archive 'CCDC 2294272'
loop_
_audit_author_name
_audit_author_address
'Yilin Jiang'
;Tongji University
China
;
_audit_update_record             
;
2023-09-11 deposited with the CCDC.	2024-01-11 downloaded from the CCDC.
;
_audit_creation_date             2023-03-30
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H10 Br2 O9 Pb3, 2(H2 O)'
_chemical_formula_sum            'C10 H14 Br2 O11 Pb3'
_chemical_formula_weight         1091.60
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Br Br -0.2901 2.4595 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.6110(7)
_cell_length_b                   14.2371(8)
_cell_length_c                   9.2448(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1791.47(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9434
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.63
_shelx_estimated_absorpt_T_max   0.139
_shelx_estimated_absorpt_T_min   0.059
_exptl_absorpt_coefficient_mu    32.639
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1208 before and 0.0768 after correction.
The Ratio of minimum to maximum transmission is 0.4949.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_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    4.047
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            22220
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.517
_diffrn_reflns_theta_min         2.627
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3819
_reflns_number_total             4113
_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       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         3.070
_refine_diff_density_min         -4.307
_refine_diff_density_rms         0.536
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4113
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0454
_refine_ls_restrained_S_all      1.076
_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)+(0.0775P)²+16.0347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1232
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C00M) \\sim Ueq, Uanis(C00H) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C00K)
\\sim Ueq, Uanis(C00N) \\sim Ueq, Uanis(C00O) \\sim Ueq, Uanis(C00J) \\sim Ueq,
Uanis(C00I) \\sim Ueq, Uanis(O009) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C00O) \\sim Ueq, Uanis(C00J) \\sim Ueq, Uanis(C00N) \\sim Ueq,
Uanis(C00K) \\sim Ueq, Uanis(O009) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3.a Free rotating group:
 O00D(H00E,H00F), O00F(H00G,H00H)
3.b Rotating group:
 O007(H00A,H00B)
3.c Ternary CH refined with riding coordinates:
 C00J(H00J), C00L(H00L), C00N(H00N), C00P(H00P)
3.d Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C00O(H00C,H00D)
;
_atom_sites_solution_hydrogens   mixed
_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
Pb01 Pb 0.41570(3) 0.70814(2) 0.66016(4) 0.01286(12) Uani 1 1 d . . . . .
O1 O 0.9275(5) 0.6804(6) 0.5843(8) 0.0195(15) Uani 1 1 d . . . . .
C1 C 0.7809(6) 0.5866(6) 0.1335(9) 0.0083(16) Uani 1 1 d . U . . .
H1A H 0.790703 0.533632 0.069097 0.010 Uiso 1 1 calc R U . . .
H1B H 0.775154 0.642515 0.074115 0.010 Uiso 1 1 calc R U . . .
Pb02 Pb 1.09650(3) 0.69874(3) 0.65634(4) 0.01361(13) Uani 1 1 d . . . . .
O2 O 0.8877(6) 0.4742(5) 0.4134(8) 0.0201(16) Uani 1 1 d . . . . .
Pb03 Pb 0.37369(3) 0.51641(3) 0.32659(4) 0.01522(13) Uani 1 1 d . . . . .
Br04 Br 0.26411(7) 0.69415(7) 0.40716(11) 0.0148(2) Uani 1 1 d . . . . .
Br05 Br 0.53180(8) 0.62158(7) 0.89336(10) 0.0201(2) Uani 1 1 d . . . . .
O006 O 0.6095(6) 0.4664(5) 0.3846(7) 0.0169(15) Uani 1 1 d . . . . .
O007 O 0.3248(6) 0.5971(6) 0.0955(8) 0.0223(16) Uani 1 1 d . . . . .
H00A H 0.266369 0.578894 0.067770 0.033 Uiso 1 1 d R U . . .
H00B H 0.362820 0.579389 0.024204 0.033 Uiso 1 1 d R U . . .
O008 O 0.7085(6) 0.4055(5) 0.2215(8) 0.0201(16) Uani 1 1 d . . . . .
O009 O 0.4948(5) 0.6386(5) 0.3143(8) 0.0174(14) Uani 1 1 d . U . . .
O00B O 0.5639(5) 0.6489(5) 0.5331(7) 0.0177(15) Uani 1 1 d . . . . .
O00C O 1.0196(6) 0.7080(7) 0.3956(9) 0.032(2) Uani 1 1 d . . . . .
O00D O 1.1186(7) 0.8897(6) 0.5777(9) 0.0295(19) Uani 1 1 d G . . . .
H00E H 1.090737 0.904831 0.498819 0.044 Uiso 1 1 d G U . . .
H00F H 1.113706 0.938442 0.630414 0.044 Uiso 1 1 d G U . . .
O00E O 0.9414(6) 0.4462(5) 0.1942(8) 0.0203(16) Uani 1 1 d . . . . .
O00F O 1.1654(7) 1.0153(6) 0.7992(9) 0.0300(19) Uani 1 1 d G . . . .
H00G H 1.143160 0.968112 0.845043 0.045 Uiso 1 1 d G U . . .
H00H H 1.145081 1.062511 0.846898 0.045 Uiso 1 1 d G U . . .
C00H C 0.9026(7) 0.5017(7) 0.2864(11) 0.0124(18) Uani 1 1 d . U . . .
C00I C 0.5676(6) 0.6447(6) 0.3954(11) 0.0115(17) Uani 1 1 d . U . . .
C00J C 0.6677(7) 0.6531(6) 0.3230(9) 0.0088(16) Uani 1 1 d . U . . .
H00J H 0.667670 0.711610 0.267126 0.011 Uiso 1 1 calc R U . . .
C00K C 0.6695(7) 0.4762(6) 0.2817(10) 0.0098(17) Uani 1 1 d . U . . .
C00L C 0.8718(7) 0.5966(6) 0.2306(9) 0.0090(17) Uani 1 1 d . . . . .
H00L H 0.925427 0.620185 0.169837 0.011 Uiso 1 1 calc R U . . .
C00M C 0.9370(7) 0.6870(6) 0.4481(10) 0.0086(16) Uani 1 1 d . U . . .
C00N C 0.6836(7) 0.5723(6) 0.2158(9) 0.0095(16) Uani 1 1 d . U . . .
H00N H 0.631619 0.578809 0.143205 0.011 Uiso 1 1 calc R U . . .
C00O C 0.7554(7) 0.6580(6) 0.4295(10) 0.0106(17) Uani 1 1 d . U . . .
H00C H 0.745603 0.709531 0.496682 0.013 Uiso 1 1 calc R U . . .
H00D H 0.758987 0.600233 0.484802 0.013 Uiso 1 1 calc R U . . .
C00P C 0.8510(7) 0.6725(7) 0.3477(10) 0.0110(17) Uani 1 1 d . . . . .
H00P H 0.843208 0.731751 0.295049 0.013 Uiso 1 1 calc R U . . .


_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
Pb01 Br04 3.1254(11) . ?
Pb01 Br05 2.9434(11) . ?
Pb01 O006 2.542(7) 3_666 ?
Pb01 O008 2.583(7) 3_666 ?
Pb01 O00B 2.482(7) . ?
O1 Pb02 2.409(8) . ?
O1 C00M 1.269(12) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C00L 1.536(13) . ?
C1 C00N 1.540(12) . ?
Pb02 O2 2.554(7) 3_766 ?
Pb02 O00C 2.631(9) . ?
Pb02 O00E 2.536(8) 3_766 ?
O2 C00H 1.254(12) . ?
Pb03 Br04 3.0303(10) . ?
Pb03 Br05 3.1063(11) 3_666 ?
Pb03 O006 2.691(7) 3_666 ?
Pb03 O007 2.516(7) . ?
Pb03 O009 2.400(7) . ?
O006 C00K 1.262(11) . ?
O007 H00A 0.8753 . ?
O007 H00B 0.8748 . ?
O008 C00K 1.267(11) . ?
O009 C00I 1.245(12) . ?
O00B C00I 1.275(12) . ?
O00C C00M 1.260(12) . ?
O00D H00E 0.8498 . ?
O00D H00F 0.8501 . ?
O00E C00H 1.277(12) . ?
O00F H00G 0.8503 . ?
O00F H00H 0.8500 . ?
C00H C00L 1.505(13) . ?
C00I C00J 1.523(12) . ?
C00J H00J 0.9800 . ?
C00J C00N 1.534(12) . ?
C00J C00O 1.549(13) . ?
C00K C00N 1.510(12) . ?
C00L H00L 0.9800 . ?
C00L C00P 1.556(12) . ?
C00M C00P 1.509(13) . ?
C00N H00N 0.9800 . ?
C00O H00C 0.9700 . ?
C00O H00D 0.9700 . ?
C00O C00P 1.518(12) . ?
C00P H00P 0.9800 . ?

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
Br05 Pb01 Br04 151.15(3) . . ?
O006 Pb01 Br04 74.15(17) 3_666 . ?
O006 Pb01 Br05 77.43(17) 3_666 . ?
O006 Pb01 O008 50.9(2) 3_666 3_666 ?
O008 Pb01 Br04 81.08(18) 3_666 . ?
O008 Pb01 Br05 77.23(18) 3_666 . ?
O00B Pb01 Br04 99.25(17) . . ?
O00B Pb01 Br05 76.58(17) . . ?
O00B Pb01 O006 72.5(2) . 3_666 ?
O00B Pb01 O008 121.3(2) . 3_666 ?
C00M O1 Pb02 99.7(6) . . ?
H1A C1 H1B 107.6 . . ?
C00L C1 H1A 108.6 . . ?
C00L C1 H1B 108.6 . . ?
C00L C1 C00N 114.6(7) . . ?
C00N C1 H1A 108.6 . . ?
C00N C1 H1B 108.6 . . ?
O1 Pb02 O2 84.6(3) . 3_766 ?
O1 Pb02 O00C 51.1(2) . . ?
O1 Pb02 O00E 82.4(3) . 3_766 ?
O2 Pb02 O00C 81.4(3) 3_766 . ?
O00E Pb02 O2 51.0(2) 3_766 3_766 ?
O00E Pb02 O00C 117.3(3) 3_766 . ?
C00H O2 Pb02 93.0(6) . 3_766 ?
Br04 Pb03 Br05 153.23(3) . 3_666 ?
O006 Pb03 Br04 73.86(16) 3_666 . ?
O006 Pb03 Br05 132.21(16) 3_666 3_666 ?
O007 Pb03 Br04 72.37(18) . . ?
O007 Pb03 Br05 80.94(18) . 3_666 ?
O007 Pb03 O006 145.4(2) . 3_666 ?
O009 Pb03 Br04 75.19(17) . . ?
O009 Pb03 Br05 98.22(17) . 3_666 ?
O009 Pb03 O006 85.6(2) . 3_666 ?
O009 Pb03 O007 79.0(3) . . ?
Pb03 Br04 Pb01 84.97(3) . . ?
Pb01 Br05 Pb03 90.44(3) . 3_666 ?
Pb01 O006 Pb03 105.2(2) 3_666 3_666 ?
C00K O006 Pb01 94.2(5) . 3_666 ?
C00K O006 Pb03 133.1(6) . 3_666 ?
Pb03 O007 H00A 110.7 . . ?
Pb03 O007 H00B 110.6 . . ?
H00A O007 H00B 103.4 . . ?
C00K O008 Pb01 92.2(5) . 3_666 ?
C00I O009 Pb03 124.6(6) . . ?
C00I O00B Pb01 121.3(6) . . ?
C00M O00C Pb02 89.4(6) . . ?
H00E O00D H00F 104.5 . . ?
C00H O00E Pb02 93.2(6) . 3_766 ?
H00G O00F H00H 104.5 . . ?
O2 C00H O00E 119.9(9) . . ?
O2 C00H C00L 123.8(9) . . ?
O00E C00H C00L 116.2(8) . . ?
O009 C00I O00B 125.0(8) . . ?
O009 C00I C00J 116.9(8) . . ?
O00B C00I C00J 118.0(8) . . ?
C00I C00J H00J 107.3 . . ?
C00I C00J C00N 110.6(7) . . ?
C00I C00J C00O 114.4(7) . . ?
C00N C00J H00J 107.3 . . ?
C00N C00J C00O 109.6(7) . . ?
C00O C00J H00J 107.3 . . ?
O006 C00K O008 120.9(8) . . ?
O006 C00K C00N 119.2(8) . . ?
O008 C00K C00N 119.3(8) . . ?
C1 C00L H00L 107.3 . . ?
C1 C00L C00P 108.9(7) . . ?
C00H C00L C1 110.0(7) . . ?
C00H C00L H00L 107.3 . . ?
C00H C00L C00P 115.8(8) . . ?
C00P C00L H00L 107.3 . . ?
O1 C00M C00P 121.4(8) . . ?
O00C C00M O1 119.4(9) . . ?
O00C C00M C00P 119.2(9) . . ?
C1 C00N H00N 105.7 . . ?
C00J C00N C1 110.0(7) . . ?
C00J C00N H00N 105.7 . . ?
C00K C00N C1 115.4(7) . . ?
C00K C00N C00J 113.6(7) . . ?
C00K C00N H00N 105.7 . . ?
C00J C00O H00C 109.6 . . ?
C00J C00O H00D 109.6 . . ?
H00C C00O H00D 108.1 . . ?
C00P C00O C00J 110.5(7) . . ?
C00P C00O H00C 109.6 . . ?
C00P C00O H00D 109.6 . . ?
C00L C00P H00P 105.8 . . ?
C00M C00P C00L 112.4(7) . . ?
C00M C00P C00O 112.2(7) . . ?
C00M C00P H00P 105.8 . . ?
C00O C00P C00L 114.1(7) . . ?
C00O C00P H00P 105.8 . . ?

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
Pb01 O006 C00K O008 -14.2(10) 3_666 . . . ?
Pb01 O006 C00K C00N 157.0(8) 3_666 . . . ?
Pb01 O008 C00K O006 13.9(10) 3_666 . . . ?
Pb01 O008 C00K C00N -157.2(8) 3_666 . . . ?
Pb01 O00B C00I O009 -24.8(13) . . . . ?
Pb01 O00B C00I C00J 151.8(6) . . . . ?
O1 C00M C00P C00L -125.6(9) . . . . ?
O1 C00M C00P C00O 4.6(12) . . . . ?
C1 C00L C00P C00M -179.9(7) . . . . ?
C1 C00L C00P C00O 50.9(10) . . . . ?
Pb02 O1 C00M O00C -6.3(10) . . . . ?
Pb02 O1 C00M C00P 175.2(7) . . . . ?
Pb02 O2 C00H O00E -17.5(10) 3_766 . . . ?
Pb02 O2 C00H C00L 158.7(8) 3_766 . . . ?
Pb02 O00C C00M O1 5.7(9) . . . . ?
Pb02 O00C C00M C00P -175.8(7) . . . . ?
Pb02 O00E C00H O2 17.6(10) 3_766 . . . ?
Pb02 O00E C00H C00L -158.8(7) 3_766 . . . ?
O2 C00H C00L C1 -104.6(10) . . . . ?
O2 C00H C00L C00P 19.3(13) . . . . ?
Pb03 O006 C00K O008 101.2(10) 3_666 . . . ?
Pb03 O006 C00K C00N -87.7(10) 3_666 . . . ?
Pb03 O009 C00I O00B -57.0(12) . . . . ?
Pb03 O009 C00I C00J 126.4(7) . . . . ?
O006 C00K C00N C1 158.6(8) . . . . ?
O006 C00K C00N C00J 30.3(12) . . . . ?
O008 C00K C00N C1 -30.1(13) . . . . ?
O008 C00K C00N C00J -158.4(9) . . . . ?
O009 C00I C00J C00N -54.2(11) . . . . ?
O009 C00I C00J C00O -178.6(8) . . . . ?
O00B C00I C00J C00N 129.0(9) . . . . ?
O00B C00I C00J C00O 4.6(12) . . . . ?
O00C C00M C00P C00L 55.9(12) . . . . ?
O00C C00M C00P C00O -173.9(9) . . . . ?
O00E C00H C00L C1 71.6(10) . . . . ?
O00E C00H C00L C00P -164.4(8) . . . . ?
C00H C00L C00P C00M 55.6(11) . . . . ?
C00H C00L C00P C00O -73.6(10) . . . . ?
C00I C00J C00N C1 174.9(7) . . . . ?
C00I C00J C00N C00K -54.1(10) . . . . ?
C00I C00J C00O C00P -176.4(7) . . . . ?
C00J C00O C00P C00L -56.2(10) . . . . ?
C00J C00O C00P C00M 174.5(7) . . . . ?
C00L C1 C00N C00J 56.2(10) . . . . ?
C00L C1 C00N C00K -73.9(10) . . . . ?
C00N C1 C00L C00H 77.1(9) . . . . ?
C00N C1 C00L C00P -50.8(10) . . . . ?
C00N C00J C00O C00P 58.7(9) . . . . ?
C00O C00J C00N C1 -58.0(9) . . . . ?
C00O C00J C00N C00K 73.0(9) . . . . ?

_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_ww
_database_code_depnum_ccdc_archive 'CCDC 2294273'
loop_
_audit_author_name
_audit_author_address
'Yilin Jiang'
;Tongji University
China
;
_audit_update_record             
;
2023-09-11 deposited with the CCDC.	2024-01-11 downloaded from the CCDC.
;
_audit_creation_date             2023-05-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C24 H14 Cl30 O26 Pb24), 2(Cl)'
_chemical_formula_sum            'C12 H7 Cl17 O13 Pb12'
_chemical_formula_weight         3448.04
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cl Cl 0.1484 0.1585 '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      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'

_cell_length_a                   12.596(3)
_cell_length_b                   12.596(3)
_cell_length_c                   16.741(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2300.4(15)
_cell_formula_units_Z            2.00004
_cell_measurement_reflns_used    8890
_cell_measurement_temperature    288(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      3.23
_shelx_estimated_absorpt_T_max   0.124
_shelx_estimated_absorpt_T_min   0.084
_exptl_absorpt_coefficient_mu    44.766
_exptl_absorpt_correction_T_max  0.9454
_exptl_absorpt_correction_T_min  0.1208
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1381 before and 0.0729 after correction.
The Ratio of minimum to maximum transmission is 0.5645.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.978
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35474
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.006
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_min         3.067
_diffrn_ambient_temperature      288.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_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                1268
_reflns_number_total             1352
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.781
_refine_diff_density_min         -2.965
_refine_diff_density_rms         0.279
_refine_ls_extinction_coef       0.00025(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0325
_refine_ls_restrained_S_all      1.133
_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)+(0.0336P)²+76.9786P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0845
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Others
 Fixed Sof: O3(0.16667) H3(0.16667)
3.a Ternary CH refined with riding coordinates:
 C2(H2), O3(H3)
;
_atom_sites_solution_hydrogens   geom
_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 0.48172(4) 0.35924(4) 0.60298(3) 0.0264(2) Uani 1 1 d . . . . .
Pb2 Pb 0.41184(7) 0.23733(6) 0.34242(3) 0.0439(2) Uani 1 1 d . . . . .
Cl2 Cl 0.5401(3) 0.1350(3) 0.43420(18) 0.0253(6) Uani 1 1 d . . . . .
Cl1 Cl 0.3837(4) 0.3837(4) 0.7500 0.0335(10) Uani 1 2 d S T P . .
Cl4 Cl 0.6667 0.3333 0.2553(4) 0.0341(12) Uani 1 3 d S T P . .
Cl3 Cl 0.2908(3) 0.3912(3) 0.33969(19) 0.0287(7) Uani 1 1 d . . . . .
O1 O 0.2446(8) 0.2445(8) 0.5948(5) 0.0257(19) Uani 1 1 d . . . . .
O2 O 0.3439(8) 0.2410(8) 0.4870(5) 0.029(2) Uani 1 1 d . . . . .
C1 C 0.2443(10) 0.2070(10) 0.5248(7) 0.019(2) Uani 1 1 d . . . . .
C2 C 0.1245(9) 0.1089(9) 0.4872(7) 0.013(2) Uani 1 1 d . . . . .
H2 H 0.1323 0.1157 0.4289 0.016 Uiso 1 1 calc R . . . .
O3 O 0.6667 0.3333 0.563(3) 0.058(11) Uani 0.5 3 d S T P . .
H3 H 0.6667 0.3333 0.5043 0.070 Uiso 0.5 3 calc RS T 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 Cl2 2.951(3) 9_556 ?
Pb1 Cl1 2.8387(13) . ?
Pb1 Cl3 3.022(3) 8_556 ?
Pb1 O1 2.591(8) . ?
Pb1 O2 2.533(9) . ?
Pb1 O3 2.597(12) . ?
Pb2 Cl2 2.953(3) . ?
Pb2 Cl2 3.012(3) 3_665 ?
Pb2 Cl3 3.006(3) . ?
Pb2 O2 2.575(9) . ?
Cl2 Pb1 2.951(3) 8_556 ?
Cl2 Pb2 3.012(3) 2_655 ?
Cl1 Pb1 2.8386(13) 4_556 ?
Cl3 Pb1 3.022(3) 9_556 ?
O1 C1 1.264(14) . ?
O2 C1 1.273(14) . ?
C1 C2 1.529(15) . ?
C2 C2 1.541(11) 9_556 ?
C2 C2 1.541(11) 8_556 ?
C2 H2 0.9800 . ?
O3 Pb1 2.597(11) 3_665 ?
O3 Pb1 2.597(11) 2_655 ?
O3 H3 0.9800 . ?

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 Pb1 Cl3 143.84(8) 9_556 8_556 ?
Cl1 Pb1 Cl2 76.77(7) . 9_556 ?
Cl1 Pb1 Cl3 83.79(10) . 8_556 ?
O1 Pb1 Cl2 71.9(2) . 9_556 ?
O1 Pb1 Cl1 70.3(2) . . ?
O1 Pb1 Cl3 73.0(2) . 8_556 ?
O1 Pb1 O3 140.6(4) . . ?
O2 Pb1 Cl2 84.2(2) . 9_556 ?
O2 Pb1 Cl1 121.4(2) . . ?
O2 Pb1 Cl3 80.3(2) . 8_556 ?
O2 Pb1 O1 51.1(3) . . ?
O2 Pb1 O3 97.0(8) . . ?
O3 Pb1 Cl2 134.6(5) . 9_556 ?
O3 Pb1 Cl1 134.7(9) . . ?
O3 Pb1 Cl3 79.9(4) . 8_556 ?
Cl2 Pb2 Cl2 79.03(12) . 3_665 ?
Cl2 Pb2 Cl3 148.66(9) . . ?
Cl3 Pb2 Cl2 78.84(9) . 3_665 ?
O2 Pb2 Cl2 67.1(2) . 3_665 ?
O2 Pb2 Cl2 77.2(2) . . ?
O2 Pb2 Cl3 73.9(2) . . ?
Pb1 Cl2 Pb2 94.57(8) 8_556 . ?
Pb1 Cl2 Pb2 102.57(9) 8_556 2_655 ?
Pb2 Cl2 Pb2 109.25(10) . 2_655 ?
Pb1 Cl1 Pb1 161.2(2) 4_556 . ?
Pb2 Cl3 Pb1 156.34(12) . 9_556 ?
C1 O1 Pb1 92.5(7) . . ?
Pb1 O2 Pb2 126.5(3) . . ?
C1 O2 Pb1 95.0(7) . . ?
C1 O2 Pb2 137.9(8) . . ?
O1 C1 O2 121.2(10) . . ?
O1 C1 C2 120.1(10) . . ?
O2 C1 C2 118.4(10) . . ?
C1 C2 C2 111.3(10) . 9_556 ?
C1 C2 C2 106.3(10) . 8_556 ?
C1 C2 H2 108.9 . . ?
C2 C2 C2 112.5(7) 8_556 9_556 ?
C2 C2 H2 108.9 9_556 . ?
C2 C2 H2 108.9 8_556 . ?
Pb1 O3 Pb1 113.6(8) 2_655 . ?
Pb1 O3 Pb1 113.6(8) 3_665 . ?
Pb1 O3 Pb1 113.6(8) 2_655 3_665 ?
Pb1 O3 H3 105.0 2_655 . ?
Pb1 O3 H3 105.0 . . ?
Pb1 O3 H3 105.0 3_665 . ?

_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_mo_j230413c_0m
_database_code_depnum_ccdc_archive 'CCDC 2294304'
loop_
_audit_author_name
_audit_author_address
'Yilin Jiang'
;Tongji University
China
;
_audit_update_record             
;
2023-09-11 deposited with the CCDC.	2024-01-11 downloaded from the CCDC.
;
_audit_creation_date             2023-05-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H4 Br16 O8 Pb10'
_chemical_formula_sum            'C8 H4 Br16 O8 Pb10'
_chemical_formula_weight         3578.57
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Br Br -0.2901 2.4595 '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      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'z, x, y'
'-z+1/2, -x, y+1/2'
'z+1/2, -x+1/2, -y'
'-z, x+1/2, -y+1/2'
'y, z, x'
'y+1/2, -z+1/2, -x'
'-y, z+1/2, -x+1/2'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'-z, -x, -y'
'z-1/2, x, -y-1/2'
'-z-1/2, x-1/2, y'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'-y-1/2, z-1/2, x'
'y, -z-1/2, x-1/2'
'y-1/2, z, -x-1/2'

_cell_length_a                   18.621(8)
_cell_length_b                   18.621(8)
_cell_length_c                   18.621(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6457(8)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9731
_cell_measurement_temperature    286.00
_cell_measurement_theta_max      24.956
_cell_measurement_theta_min      2.679
_shelx_estimated_absorpt_T_max   0.099
_shelx_estimated_absorpt_T_min   0.099
_exptl_absorpt_coefficient_mu    53.838
_exptl_absorpt_correction_T_max  0.0265
_exptl_absorpt_correction_T_min  0.0061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1552 before and 0.1130 after correction.
The Ratio of minimum to maximum transmission is 0.2302.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.522
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             8976
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1387
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            68217
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         25.370
_diffrn_reflns_theta_min         2.446
_diffrn_ambient_temperature      286.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1626
_reflns_number_total             1982
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.346
_refine_diff_density_min         -1.711
_refine_diff_density_rms         0.303
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1982
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0431
_refine_ls_restrained_S_all      1.088
_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)+(0.0612P)²+143.2931P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1217
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Riding coordinates:
 C1(H1)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_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 0.57100(4) 0.24957(4) 0.58413(4) 0.0519(3) Uani 1 1 d . . . . .
Pb2 Pb 0.75666(5) 0.24334(5) 0.74334(5) 0.0604(4) Uani 1 3 d S T P . .
Pb3 Pb 0.77927(4) 0.00351(4) 0.64055(4) 0.0472(2) Uani 1 1 d . . . . .
Pb4 Pb 0.500000 0.500000 0.500000 0.0416(4) Uani 1 6 d S T P . .
Br1 Br 0.71799(10) 0.16053(9) 0.60617(10) 0.0465(4) Uani 1 1 d . . . . .
Br2 Br 0.70349(10) 0.36036(10) 0.57639(11) 0.0519(5) Uani 1 1 d . . . . .
Br3 Br 0.59328(11) 0.27298(12) 0.74460(11) 0.0562(5) Uani 1 1 d . . . . .
Br4 Br 0.51909(11) 0.34559(9) 0.45303(9) 0.0478(5) Uani 1 1 d . . . . .
O1 O 0.5077(6) 0.0306(7) 0.6839(6) 0.040(3) Uani 1 1 d . . . . .
O2 O 0.5284(7) 0.1403(6) 0.6487(6) 0.041(3) Uani 1 1 d . . . . .
C1 C 0.5273(8) 0.0523(8) 0.5581(9) 0.031(3) Uani 1 1 d . . . . .
H1 H 0.558446 0.084908 0.531061 0.037 Uiso 1 1 d R . . . .
C2 C 0.5222(9) 0.0750(8) 0.6341(9) 0.035(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.226(2) . ?
Pb1 Br2 3.219(2) . ?
Pb1 Br2 3.060(3) 17_666 ?
Pb1 Br3 3.048(3) . ?
Pb1 Br4 3.177(2) . ?
Pb1 O1 2.665(11) 22_655 ?
Pb1 O2 2.494(12) . ?
Pb2 Br1 3.069(2) 11_646 ?
Pb2 Br1 3.069(2) 6_665 ?
Pb2 Br1 3.069(2) . ?
Pb2 Br3 3.092(3) 6_665 ?
Pb2 Br3 3.092(3) 11_646 ?
Pb2 Br3 3.092(3) . ?
Pb3 Br1 3.203(2) . ?
Pb3 Br2 2.939(2) 15_755 ?
Pb3 Br3 3.122(3) 20_566 ?
Pb3 O1 2.718(12) 20_566 ?
Pb3 O2 2.502(12) 20_566 ?
Pb4 Br4 3.026(2) 21_666 ?
Pb4 Br4 3.026(2) . ?
Pb4 Br4 3.026(2) 13_666 ?
Pb4 Br4 3.026(2) 5 ?
Pb4 Br4 3.026(2) 9 ?
Pb4 Br4 3.026(2) 17_666 ?
O1 C2 1.27(2) . ?
O2 C2 1.251(19) . ?
C1 C1 1.593(16) 20_566 ?
C1 C1 1.593(16) 22_655 ?
C1 H1 0.9794 . ?
C1 C2 1.48(2) . ?

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
Br2 Pb1 Br1 149.84(6) 17_666 . ?
Br2 Pb1 Br1 71.63(5) . . ?
Br2 Pb1 Br2 121.30(7) 17_666 . ?
Br2 Pb1 Br4 79.98(5) 17_666 . ?
Br3 Pb1 Br1 80.40(6) . . ?
Br3 Pb1 Br2 75.53(6) . 17_666 ?
Br3 Pb1 Br2 81.25(6) . . ?
Br3 Pb1 Br4 135.59(6) . . ?
Br4 Pb1 Br1 130.18(6) . . ?
Br4 Pb1 Br2 80.68(6) . . ?
O1 Pb1 Br1 115.7(3) 22_655 . ?
O1 Pb1 Br2 71.0(3) 22_655 17_666 ?
O1 Pb1 Br2 144.5(3) 22_655 . ?
O1 Pb1 Br3 133.3(3) 22_655 . ?
O1 Pb1 Br4 68.4(2) 22_655 . ?
O2 Pb1 Br1 77.8(3) . . ?
O2 Pb1 Br2 142.0(3) . . ?
O2 Pb1 Br2 77.6(3) . 17_666 ?
O2 Pb1 Br3 71.8(3) . . ?
O2 Pb1 Br4 137.2(3) . . ?
O2 Pb1 O1 70.0(4) . 22_655 ?
Br1 Pb2 Br1 83.97(6) . 11_646 ?
Br1 Pb2 Br1 83.97(6) 6_665 11_646 ?
Br1 Pb2 Br1 83.97(6) . 6_665 ?
Br1 Pb2 Br3 141.33(5) 6_665 . ?
Br1 Pb2 Br3 129.87(5) 6_665 11_646 ?
Br1 Pb2 Br3 129.87(5) 11_646 . ?
Br1 Pb2 Br3 141.33(5) 11_646 6_665 ?
Br1 Pb2 Br3 82.25(5) . . ?
Br1 Pb2 Br3 82.25(5) 11_646 11_646 ?
Br1 Pb2 Br3 82.25(5) 6_665 6_665 ?
Br1 Pb2 Br3 141.33(5) . 11_646 ?
Br1 Pb2 Br3 129.87(5) . 6_665 ?
Br3 Pb2 Br3 79.37(7) . 6_665 ?
Br3 Pb2 Br3 79.37(7) 6_665 11_646 ?
Br3 Pb2 Br3 79.37(7) . 11_646 ?
Br2 Pb3 Br1 141.78(6) 15_755 . ?
Br2 Pb3 Br3 79.63(6) 15_755 20_566 ?
Br3 Pb3 Br1 127.67(5) 20_566 . ?
O1 Pb3 Br1 71.7(2) 20_566 . ?
O1 Pb3 Br2 72.3(2) 20_566 15_755 ?
O1 Pb3 Br3 114.6(3) 20_566 20_566 ?
O2 Pb3 Br1 82.5(3) 20_566 . ?
O2 Pb3 Br2 83.7(3) 20_566 15_755 ?
O2 Pb3 Br3 70.3(3) 20_566 20_566 ?
O2 Pb3 O1 49.1(4) 20_566 20_566 ?
Br4 Pb4 Br4 97.41(6) 13_666 9 ?
Br4 Pb4 Br4 97.41(6) 13_666 5 ?
Br4 Pb4 Br4 180.0 . 13_666 ?
Br4 Pb4 Br4 97.41(6) . 21_666 ?
Br4 Pb4 Br4 82.59(6) . 5 ?
Br4 Pb4 Br4 180.0 21_666 9 ?
Br4 Pb4 Br4 82.59(6) 5 9 ?
Br4 Pb4 Br4 82.59(6) 21_666 13_666 ?
Br4 Pb4 Br4 97.41(6) . 17_666 ?
Br4 Pb4 Br4 97.41(6) 17_666 9 ?
Br4 Pb4 Br4 97.41(6) 21_666 5 ?
Br4 Pb4 Br4 82.59(6) 13_666 17_666 ?
Br4 Pb4 Br4 82.59(6) . 9 ?
Br4 Pb4 Br4 180.0 5 17_666 ?
Br4 Pb4 Br4 82.59(6) 21_666 17_666 ?
Pb2 Br1 Pb1 92.67(5) . . ?
Pb2 Br1 Pb3 102.04(6) . . ?
Pb3 Br1 Pb1 142.82(7) . . ?
Pb1 Br2 Pb1 118.39(7) 21_666 . ?
Pb3 Br2 Pb1 130.30(7) 15_765 . ?
Pb3 Br2 Pb1 91.55(5) 15_765 21_666 ?
Pb1 Br3 Pb2 95.79(6) . . ?
Pb1 Br3 Pb3 90.64(5) . 22_655 ?
Pb2 Br3 Pb3 115.38(7) . 22_655 ?
Pb4 Br4 Pb1 110.39(6) . . ?
Pb1 O1 Pb3 106.0(4) 20_566 22_655 ?
C2 O1 Pb1 133.1(10) . 20_566 ?
C2 O1 Pb3 90.2(10) . 22_655 ?
Pb1 O2 Pb3 122.9(4) . 22_655 ?
C2 O2 Pb1 135.8(11) . . ?
C2 O2 Pb3 101.1(10) . 22_655 ?
C1 C1 C1 112.0(10) 20_566 22_655 ?
C1 C1 H1 109.1 20_566 . ?
C1 C1 H1 108.9 22_655 . ?
C2 C1 C1 110.7(14) . 20_566 ?
C2 C1 C1 105.4(14) . 22_655 ?
C2 C1 H1 110.7 . . ?
O1 C2 C1 121.7(14) . . ?
O2 C2 O1 119.5(15) . . ?
O2 C2 C1 118.7(14) . . ?

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
Pb1 O1 C2 O2 -108.8(16) 20_566 . . . ?
Pb1 O1 C2 C1 75.4(19) 20_566 . . . ?
Pb1 O2 C2 O1 169.8(10) . . . . ?
Pb1 O2 C2 C1 -14(2) . . . . ?
Pb3 O1 C2 O2 3.6(15) 22_655 . . . ?
Pb3 O1 C2 C1 -172.2(13) 22_655 . . . ?
Pb3 O2 C2 O1 -4.0(17) 22_655 . . . ?
Pb3 O2 C2 C1 172.0(12) 22_655 . . . ?
C1 C1 C2 O1 87.9(18) 22_655 . . . ?
C1 C1 C2 O1 -33(2) 20_566 . . . ?
C1 C1 C2 O2 150.8(15) 20_566 . . . ?
C1 C1 C2 O2 -88.0(19) 22_655 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
