# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1819917'
_audit_update_record             
;
2018-01-28 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H8 Br2 Cd O4 Pb2'
_chemical_formula_sum            'C4 H8 Br2 Cd O4 Pb2'
_chemical_formula_weight         806.71

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'
O O 0.0106 0.0060 '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'
Cd Cd -0.8075 1.2024 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.531(6)
_cell_length_b                   8.246(7)
_cell_length_c                   10.797(8)
_cell_angle_alpha                84.67(3)
_cell_angle_beta                 89.27(2)
_cell_angle_gamma                63.92(3)
_cell_volume                     599.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17470
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.95

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             692
_exptl_absorpt_coefficient_mu    36.428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1081
_exptl_absorpt_correction_T_max  0.1848
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17470
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.95
_reflns_number_total             2854
_reflns_number_gt                2426
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0400P)²+5.0880P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2854
_refine_ls_number_parameters     118
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0855
_refine_ls_wR_factor_gt          0.0800
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.73680(5) 0.42824(5) 0.60149(3) 0.01929(11) Uani 1 1 d . . .
Pb2 Pb 0.57710(5) 0.65918(5) 0.89010(3) 0.02045(11) Uani 1 1 d . . .
Cd1 Cd 0.67866(10) 0.54403(9) 0.24416(6) 0.01977(16) Uani 1 1 d . . .
Br1 Br 1.05220(14) 0.31277(15) 0.32115(10) 0.0298(2) Uani 1 1 d . . .
Br2 Br 0.67775(16) 0.85384(14) 0.15472(10) 0.0284(2) Uani 1 1 d . . .
O1 O 0.5328(10) 0.6372(8) 0.4275(6) 0.0187(13) Uani 1 1 d . . .
O2 O 0.4741(9) 0.6647(8) 0.6764(6) 0.0183(13) Uani 1 1 d . . .
O3 O 0.6891(9) 0.4048(9) 1.0694(6) 0.0198(13) Uani 1 1 d . . .
O4 O 0.6700(10) 0.3790(9) 0.8181(6) 0.0204(14) Uani 1 1 d . . .
C1 C 0.4787(15) 0.8126(12) 0.4716(9) 0.0195(18) Uani 1 1 d U . .
H1A H 0.3939 0.9077 0.4098 0.023 Uiso 1 1 calc R . .
H1B H 0.5965 0.8292 0.4848 0.023 Uiso 1 1 calc R . .
C2 C 0.3707(15) 0.8251(12) 0.5930(8) 0.0205(18) Uani 1 1 d U . .
H2A H 0.3601 0.9303 0.6318 0.025 Uiso 1 1 calc R . .
H2B H 0.2379 0.8400 0.5759 0.025 Uiso 1 1 calc R . .
C3 C 0.8578(16) 0.2753(15) 1.0144(10) 0.030(2) Uani 1 1 d U . .
H3A H 0.9239 0.1684 1.0728 0.036 Uiso 1 1 calc R . .
H3B H 0.9501 0.3260 0.9938 0.036 Uiso 1 1 calc R . .
C4 C 0.7945(16) 0.2237(14) 0.8980(9) 0.027(2) Uani 1 1 d U . .
H4A H 0.9109 0.1501 0.8537 0.032 Uiso 1 1 calc R . .
H4B H 0.7245 0.1514 0.9210 0.032 Uiso 1 1 calc R . .


_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 O2 2.287(6) . ?
Pb1 O1 2.350(7) 2_666 ?
Pb1 O4 2.421(6) . ?
Pb1 O1 2.451(7) . ?
Pb1 Cd1 3.453(2) 2_666 ?
Pb2 O4 2.308(7) . ?
Pb2 O3 2.313(7) 2_667 ?
Pb2 O2 2.434(6) . ?
Pb2 O3 2.567(7) . ?
Pb2 Cd1 3.4612(19) 2_666 ?
Cd1 O1 2.280(6) . ?
Cd1 O3 2.282(6) 1_554 ?
Cd1 O4 2.500(7) 2_666 ?
Cd1 O2 2.542(7) 2_666 ?
Cd1 Br2 2.643(2) . ?
Cd1 Br1 2.700(2) . ?
Cd1 Pb1 3.453(2) 2_666 ?
Cd1 Pb2 3.4612(19) 2_666 ?
O1 C1 1.446(10) . ?
O1 Pb1 2.350(7) 2_666 ?
O2 C2 1.434(10) . ?
O2 Cd1 2.542(7) 2_666 ?
O3 C3 1.419(12) . ?
O3 Cd1 2.282(6) 1_556 ?
O3 Pb2 2.313(7) 2_667 ?
O4 C4 1.422(11) . ?
O4 Cd1 2.500(7) 2_666 ?
C1 C2 1.521(13) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.510(14) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 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
O2 Pb1 O1 75.7(2) . 2_666 ?
O2 Pb1 O4 64.9(2) . . ?
O1 Pb1 O4 81.7(2) 2_666 . ?
O2 Pb1 O1 70.4(2) . . ?
O1 Pb1 O1 72.8(2) 2_666 . ?
O4 Pb1 O1 132.6(2) . . ?
O2 Pb1 Cd1 47.39(17) . 2_666 ?
O1 Pb1 Cd1 41.00(16) 2_666 2_666 ?
O4 Pb1 Cd1 46.38(17) . 2_666 ?
O1 Pb1 Cd1 91.26(16) . 2_666 ?
O4 Pb2 O3 75.7(2) . 2_667 ?
O4 Pb2 O2 64.4(2) . . ?
O3 Pb2 O2 81.5(2) 2_667 . ?
O4 Pb2 O3 68.5(2) . . ?
O3 Pb2 O3 73.5(2) 2_667 . ?
O2 Pb2 O3 130.6(2) . . ?
O4 Pb2 Cd1 46.21(18) . 2_666 ?
O3 Pb2 Cd1 40.79(16) 2_667 2_666 ?
O2 Pb2 Cd1 47.23(15) . 2_666 ?
O3 Pb2 Cd1 88.98(16) . 2_666 ?
O1 Cd1 O3 148.6(2) . 1_554 ?
O1 Cd1 O4 81.3(2) . 2_666 ?
O3 Cd1 O4 72.6(2) 1_554 2_666 ?
O1 Cd1 O2 72.1(2) . 2_666 ?
O3 Cd1 O2 79.8(2) 1_554 2_666 ?
O4 Cd1 O2 60.2(2) 2_666 2_666 ?
O1 Cd1 Br2 97.27(16) . . ?
O3 Cd1 Br2 103.09(18) 1_554 . ?
O4 Cd1 Br2 97.36(15) 2_666 . ?
O2 Cd1 Br2 155.87(15) 2_666 . ?
O1 Cd1 Br1 101.91(18) . . ?
O3 Cd1 Br1 94.33(17) 1_554 . ?
O4 Cd1 Br1 153.74(15) 2_666 . ?
O2 Cd1 Br1 95.61(16) 2_666 . ?
Br2 Cd1 Br1 107.92(6) . . ?
O1 Cd1 Pb1 42.54(16) . 2_666 ?
O3 Cd1 Pb1 106.26(17) 1_554 2_666 ?
O4 Cd1 Pb1 44.51(15) 2_666 2_666 ?
O2 Cd1 Pb1 41.46(15) 2_666 2_666 ?
Br2 Cd1 Pb1 116.73(5) . 2_666 ?
Br1 Cd1 Pb1 123.87(6) . 2_666 ?
O1 Cd1 Pb2 107.11(16) . 2_666 ?
O3 Cd1 Pb2 41.48(17) 1_554 2_666 ?
O4 Cd1 Pb2 41.80(15) 2_666 2_666 ?
O2 Cd1 Pb2 44.64(15) 2_666 2_666 ?
Br2 Cd1 Pb2 124.61(5) . 2_666 ?
Br1 Cd1 Pb2 114.20(7) . 2_666 ?
Pb1 Cd1 Pb2 64.93(5) 2_666 2_666 ?
C1 O1 Cd1 126.3(5) . . ?
C1 O1 Pb1 113.8(5) . 2_666 ?
Cd1 O1 Pb1 96.5(2) . 2_666 ?
C1 O1 Pb1 102.4(5) . . ?
Cd1 O1 Pb1 109.8(3) . . ?
Pb1 O1 Pb1 107.2(2) 2_666 . ?
C2 O2 Pb1 117.7(5) . . ?
C2 O2 Pb2 125.4(5) . . ?
Pb1 O2 Pb2 103.6(2) . . ?
C2 O2 Cd1 122.8(6) . 2_666 ?
Pb1 O2 Cd1 91.1(2) . 2_666 ?
Pb2 O2 Cd1 88.1(2) . 2_666 ?
C3 O3 Cd1 127.9(6) . 1_556 ?
C3 O3 Pb2 119.0(6) . 2_667 ?
Cd1 O3 Pb2 97.7(2) 1_556 2_667 ?
C3 O3 Pb2 98.6(6) . . ?
Cd1 O3 Pb2 105.2(3) 1_556 . ?
Pb2 O3 Pb2 106.5(2) 2_667 . ?
C4 O4 Pb2 117.3(6) . . ?
C4 O4 Pb1 123.4(6) . . ?
Pb2 O4 Pb1 103.4(2) . . ?
C4 O4 Cd1 124.6(6) . 2_666 ?
Pb2 O4 Cd1 92.0(2) . 2_666 ?
Pb1 O4 Cd1 89.1(2) . 2_666 ?
O1 C1 C2 109.6(7) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
O2 C2 C1 110.7(8) . . ?
O2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
O3 C3 C4 109.4(8) . . ?
O3 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
O3 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
O4 C4 C3 111.8(9) . . ?
O4 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
O4 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?

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
O3 Cd1 O1 C1 -134.2(7) 1_554 . . . ?
O4 Cd1 O1 C1 -100.3(7) 2_666 . . . ?
O2 Cd1 O1 C1 -161.6(7) 2_666 . . . ?
Br2 Cd1 O1 C1 -3.9(7) . . . . ?
Br1 Cd1 O1 C1 106.2(7) . . . . ?
Pb1 Cd1 O1 C1 -126.0(8) 2_666 . . . ?
Pb2 Cd1 O1 C1 -133.5(6) 2_666 . . . ?
O3 Cd1 O1 Pb1 -8.2(5) 1_554 . . 2_666 ?
O4 Cd1 O1 Pb1 25.7(2) 2_666 . . 2_666 ?
O2 Cd1 O1 Pb1 -35.7(2) 2_666 . . 2_666 ?
Br2 Cd1 O1 Pb1 122.11(17) . . . 2_666 ?
Br1 Cd1 O1 Pb1 -127.78(17) . . . 2_666 ?
Pb2 Cd1 O1 Pb1 -7.6(2) 2_666 . . 2_666 ?
O3 Cd1 O1 Pb1 102.7(4) 1_554 . . . ?
O4 Cd1 O1 Pb1 136.6(3) 2_666 . . . ?
O2 Cd1 O1 Pb1 75.2(3) 2_666 . . . ?
Br2 Cd1 O1 Pb1 -127.0(2) . . . . ?
Br1 Cd1 O1 Pb1 -16.9(2) . . . . ?
Pb1 Cd1 O1 Pb1 110.9(3) 2_666 . . . ?
Pb2 Cd1 O1 Pb1 103.3(2) 2_666 . . . ?
O2 Pb1 O1 C1 39.5(5) . . . . ?
O1 Pb1 O1 C1 120.1(6) 2_666 . . . ?
O4 Pb1 O1 C1 59.5(6) . . . . ?
Cd1 Pb1 O1 C1 82.9(5) 2_666 . . . ?
O2 Pb1 O1 Cd1 175.8(3) . . . . ?
O1 Pb1 O1 Cd1 -103.7(3) 2_666 . . . ?
O4 Pb1 O1 Cd1 -164.2(2) . . . . ?
Cd1 Pb1 O1 Cd1 -140.8(2) 2_666 . . . ?
O2 Pb1 O1 Pb1 -80.5(3) . . . 2_666 ?
O1 Pb1 O1 Pb1 0.0 2_666 . . 2_666 ?
O4 Pb1 O1 Pb1 -60.6(4) . . . 2_666 ?
Cd1 Pb1 O1 Pb1 -37.2(2) 2_666 . . 2_666 ?
O1 Pb1 O2 C2 -94.0(6) 2_666 . . . ?
O4 Pb1 O2 C2 178.7(7) . . . . ?
O1 Pb1 O2 C2 -17.4(6) . . . . ?
Cd1 Pb1 O2 C2 -128.5(7) 2_666 . . . ?
O1 Pb1 O2 Pb2 122.9(3) 2_666 . . . ?
O4 Pb1 O2 Pb2 35.5(2) . . . . ?
O1 Pb1 O2 Pb2 -160.5(3) . . . . ?
Cd1 Pb1 O2 Pb2 88.4(2) 2_666 . . . ?
O1 Pb1 O2 Cd1 34.56(19) 2_666 . . 2_666 ?
O4 Pb1 O2 Cd1 -52.8(2) . . . 2_666 ?
O1 Pb1 O2 Cd1 111.1(2) . . . 2_666 ?
O4 Pb2 O2 C2 -177.1(7) . . . . ?
O3 Pb2 O2 C2 104.8(7) 2_667 . . . ?
O3 Pb2 O2 C2 164.3(6) . . . . ?
Cd1 Pb2 O2 C2 130.0(7) 2_666 . . . ?
O4 Pb2 O2 Pb1 -37.8(2) . . . . ?
O3 Pb2 O2 Pb1 -115.9(3) 2_667 . . . ?
O3 Pb2 O2 Pb1 -56.4(4) . . . . ?
Cd1 Pb2 O2 Pb1 -90.7(2) 2_666 . . . ?
O4 Pb2 O2 Cd1 53.0(2) . . . 2_666 ?
O3 Pb2 O2 Cd1 -25.2(2) 2_667 . . 2_666 ?
O3 Pb2 O2 Cd1 34.3(3) . . . 2_666 ?
O4 Pb2 O3 C3 42.9(6) . . . . ?
O3 Pb2 O3 C3 123.8(7) 2_667 . . . ?
O2 Pb2 O3 C3 61.0(6) . . . . ?
Cd1 Pb2 O3 C3 85.5(6) 2_666 . . . ?
O4 Pb2 O3 Cd1 176.1(3) . . . 1_556 ?
O3 Pb2 O3 Cd1 -103.1(3) 2_667 . . 1_556 ?
O2 Pb2 O3 Cd1 -165.8(2) . . . 1_556 ?
Cd1 Pb2 O3 Cd1 -141.4(2) 2_666 . . 1_556 ?
O4 Pb2 O3 Pb2 -80.8(3) . . . 2_667 ?
O3 Pb2 O3 Pb2 0.0 2_667 . . 2_667 ?
O2 Pb2 O3 Pb2 -62.8(3) . . . 2_667 ?
Cd1 Pb2 O3 Pb2 -38.3(2) 2_666 . . 2_667 ?
O3 Pb2 O4 C4 -98.1(7) 2_667 . . . ?
O2 Pb2 O4 C4 174.6(7) . . . . ?
O3 Pb2 O4 C4 -20.5(6) . . . . ?
Cd1 Pb2 O4 C4 -131.1(7) 2_666 . . . ?
O3 Pb2 O4 Pb1 122.6(3) 2_667 . . . ?
O2 Pb2 O4 Pb1 35.3(2) . . . . ?
O3 Pb2 O4 Pb1 -159.8(3) . . . . ?
Cd1 Pb2 O4 Pb1 89.6(3) 2_666 . . . ?
O3 Pb2 O4 Cd1 33.0(2) 2_667 . . 2_666 ?
O2 Pb2 O4 Cd1 -54.3(2) . . . 2_666 ?
O3 Pb2 O4 Cd1 110.6(2) . . . 2_666 ?
O2 Pb1 O4 C4 -173.8(8) . . . . ?
O1 Pb1 O4 C4 108.1(7) 2_666 . . . ?
O1 Pb1 O4 C4 165.4(7) . . . . ?
Cd1 Pb1 O4 C4 132.1(8) 2_666 . . . ?
O2 Pb1 O4 Pb2 -37.7(2) . . . . ?
O1 Pb1 O4 Pb2 -115.8(3) 2_666 . . . ?
O1 Pb1 O4 Pb2 -58.5(4) . . . . ?
Cd1 Pb1 O4 Pb2 -91.8(3) 2_666 . . . ?
O2 Pb1 O4 Cd1 54.1(2) . . . 2_666 ?
O1 Pb1 O4 Cd1 -23.9(2) 2_666 . . 2_666 ?
O1 Pb1 O4 Cd1 33.3(3) . . . 2_666 ?
Cd1 O1 C1 C2 175.6(6) . . . . ?
Pb1 O1 C1 C2 57.1(8) 2_666 . . . ?
Pb1 O1 C1 C2 -58.2(8) . . . . ?
Pb1 O2 C2 C1 -7.6(10) . . . . ?
Pb2 O2 C2 C1 126.7(6) . . . . ?
Cd1 O2 C2 C1 -119.0(7) 2_666 . . . ?
O1 C1 C2 O2 46.8(10) . . . . ?
Cd1 O3 C3 C4 -178.7(6) 1_556 . . . ?
Pb2 O3 C3 C4 52.6(10) 2_667 . . . ?
Pb2 O3 C3 C4 -61.8(9) . . . . ?
Pb2 O4 C4 C3 -5.0(11) . . . . ?
Pb1 O4 C4 C3 125.6(8) . . . . ?
Cd1 O4 C4 C3 -118.7(8) 2_666 . . . ?
O3 C3 C4 O4 50.1(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.95
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.238
_refine_diff_density_min         -2.635
_refine_diff_density_rms         0.353
####################################################################### 
# 
# 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_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1819918'
_audit_update_record             
;
2018-01-28 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H16 Br6 Cd O8 Pb6'
_chemical_formula_sum            'C8 H16 Br6 Cd O8 Pb6'
_chemical_formula_weight         2075.22

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'
O O 0.0106 0.0060 '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'
Cd Cd -0.8075 1.2024 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   9.4173(9)
_cell_length_b                   13.6560(11)
_cell_length_c                   21.909(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.965(4)
_cell_angle_gamma                90.00
_cell_volume                     2783.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    28432
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      27.90

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3512
_exptl_absorpt_coefficient_mu    45.552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1920
_exptl_absorpt_correction_T_max  0.6386
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28432
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.65
_diffrn_reflns_theta_max         27.90
_reflns_number_total             3305
_reflns_number_gt                2888
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0443P)²+390.5807P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000109(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3305
_refine_ls_number_parameters     134
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1237
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb -0.07939(6) 0.35447(4) 0.54485(3) 0.02133(17) Uani 1 1 d . . .
Pb2 Pb 0.65093(7) 0.49802(5) 0.64317(3) 0.02789(19) Uani 1 1 d . . .
Pb3 Pb 0.76548(6) 0.50271(4) 0.83909(3) 0.02305(17) Uani 1 1 d . . .
Cd1 Cd 0.5000 0.34034(12) 0.7500 0.0204(3) Uani 1 2 d S . .
Br1 Br 0.5000 0.59647(16) 0.7500 0.0254(5) Uani 1 2 d S . .
Br2 Br -0.08209(19) 0.56410(12) 0.56675(8) 0.0288(4) Uani 1 1 d . . .
Br3 Br -0.38245(18) 0.39193(12) 0.45332(8) 0.0279(4) Uani 1 1 d . . .
Br4 Br 0.5000 0.13905(12) 0.7500 0.0135(4) Uani 1 2 d S . .
O1 O 0.2896(12) 0.4086(9) 0.7630(5) 0.024(2) Uani 1 1 d . . .
O2 O 0.2332(14) 0.3606(9) 0.8824(6) 0.034(3) Uani 1 1 d . . .
O3 O 0.1390(12) 0.3632(9) 0.6145(6) 0.030(3) Uani 1 1 d . . .
O4 O 0.4357(11) 0.4022(8) 0.6497(5) 0.022(2) Uani 1 1 d . . .
C1 C 0.178(2) 0.3426(17) 0.7717(9) 0.040(5) Uani 1 1 d . . .
H1A H 0.1675 0.2940 0.7390 0.048 Uiso 1 1 calc R . .
H1B H 0.0886 0.3781 0.7693 0.048 Uiso 1 1 calc R . .
C2 C 0.211(2) 0.2921(13) 0.8331(9) 0.037(4) Uani 1 1 d . . .
H2A H 0.1308 0.2496 0.8384 0.044 Uiso 1 1 calc R . .
H2B H 0.2956 0.2518 0.8341 0.044 Uiso 1 1 calc R . .
C3 C 0.3861(19) 0.3355(13) 0.5994(8) 0.027(3) Uani 1 1 d . . .
H3A H 0.4568 0.2842 0.5983 0.032 Uiso 1 1 calc R . .
H3B H 0.3759 0.3707 0.5605 0.032 Uiso 1 1 calc R . .
C4 C 0.2442(18) 0.2905(12) 0.6071(9) 0.028(4) Uani 1 1 d . . .
H4A H 0.2096 0.2509 0.5711 0.034 Uiso 1 1 calc R . .
H4B H 0.2576 0.2479 0.6429 0.034 Uiso 1 1 calc R . .


_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 O2 2.316(11) 2_556 ?
Pb1 O3 2.365(11) . ?
Pb1 Br2 2.9034(17) . ?
Pb2 O2 2.285(11) 2_656 ?
Pb2 O1 2.382(12) 2_656 ?
Pb2 O4 2.435(11) . ?
Pb2 Br1 3.2159(12) . ?
Pb3 O3 2.277(12) 2_656 ?
Pb3 O4 2.384(10) 2_656 ?
Pb3 O1 2.561(11) 2_656 ?
Pb3 Br1 3.1904(11) . ?
Cd1 O1 2.248(11) 2_656 ?
Cd1 O1 2.248(11) . ?
Cd1 O4 2.345(11) 2_656 ?
Cd1 O4 2.345(11) . ?
Cd1 Br4 2.749(2) . ?
Br1 Pb3 3.1904(11) 2_656 ?
Br1 Pb2 3.2159(12) 2_656 ?
O1 C1 1.42(2) . ?
O1 Pb2 2.382(12) 2_656 ?
O1 Pb3 2.561(11) 2_656 ?
O2 C2 1.42(2) . ?
O2 Pb2 2.285(11) 2_656 ?
O2 Pb1 2.316(11) 2_556 ?
O3 C4 1.430(19) . ?
O3 Pb3 2.277(12) 2_656 ?
O4 C3 1.448(19) . ?
O4 Pb3 2.384(10) 2_656 ?
C1 C2 1.50(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.50(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 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
O2 Pb1 O3 97.4(5) 2_556 . ?
O2 Pb1 Br2 80.1(3) 2_556 . ?
O3 Pb1 Br2 82.7(3) . . ?
O2 Pb2 O1 74.5(4) 2_656 2_656 ?
O2 Pb2 O4 90.4(4) 2_656 . ?
O1 Pb2 O4 76.1(4) 2_656 . ?
O2 Pb2 Br1 143.5(3) 2_656 . ?
O1 Pb2 Br1 70.0(3) 2_656 . ?
O4 Pb2 Br1 73.5(3) . . ?
O3 Pb3 O4 74.8(4) 2_656 2_656 ?
O3 Pb3 O1 89.0(4) 2_656 2_656 ?
O4 Pb3 O1 75.2(4) 2_656 2_656 ?
O3 Pb3 Br1 145.7(3) 2_656 . ?
O4 Pb3 Br1 74.6(3) 2_656 . ?
O1 Pb3 Br1 68.6(2) 2_656 . ?
O1 Cd1 O1 131.0(6) 2_656 . ?
O1 Cd1 O4 82.3(4) 2_656 2_656 ?
O1 Cd1 O4 80.6(4) . 2_656 ?
O1 Cd1 O4 80.6(4) 2_656 . ?
O1 Cd1 O4 82.3(4) . . ?
O4 Cd1 O4 137.8(5) 2_656 . ?
O1 Cd1 Br4 114.5(3) 2_656 . ?
O1 Cd1 Br4 114.5(3) . . ?
O4 Cd1 Br4 111.1(3) 2_656 . ?
O4 Cd1 Br4 111.1(3) . . ?
Pb3 Br1 Pb3 132.68(8) 2_656 . ?
Pb3 Br1 Pb2 77.29(3) 2_656 . ?
Pb3 Br1 Pb2 83.36(3) . . ?
Pb3 Br1 Pb2 83.36(3) 2_656 2_656 ?
Pb3 Br1 Pb2 77.29(3) . 2_656 ?
Pb2 Br1 Pb2 130.58(8) . 2_656 ?
C1 O1 Cd1 116.0(12) . . ?
C1 O1 Pb2 106.8(10) . 2_656 ?
Cd1 O1 Pb2 103.2(4) . 2_656 ?
C1 O1 Pb3 112.6(10) . 2_656 ?
Cd1 O1 Pb3 99.2(4) . 2_656 ?
Pb2 O1 Pb3 119.0(5) 2_656 2_656 ?
C2 O2 Pb2 112.1(10) . 2_656 ?
C2 O2 Pb1 117.6(10) . 2_556 ?
Pb2 O2 Pb1 124.9(5) 2_656 2_556 ?
C4 O3 Pb3 113.5(9) . 2_656 ?
C4 O3 Pb1 116.1(10) . . ?
Pb3 O3 Pb1 125.0(5) 2_656 . ?
C3 O4 Cd1 119.4(10) . . ?
C3 O4 Pb3 105.8(9) . 2_656 ?
Cd1 O4 Pb3 101.8(4) . 2_656 ?
C3 O4 Pb2 117.8(9) . . ?
Cd1 O4 Pb2 98.8(4) . . ?
Pb3 O4 Pb2 112.2(4) 2_656 . ?
O1 C1 C2 111.4(15) . . ?
O1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
O1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
O2 C2 C1 111.4(16) . . ?
O2 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
O2 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
O4 C3 C4 111.1(14) . . ?
O4 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
O4 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
O3 C4 C3 111.9(14) . . ?
O3 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
O3 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.90
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         3.290
_refine_diff_density_min         -2.007
_refine_diff_density_rms         0.459
