# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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. 
# 
#######################################################################

data_23025a
_database_code_depnum_ccdc_archive 'CCDC 2314262'
loop_
_audit_author_name
_audit_author_address
'Douglas R. Powell'
;University of Oklahoma
United States of America
;
_audit_update_record             
;
2023-12-13 deposited with the CCDC.	2024-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
#_shelx_SHELXL_version_number      '2018/3' 
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H8 Br4 Cu N2 O4 Pb2'
_chemical_formula_sum            'C4 H8 Br4 Cu N2 O4 Pb2'
_chemical_formula_weight         945.68

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'
N N 0.0061 0.0033 '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'
Cu Cu 0.3201 1.2651 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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. 
;

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                   8.5509(2)
_cell_length_b                   10.9451(3)
_cell_length_c                   8.3697(2)
_cell_angle_alpha                90
_cell_angle_beta                 108.7003(10)
_cell_angle_gamma                90
_cell_volume                     741.97(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9788
_cell_measurement_theta_min      3.13
_cell_measurement_theta_max      36.28

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.233
_exptl_crystal_F_000             822
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    34.826
_shelx_estimated_absorpt_T_min   0.083
_shelx_estimated_absorpt_T_max   0.229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3386
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
#_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40882
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.129
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1515
_reflns_number_gt                1492
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0100P)²+1.4000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     shelxt
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick, 2015b)'
_refine_ls_extinction_coef       0.0079(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1515
_refine_ls_number_parameters     86
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0134
_refine_ls_R_factor_gt           0.0131
_refine_ls_wR_factor_ref         0.0298
_refine_ls_wR_factor_gt          0.0297
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.002
_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_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 0.50919(2) 0.70010(2) 0.63273(2) 0.01903(6) Uani 1 1 d . . . . .
Br1 Br 0.60113(4) 0.44554(3) 0.72215(4) 0.01925(8) Uani 1 1 d . . . . .
Br2 Br 0.79076(4) 0.75829(3) 0.97054(4) 0.02220(9) Uani 1 1 d . . . . .
Cu1 Cu 0.000000 0.500000 0.500000 0.02486(14) Uani 1 2 d S . P . .
O1 O 0.3613(3) 0.6614(2) 0.8544(3) 0.0244(5) Uani 1 1 d . . . . .
O2 O 0.2003(3) 0.5971(2) 0.6073(3) 0.0207(5) Uani 1 1 d . . . . .
N1 N 0.0014(4) 0.4709(3) 0.7322(3) 0.0223(6) Uani 1 1 d . . . . .
H1NA H -0.094(5) 0.472(4) 0.741(5) 0.027 Uiso 1 1 d . U . . .
H1NB H 0.038(5) 0.400(4) 0.762(5) 0.027 Uiso 1 1 d . U . . .
C1 C 0.2335(4) 0.6095(3) 0.7650(4) 0.0174(6) Uani 1 1 d . . . . .
C2 C 0.1134(4) 0.5582(3) 0.8463(4) 0.0240(7) Uani 1 1 d . . . . .
H2A H 0.174950 0.516762 0.953136 0.029 Uiso 1 1 calc R U . . .
H2B H 0.048562 0.625560 0.873058 0.029 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
Pb1 O1 2.593(2) . ?
Pb1 O1 2.727(2) 4_575 ?
Pb1 Br1 2.9265(3) . ?
Pb1 Br2 3.1355(3) . ?
Pb1 Br2 3.1532(3) 4_575 ?
Pb1 Br1 3.2119(3) 2_656 ?
Pb1 Br1 3.2336(3) 3_666 ?
Cu1 N1 1.965(3) . ?
Cu1 N1 1.965(3) 3_566 ?
Cu1 O2 1.970(2) 3_566 ?
Cu1 O2 1.970(2) . ?
O1 C1 1.245(4) . ?
O2 C1 1.265(4) . ?
N1 C2 1.469(4) . ?
N1 H1NA 0.84(4) . ?
N1 H1NB 0.84(5) . ?
C1 C2 1.511(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?

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
O1 Pb1 O1 120.20(9) . 4_575 ?
O1 Pb1 Br1 79.29(6) . . ?
O1 Pb1 Br1 139.53(5) 4_575 . ?
O1 Pb1 Br2 78.33(5) . . ?
O1 Pb1 Br2 132.00(6) 4_575 . ?
Br1 Pb1 Br2 84.094(9) . . ?
O1 Pb1 Br2 161.16(5) . 4_575 ?
O1 Pb1 Br2 76.17(5) 4_575 4_575 ?
Br1 Pb1 Br2 93.899(9) . 4_575 ?
Br2 Pb1 Br2 83.531(8) . 4_575 ?
O1 Pb1 Br1 66.20(6) . 2_656 ?
O1 Pb1 Br1 75.29(5) 4_575 2_656 ?
Br1 Pb1 Br1 141.903(5) . 2_656 ?
Br2 Pb1 Br1 73.909(8) . 2_656 ?
Br2 Pb1 Br1 113.541(9) 4_575 2_656 ?
O1 Pb1 Br1 120.73(5) . 3_666 ?
O1 Pb1 Br1 64.56(5) 4_575 3_666 ?
Br1 Pb1 Br1 74.986(9) . 3_666 ?
Br2 Pb1 Br1 147.346(9) . 3_666 ?
Br2 Pb1 Br1 73.375(8) 4_575 3_666 ?
Br1 Pb1 Br1 136.476(10) 2_656 3_666 ?
Pb1 Br1 Pb1 143.669(11) . 2_646 ?
Pb1 Br1 Pb1 105.015(9) . 3_666 ?
Pb1 Br1 Pb1 84.290(8) 2_646 3_666 ?
Pb1 Br2 Pb1 86.904(8) . 4_576 ?
N1 Cu1 N1 180.0 . 3_566 ?
N1 Cu1 O2 95.28(10) . 3_566 ?
N1 Cu1 O2 84.72(10) 3_566 3_566 ?
N1 Cu1 O2 84.72(10) . . ?
N1 Cu1 O2 95.28(10) 3_566 . ?
O2 Cu1 O2 180.0 3_566 . ?
C1 O1 Pb1 100.36(19) . . ?
C1 O1 Pb1 147.5(2) . 4_576 ?
Pb1 O1 Pb1 108.74(8) . 4_576 ?
C1 O2 Cu1 113.92(19) . . ?
C2 N1 Cu1 109.5(2) . . ?
C2 N1 H1NA 113(3) . . ?
Cu1 N1 H1NA 112(3) . . ?
C2 N1 H1NB 108(3) . . ?
Cu1 N1 H1NB 109(3) . . ?
H1NA N1 H1NB 105(4) . . ?
O1 C1 O2 122.4(3) . . ?
O1 C1 C2 119.4(3) . . ?
O2 C1 C2 118.2(3) . . ?
N1 C2 C1 110.1(3) . . ?
N1 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?

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 C1 O2 -5.1(3) . . . . ?
Pb1 O1 C1 O2 148.5(3) 4_576 . . . ?
Pb1 O1 C1 C2 174.3(2) . . . . ?
Pb1 O1 C1 C2 -32.0(6) 4_576 . . . ?
Cu1 O2 C1 O1 175.3(2) . . . . ?
Cu1 O2 C1 C2 -4.2(4) . . . . ?
Cu1 N1 C2 C1 -20.1(3) . . . . ?
O1 C1 C2 N1 -162.9(3) . . . . ?
O2 C1 C2 N1 16.6(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1NA Br1 0.84(4) 2.58(4) 3.408(3) 170(4) 1_455 yes
N1 H1NB Br2 0.84(5) 2.84(5) 3.578(3) 147(4) 3_667 yes
C2 H2A Br1 0.99 2.81 3.654(3) 143.8 3_667 yes
C2 H2A Br2 0.99 3.07 3.770(4) 128.7 3_667 yes
C2 H2B Br2 0.99 2.96 3.915(4) 161.2 1_455 yes

_refine_diff_density_max         0.768
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.165



####################################################################### 
# 
# 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_23078
_database_code_depnum_ccdc_archive 'CCDC 2314263'
loop_
_audit_author_name
_audit_author_address
'Douglas R. Powell'
;University of Oklahoma
United States of America
;
_audit_update_record             
;
2023-12-13 deposited with the CCDC.	2024-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
#_shelx_SHELXL_version_number      '2018/3' 
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H18 Br4 Cu N2 O4 Pb'
_chemical_formula_sum            'C8 H18 Br4 Cu N2 O4 Pb'
_chemical_formula_weight         796.61

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'
N N 0.0061 0.0033 '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'
Cu Cu 0.3201 1.2651 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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. 
;

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

_cell_length_a                   8.4521(7)
_cell_length_b                   8.3195(7)
_cell_length_c                   26.858(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.396(3)
_cell_angle_gamma                90
_cell_volume                     1868.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9935
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      33.51

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.832
_exptl_crystal_F_000             1452
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    18.701
_shelx_estimated_absorpt_T_min   0.134
_shelx_estimated_absorpt_T_max   0.400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2995
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_process_details   
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
#_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            77900
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.444
_diffrn_reflns_theta_max         33.787
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7485
_reflns_number_gt                6125
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_molecular_graphics    'Mercury (CCDC, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2015b)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0326P)²+2.1362P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     shelxt
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick, 2015b)'
_refine_ls_extinction_coef       0.00879(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7485
_refine_ls_number_parameters     200
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0696
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.002
_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_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 0.50976(2) 0.49993(2) 0.24772(2) 0.01877(4) Uani 1 1 d . . . . .
Br1 Br 0.54891(4) 0.39650(4) 0.35970(2) 0.02523(7) Uani 1 1 d . . . . .
Br2 Br 0.23518(4) 0.72381(4) 0.26259(2) 0.02740(7) Uani 1 1 d . . . . .
Br3 Br 0.42664(5) 0.54648(5) 0.14119(2) 0.03332(8) Uani 1 1 d . . . . .
Br4 Br 0.70424(5) 0.79916(5) 0.26455(2) 0.03641(9) Uani 1 1 d . . . . .
Cu1 Cu 0.52222(4) 0.44714(4) 0.45518(2) 0.01714(7) Uani 1 1 d . . . . .
O1A O 0.6224(3) 0.6581(3) 0.45384(9) 0.0270(5) Uani 1 1 d . . . . .
O2A O 0.5813(3) 0.7530(3) 0.52866(9) 0.0308(5) Uani 1 1 d . . . . .
N1A N 0.4825(5) 1.0084(4) 0.34069(14) 0.0362(8) Uani 1 1 d D . . . .
H1A1 H 0.515(5) 1.111(3) 0.3388(17) 0.043 Uiso 1 1 d D U . . .
H1A2 H 0.380(3) 0.997(5) 0.3266(18) 0.043 Uiso 1 1 d D U . . .
H1A3 H 0.548(5) 0.957(5) 0.3219(16) 0.043 Uiso 1 1 d D U . . .
C1A C 0.6289(4) 0.7669(3) 0.48674(11) 0.0203(5) Uani 1 1 d . . . . .
C2A C 0.6968(4) 0.9276(4) 0.47421(12) 0.0237(6) Uani 1 1 d . . . . .
H2AA H 0.811768 0.930795 0.488197 0.028 Uiso 1 1 calc R U . . .
H2AB H 0.642504 1.013536 0.490840 0.028 Uiso 1 1 calc R U . . .
C3A C 0.6785(4) 0.9630(4) 0.41764(13) 0.0269(6) Uani 1 1 d . . . . .
H3AA H 0.721306 1.071391 0.412242 0.032 Uiso 1 1 calc R U . . .
H3AB H 0.740967 0.883763 0.401090 0.032 Uiso 1 1 calc R U . . .
C4A C 0.5053(4) 0.9549(5) 0.39442(13) 0.0302(7) Uani 1 1 d . . . . .
H4AA H 0.466470 0.843145 0.396274 0.036 Uiso 1 1 calc R U . . .
H4AB H 0.441079 1.024154 0.413799 0.036 Uiso 1 1 calc R U . . .
O1B O 0.3076(3) 0.5444(3) 0.43678(9) 0.0292(5) Uani 1 1 d . . . . .
O2B O 0.2727(3) 0.6374(3) 0.51208(8) 0.0278(5) Uani 1 1 d . . . . .
N1B N 0.1316(4) 0.4457(4) 0.34737(11) 0.0307(6) Uani 1 1 d D . . . .
H1B1 H 0.150(6) 0.469(5) 0.3160(10) 0.037 Uiso 1 1 d D U . . .
H1B2 H 0.106(5) 0.343(3) 0.3521(16) 0.037 Uiso 1 1 d D U . . .
H1B3 H 0.213(4) 0.470(5) 0.3715(14) 0.037 Uiso 1 1 d D U . . .
C1B C 0.2244(4) 0.6107(4) 0.46665(12) 0.0212(5) Uani 1 1 d . . . . .
C2B C 0.0558(4) 0.6594(4) 0.44612(13) 0.0287(7) Uani 1 1 d . . . . .
H2BA H 0.059683 0.762851 0.428102 0.034 Uiso 1 1 calc R U . . .
H2BB H -0.003307 0.678249 0.474812 0.034 Uiso 1 1 calc R U . . .
C3B C -0.0385(5) 0.5391(6) 0.41049(17) 0.0419(9) Uani 1 1 d . . . . .
H3BA H -0.013896 0.430130 0.424298 0.050 Uiso 1 1 calc R U . . .
H3BB H -0.153657 0.558447 0.411338 0.050 Uiso 1 1 calc R U . . .
C4B C -0.0132(6) 0.5377(7) 0.35657(17) 0.0479(11) Uani 1 1 d . . . . .
H4BA H -0.108540 0.490158 0.336038 0.057 Uiso 1 1 calc R U . . .
H4BB H -0.003179 0.649918 0.345181 0.057 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
Pb1 Br3 2.8711(4) . ?
Pb1 Br4 2.9810(4) . ?
Pb1 Br4 2.9958(4) 2_645 ?
Pb1 Br2 3.0472(4) . ?
Pb1 Br2 3.0777(4) 2_545 ?
Pb1 Br1 3.0992(4) . ?
Br1 Cu1 2.6408(5) . ?
Cu1 O1A 1.951(2) . ?
Cu1 O2B 1.956(2) 3_666 ?
Cu1 O2A 1.959(2) 3_666 ?
Cu1 O1B 1.982(2) . ?
Cu1 Cu1 2.6408(7) 3_666 ?
O1A C1A 1.260(4) . ?
O2A C1A 1.255(4) . ?
N1A C4A 1.496(5) . ?
N1A H1A1 0.90(2) . ?
N1A H1A2 0.90(2) . ?
N1A H1A3 0.91(2) . ?
C1A C2A 1.513(4) . ?
C2A C3A 1.533(5) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C3A C4A 1.506(5) . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
O1B C1B 1.268(4) . ?
O2B C1B 1.248(4) . ?
N1B C4B 1.494(5) . ?
N1B H1B1 0.90(2) . ?
N1B H1B2 0.90(2) . ?
N1B H1B3 0.90(2) . ?
C1B C2B 1.507(4) . ?
C2B C3B 1.527(5) . ?
C2B H2BA 0.9900 . ?
C2B H2BB 0.9900 . ?
C3B C4B 1.494(6) . ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C4B H4BA 0.9900 . ?
C4B H4BB 0.9900 . ?

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
Br3 Pb1 Br4 95.031(13) . . ?
Br3 Pb1 Br4 92.839(12) . 2_645 ?
Br4 Pb1 Br4 92.658(8) . 2_645 ?
Br3 Pb1 Br2 88.164(11) . . ?
Br4 Pb1 Br2 83.300(12) . . ?
Br4 Pb1 Br2 175.908(11) 2_645 . ?
Br3 Pb1 Br2 86.988(11) . 2_545 ?
Br4 Pb1 Br2 170.308(11) . 2_545 ?
Br4 Pb1 Br2 96.714(13) 2_645 2_545 ?
Br2 Pb1 Br2 87.297(8) . 2_545 ?
Br3 Pb1 Br1 168.661(12) . . ?
Br4 Pb1 Br1 96.107(11) . . ?
Br4 Pb1 Br1 88.764(11) 2_645 . ?
Br2 Pb1 Br1 91.027(10) . . ?
Br2 Pb1 Br1 81.676(10) 2_545 . ?
Cu1 Br1 Pb1 152.369(16) . . ?
Pb1 Br2 Pb1 163.658(14) . 2 ?
Pb1 Br4 Pb1 152.236(16) . 2_655 ?
O1A Cu1 O2B 88.47(11) . 3_666 ?
O1A Cu1 O2A 167.88(10) . 3_666 ?
O2B Cu1 O2A 89.42(11) 3_666 3_666 ?
O1A Cu1 O1B 90.67(11) . . ?
O2B Cu1 O1B 167.82(10) 3_666 . ?
O2A Cu1 O1B 88.87(12) 3_666 . ?
O1A Cu1 Cu1 80.63(7) . 3_666 ?
O2B Cu1 Cu1 86.82(7) 3_666 3_666 ?
O2A Cu1 Cu1 87.34(7) 3_666 3_666 ?
O1B Cu1 Cu1 81.05(7) . 3_666 ?
O1A Cu1 Br1 91.53(7) . . ?
O2B Cu1 Br1 100.57(7) 3_666 . ?
O2A Cu1 Br1 100.59(7) 3_666 . ?
O1B Cu1 Br1 91.60(7) . . ?
Cu1 Cu1 Br1 169.13(2) 3_666 . ?
C1A O1A Cu1 127.4(2) . . ?
C1A O2A Cu1 119.3(2) . 3_666 ?
C4A N1A H1A1 110(3) . . ?
C4A N1A H1A2 111(3) . . ?
H1A1 N1A H1A2 111(4) . . ?
C4A N1A H1A3 113(3) . . ?
H1A1 N1A H1A3 101(4) . . ?
H1A2 N1A H1A3 110(4) . . ?
O2A C1A O1A 125.2(3) . . ?
O2A C1A C2A 117.6(3) . . ?
O1A C1A C2A 117.3(3) . . ?
C1A C2A C3A 113.8(3) . . ?
C1A C2A H2AA 108.8 . . ?
C3A C2A H2AA 108.8 . . ?
C1A C2A H2AB 108.8 . . ?
C3A C2A H2AB 108.8 . . ?
H2AA C2A H2AB 107.7 . . ?
C4A C3A C2A 110.7(3) . . ?
C4A C3A H3AA 109.5 . . ?
C2A C3A H3AA 109.5 . . ?
C4A C3A H3AB 109.5 . . ?
C2A C3A H3AB 109.5 . . ?
H3AA C3A H3AB 108.1 . . ?
N1A C4A C3A 111.5(3) . . ?
N1A C4A H4AA 109.3 . . ?
C3A C4A H4AA 109.3 . . ?
N1A C4A H4AB 109.3 . . ?
C3A C4A H4AB 109.3 . . ?
H4AA C4A H4AB 108.0 . . ?
C1B O1B Cu1 126.3(2) . . ?
C1B O2B Cu1 121.1(2) . 3_666 ?
C4B N1B H1B1 108(3) . . ?
C4B N1B H1B2 104(3) . . ?
H1B1 N1B H1B2 114(4) . . ?
C4B N1B H1B3 109(3) . . ?
H1B1 N1B H1B3 114(4) . . ?
H1B2 N1B H1B3 107(4) . . ?
O2B C1B O1B 124.3(3) . . ?
O2B C1B C2B 117.8(3) . . ?
O1B C1B C2B 117.9(3) . . ?
C1B C2B C3B 115.6(3) . . ?
C1B C2B H2BA 108.4 . . ?
C3B C2B H2BA 108.4 . . ?
C1B C2B H2BB 108.4 . . ?
C3B C2B H2BB 108.4 . . ?
H2BA C2B H2BB 107.4 . . ?
C4B C3B C2B 118.5(4) . . ?
C4B C3B H3BA 107.7 . . ?
C2B C3B H3BA 107.7 . . ?
C4B C3B H3BB 107.7 . . ?
C2B C3B H3BB 107.7 . . ?
H3BA C3B H3BB 107.1 . . ?
N1B C4B C3B 113.6(4) . . ?
N1B C4B H4BA 108.8 . . ?
C3B C4B H4BA 108.8 . . ?
N1B C4B H4BB 108.8 . . ?
C3B C4B H4BB 108.8 . . ?
H4BA C4B H4BB 107.7 . . ?

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
Cu1 O2A C1A O1A -3.3(4) 3_666 . . . ?
Cu1 O2A C1A C2A 175.5(2) 3_666 . . . ?
Cu1 O1A C1A O2A 5.7(5) . . . . ?
Cu1 O1A C1A C2A -173.1(2) . . . . ?
O2A C1A C2A C3A -152.7(3) . . . . ?
O1A C1A C2A C3A 26.2(4) . . . . ?
C1A C2A C3A C4A 56.9(4) . . . . ?
C2A C3A C4A N1A 173.1(3) . . . . ?
Cu1 O2B C1B O1B -8.1(5) 3_666 . . . ?
Cu1 O2B C1B C2B 171.4(2) 3_666 . . . ?
Cu1 O1B C1B O2B 6.8(5) . . . . ?
Cu1 O1B C1B C2B -172.7(2) . . . . ?
O2B C1B C2B C3B -138.1(3) . . . . ?
O1B C1B C2B C3B 41.5(5) . . . . ?
C1B C2B C3B C4B -81.6(5) . . . . ?
C2B C3B C4B N1B 81.7(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1A H1A1 Br1 0.90(2) 2.45(3) 3.304(3) 159(4) 1_565 yes
N1A H1A2 Br2 0.90(2) 3.00(4) 3.619(4) 127(3) . yes
N1A H1A2 Br2 0.90(2) 3.09(4) 3.578(4) 116(3) 2 yes
N1A H1A2 Br3 0.90(2) 2.88(4) 3.576(5) 136(4) 2 yes
N1A H1A3 Br4 0.91(2) 2.53(2) 3.441(4) 174(4) . yes
C4A H4AB O2A 0.99 2.44 3.339(5) 151.0 3_676 yes
C4A H4AA O1A 0.99 2.43 3.027(4) 118.3 . yes
N1B H1B1 Br2 0.90(2) 2.72(3) 3.448(3) 139(4) . yes
N1B H1B2 Br3 0.90(2) 2.49(2) 3.378(4) 171(4) 2_545 yes
N1B H1B3 Br1 0.90(2) 2.97(4) 3.518(3) 121(4) . yes
N1B H1B3 O1B 0.90(2) 1.92(3) 2.759(4) 155(4) . yes
C2B H2BA Br3 0.99 3.02 3.999(4) 171.1 2 yes
C3B H3BB Br1 0.99 3.01 3.747(4) 132.5 1_455 yes
C3B H3BB O1A 0.99 2.49 3.395(5) 151.7 1_455 yes
C4B H4BA Br4 0.99 3.14 3.949(5) 140.2 2_545 yes

_refine_diff_density_max         1.433
_refine_diff_density_min         -1.649
_refine_diff_density_rms         0.217



