# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_220908li_lidz030305_410k_0m_5
_database_code_depnum_ccdc_archive 'CCDC 2212352'
loop_
_audit_author_name
_audit_author_address
'Zhuoer Cai'
;Southeast University
China
;
_audit_update_record             
;
2022-11-22 deposited with the CCDC.	2022-12-16 downloaded from the CCDC.
;
_audit_creation_date             2022-09-11
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb1, 0.5(C14 H34 Cl2 N2)'
_chemical_formula_sum            'C7 H17 Br3 Cl N Pb'
_chemical_formula_weight         597.59
_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'
Cl Cl 0.1484 0.1585 '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'
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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -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'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   10.570(2)
_cell_length_b                   10.570(2)
_cell_length_c                   7.9754(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     771.7(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1722
_cell_measurement_temperature    410
_cell_measurement_theta_max      21.01
_cell_measurement_theta_min      2.22
_shelx_estimated_absorpt_T_max   0.255
_shelx_estimated_absorpt_T_min   0.193
_exptl_absorpt_coefficient_mu    18.839
_exptl_absorpt_correction_T_max  0.094895
_exptl_absorpt_correction_T_min  0.023327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1488 before and 0.0683 after correction.
 
For component 2:
 wR2(int) was 0.1736 before and 0.0784 after correction.
 The Ratio of minimum to maximum transmission is 0.23.

Final HKLF 4 output contains 11652 reflections, Rint = 0.1278
 (2954 with I > 3sig(I), Rint = 0.1000)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.572
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.13
_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  0.078
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            895
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.341
_diffrn_reflns_theta_min         2.225
_diffrn_ambient_temperature      410
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE TXS PHOTON 100'
_diffrn_measurement_method       'ω and φ shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   TXS
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_type              'Rotaing Anode'
_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                520
_reflns_number_total             895
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.827
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.362
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         895
_refine_ls_number_restraints     130
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.0893
_refine_ls_restrained_S_all      0.960
_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)+(0.1946P)²+1.6317P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2454
_refine_ls_wR_factor_ref         0.3051
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.62(4)
 0.38(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N9-C5 = N9-C2 = N9-C3 = N9-C6
 1.5 with sigma of 0.005
 C2-C1 = C4-C3 = C6-C7
 1.53 with sigma of 0.005
 C1-Cl1
 -3 with sigma of 0.02
 Cl1-C5
 1.7 with sigma of 0.005
 C1-N9
 2.6 with sigma of 0.005
 C7-N9
 2.6 with sigma of 0.005
 N9-C4
 2.6 with sigma of 0.005
 Cl1-N9
 2.7 with sigma of 0.005
 C5-C2 \\sim C3-C2 \\sim C3-C5 \\sim C6-C5 \\sim C6-C3 \\sim C6-C2
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim N9 \\sim C3 \\sim C6 \\sim C5 \\sim C4 \\sim C7 \\sim Cl1:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Others
 Fixed Sof: C2(0.08333) H2A(0.08333) H2B(0.08333) C3(0.08333) H3A(0.08333)
 H3B(0.08333) C6(0.08333) H6B(0.08333) H6A(0.08333) C4(0.08333) H4B(0.08333)
 H4A(0.08333) H4C(0.08333) N9(0.08333) C7(0.08333) H7C(0.08333) H7B(0.08333)
 H7A(0.08333) C1(0.08333) H1A(0.08333) H1B(0.08333) H1C(0.08333) C5(0.08333)
 H5B(0.08333) H5A(0.08333) Cl1(0.08333)
6.a Riding coordinates:
 C4(H4B,H4A,H4C), C7(H7C,H7B,H7A), C1(H1A,H1B,H1C)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6B,H6A), C5(H5B,H5A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.000000 0.000000 1.000000 0.1013(19) Uani 1 12 d S T P . .
Br1 Br 0.1243(4) 0.2486(8) 1.250000 0.229(8) Uani 1 4 d S T P . .
C2 C 0.394(14) 0.196(12) 1.06(2) 0.28(7) Uani 0.0833 1 d D U P A -1
H2A H 0.390801 0.191606 0.939484 0.331 Uiso 0.0833 1 calc R U P A -1
H2B H 0.300271 0.184941 1.102196 0.331 Uiso 0.0833 1 calc R U P A -1
C3 C 0.559(18) 0.34(2) 1.290(12) 0.28(7) Uani 0.0833 1 d D U P A -1
H3A H 0.470816 0.306983 1.361655 0.331 Uiso 0.0833 1 calc R U P A -1
H3B H 0.626135 0.446429 1.324204 0.331 Uiso 0.0833 1 calc R U P A -1
C6 C 0.457(19) 0.452(16) 1.10(2) 0.28(7) Uani 0.0833 1 d D U P A -1
H6B H 0.354734 0.401115 1.138022 0.331 Uiso 0.0833 1 calc R U P A -1
H6A H 0.455275 0.473117 0.977575 0.331 Uiso 0.0833 1 calc R U P A -1
C4 C 0.63(2) 0.26(2) 1.33(2) 0.28(7) Uani 0.0833 1 d D U P A -1
H4B H 0.644704 0.246279 1.449905 0.415 Uiso 0.0833 1 d R U P A -1
H4A H 0.729303 0.308979 1.276405 0.415 Uiso 0.0833 1 d R U P A -1
H4C H 0.578153 0.157339 1.279635 0.415 Uiso 0.0833 1 d R U P A -1
N9 N 0.513(12) 0.346(10) 1.112(12) 0.28(7) Uani 0.0833 1 d D U P A -1
C7 C 0.54(3) 0.597(19) 1.19(5) 0.27(7) Uani 0.0833 1 d D U P A -1
H7C H 0.587520 0.583426 1.288576 0.412 Uiso 0.0833 1 d R U P A -1
H7B H 0.472900 0.630995 1.228306 0.412 Uiso 0.0833 1 d R U P A -1
H7A H 0.613450 0.670516 1.116156 0.412 Uiso 0.0833 1 d R U P A -1
C1 C 0.40(3) 0.065(10) 1.13(3) 0.28(7) Uani 0.0833 1 d D U P A -1
H1A H 0.324478 -0.022859 1.076015 0.415 Uiso 0.0833 1 d R U P A -1
H1B H 0.395388 0.056841 1.249805 0.415 Uiso 0.0833 1 d R U P A -1
H1C H 0.498138 0.075641 1.093286 0.415 Uiso 0.0833 1 d R U P A -1
C5 C 0.641(14) 0.394(10) 0.998(15) 0.28(7) Uani 0.0833 1 d D U P A -1
H5B H 0.731892 0.443359 1.065716 0.330 Uiso 0.0833 1 calc R U P A -1
H5A H 0.643533 0.466176 0.917621 0.330 Uiso 0.0833 1 calc R U P A -1
Cl1 Cl 0.642(18) 0.256(13) 0.888(15) 0.27(7) Uani 0.0833 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.025(6) . ?
Pb1 Br1 3.025(6) 15_557 ?
Pb1 Br1 3.025(6) 14_557 ?
Pb1 Br1 3.025(6) 2 ?
Pb1 Br1 3.025(6) 3 ?
Pb1 Br1 3.025(6) 13_557 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 N9 1.500(10) . ?
C2 C1 1.530(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.530(10) . ?
C3 N9 1.500(10) . ?
C6 H6B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 N9 1.500(10) . ?
C6 C7 1.530(11) . ?
C4 H4B 0.9801 . ?
C4 H4A 0.9800 . ?
C4 H4C 0.9801 . ?
N9 C5 1.500(10) . ?
C7 H7C 0.9801 . ?
C7 H7B 0.9799 . ?
C7 H7A 0.9799 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9801 . ?
C1 H1C 0.9802 . ?
C5 H5B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 Cl1 1.700(10) . ?

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
Br1 Pb1 Br1 180.00(17) . 13_557 ?
Br1 Pb1 Br1 81.29(15) 3 2 ?
Br1 Pb1 Br1 98.71(15) 3 14_557 ?
Br1 Pb1 Br1 98.71(15) 15_557 2 ?
Br1 Pb1 Br1 81.29(15) 13_557 14_557 ?
Br1 Pb1 Br1 81.29(15) 15_557 14_557 ?
Br1 Pb1 Br1 180.0 2 14_557 ?
Br1 Pb1 Br1 98.71(15) . 15_557 ?
Br1 Pb1 Br1 98.71(15) 13_557 3 ?
Br1 Pb1 Br1 98.71(15) . 14_557 ?
Br1 Pb1 Br1 180.0 15_557 3 ?
Br1 Pb1 Br1 81.29(15) 13_557 15_557 ?
Br1 Pb1 Br1 81.29(15) . 2 ?
Br1 Pb1 Br1 98.71(15) 13_557 2 ?
Br1 Pb1 Br1 81.29(15) . 3 ?
Pb1 Br1 Pb1 82.45(19) . 4 ?
H2A C2 H2B 107.1 . . ?
N9 C2 H2A 107.8 . . ?
N9 C2 H2B 107.8 . . ?
N9 C2 C1 118.2(12) . . ?
C1 C2 H2A 107.8 . . ?
C1 C2 H2B 107.8 . . ?
H3A C3 H3B 107.1 . . ?
C4 C3 H3A 107.8 . . ?
C4 C3 H3B 107.8 . . ?
N9 C3 H3A 107.8 . . ?
N9 C3 H3B 107.8 . . ?
N9 C3 C4 118.2(12) . . ?
H6B C6 H6A 107.1 . . ?
N9 C6 H6B 107.8 . . ?
N9 C6 H6A 107.8 . . ?
N9 C6 C7 118.2(12) . . ?
C7 C6 H6B 107.8 . . ?
C7 C6 H6A 107.8 . . ?
C3 C4 H4B 112.8 . . ?
C3 C4 H4A 104.9 . . ?
C3 C4 H4C 110.6 . . ?
H4B C4 H4A 109.5 . . ?
H4B C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
C2 N9 C3 109.5(19) . . ?
C2 N9 C6 109.5(18) . . ?
C2 N9 C5 109.4(18) . . ?
C3 N9 C5 109.5(19) . . ?
C6 N9 C3 109.5(18) . . ?
C6 N9 C5 109.4(19) . . ?
C6 C7 H7C 108.0 . . ?
C6 C7 H7B 111.2 . . ?
C6 C7 H7A 109.1 . . ?
H7C C7 H7B 109.5 . . ?
H7C C7 H7A 109.5 . . ?
H7B C7 H7A 109.5 . . ?
C2 C1 H1A 107.7 . . ?
C2 C1 H1B 111.5 . . ?
C2 C1 H1C 109.2 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N9 C5 H5B 108.5 . . ?
N9 C5 H5A 108.5 . . ?
N9 C5 Cl1 114.9(11) . . ?
H5B C5 H5A 107.5 . . ?
Cl1 C5 H5B 108.5 . . ?
Cl1 C5 H5A 108.5 . . ?

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
C2 N9 C5 Cl1 -17(9) . . . . ?
C3 N9 C5 Cl1 103(9) . . . . ?
C6 N9 C5 Cl1 -137(9) . . . . ?
C4 C3 N9 C2 66(17) . . . . ?
C4 C3 N9 C6 -174(16) . . . . ?
C4 C3 N9 C5 -54(17) . . . . ?
C7 C6 N9 C2 161(20) . . . . ?
C7 C6 N9 C3 41(20) . . . . ?
C7 C6 N9 C5 -79(20) . . . . ?
C1 C2 N9 C3 -38(5) . . . . ?
C1 C2 N9 C6 -158(5) . . . . ?
C1 C2 N9 C5 82(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.62(4)
2 0.38(4)

# start Validation Reply Form
_vrf_PLAT088_220908li_lidz030305_410k_0m_5 
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.36 Note  
RESPONSE: The crystal was twinning and the structure was refined against 
detwined HKLF5 file. Besides, the organic moiety disordered across symmetry 
elements, these all lead to the poor data / parameter ratio.
;
####################################################################### 
# 
# 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_GSW220829_PbBr2_a
_database_code_depnum_ccdc_archive 'CCDC 2212353'
loop_
_audit_author_name
_audit_author_address
'Zhuoer Cai'
;Southeast University
China
;
_audit_update_record             
;
2022-10-12 deposited with the CCDC.	2022-12-16 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         'Br3 Pb, C7 H17 Cl N'
_chemical_formula_sum            'C7 H17 Br3 Cl N Pb'
_chemical_formula_weight         597.58

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'
Cl Cl 0.1484 0.1585 '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                   10.8678(4)
_cell_length_b                   35.6850(15)
_cell_length_c                   7.7853(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.9530(10)
_cell_angle_gamma                90
_cell_volume                     2964.3(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7228
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      27.42

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.678
_exptl_crystal_F_000             2160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    19.617
_shelx_estimated_absorpt_T_min   0.303
_shelx_estimated_absorpt_T_max   0.341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3579
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source.type              microfocus
_diffrn_radiation_type           MoK\a
_diffrn_source.source            'Ius 2.0'
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            23023
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.992
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             5192
_reflns_number_gt                3719
_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0256P)²+20.0927P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5192
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.0862
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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_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 0.500000 0.500000 0.500000 0.03352(15) Uani 1 2 d S . P . .
Pb2 Pb 0.500000 0.500000 1.000000 0.03364(15) Uani 1 2 d S . P . .
Pb3 Pb 1.01377(3) 0.24952(2) 0.59507(4) 0.03204(11) Uani 1 1 d . . . . .
Br1 Br 0.54988(10) 0.43813(3) 0.76469(14) 0.0473(3) Uani 1 1 d . . . . .
Br2 Br 0.65189(10) 0.54811(3) 0.79059(14) 0.0480(3) Uani 1 1 d . . . . .
Br3 Br 0.29281(9) 0.52154(3) 0.69438(15) 0.0459(3) Uani 1 1 d . . . . .
Br4 Br 0.82280(11) 0.21828(4) 0.28708(16) 0.0637(4) Uani 1 1 d . . . . .
Br5 Br 1.19803(11) 0.21760(3) 0.38662(16) 0.0554(3) Uani 1 1 d . . . . .
Br6 Br 1.01177(10) 0.31503(3) 0.36412(13) 0.0400(3) Uani 1 1 d . . . . .
C1 C 0.0758(10) 0.3780(3) 1.0045(12) 0.044(3) Uani 1 1 d . . . . .
H1A H 0.165061 0.374671 1.023685 0.065 Uiso 1 1 calc R U . . .
H1B H 0.037945 0.356351 1.046055 0.065 Uiso 1 1 calc R U . . .
H1C H 0.056472 0.399799 1.066528 0.065 Uiso 1 1 calc R U . . .
C2 C 0.0247(10) 0.3831(3) 0.8078(15) 0.048(3) Uani 1 1 d . . . . .
H2A H 0.043940 0.360589 0.748058 0.058 Uiso 1 1 calc R U . . .
H2B H -0.065904 0.384925 0.790766 0.058 Uiso 1 1 calc R U . . .
C3 C 0.2138(8) 0.4135(3) 0.7265(15) 0.045(3) Uani 1 1 d . . . . .
H3A H 0.255126 0.412694 0.848368 0.054 Uiso 1 1 calc R U . . .
H3B H 0.242458 0.435880 0.675351 0.054 Uiso 1 1 calc R U . . .
C4 C 0.2549(9) 0.3793(3) 0.6335(16) 0.052(3) Uani 1 1 d . . . . .
H4A H 0.217961 0.357136 0.671791 0.079 Uiso 1 1 calc R U . . .
H4B H 0.344561 0.377200 0.660819 0.079 Uiso 1 1 calc R U . . .
H4C H 0.228021 0.382107 0.509363 0.079 Uiso 1 1 calc R U . . .
C5 C 0.0017(10) 0.4183(3) 0.5337(13) 0.044(3) Uani 1 1 d . . . . .
H5A H -0.085563 0.423537 0.536095 0.052 Uiso 1 1 calc R U . . .
H5B H 0.005244 0.393676 0.481746 0.052 Uiso 1 1 calc R U . . .
C6 C 0.0503(8) 0.4485(2) 0.4106(11) 0.028(2) Uani 1 1 d . . . . .
H6A H 0.059188 0.472379 0.468448 0.043 Uiso 1 1 calc R U . . .
H6B H -0.008937 0.450560 0.302637 0.043 Uiso 1 1 calc R U . . .
H6C H 0.130005 0.440714 0.386924 0.043 Uiso 1 1 calc R U . . .
C7 C 0.0573(9) 0.4529(3) 0.8145(14) 0.042(3) Uani 1 1 d . . . . .
H7A H 0.087511 0.473539 0.752913 0.051 Uiso 1 1 calc R U . . .
H7B H 0.109053 0.451658 0.930457 0.051 Uiso 1 1 calc R U . . .
C8 C 0.4489(10) 0.3412(3) 0.2444(16) 0.060(3) Uani 1 1 d . . . . .
H8A H 0.395716 0.342570 0.129486 0.073 Uiso 1 1 calc R U . . .
H8B H 0.438651 0.364430 0.304596 0.073 Uiso 1 1 calc R U . . .
C9 C 0.4008(10) 0.3086(3) 0.3468(15) 0.057(3) Uani 1 1 d . . . . .
H9A H 0.413425 0.285151 0.291967 0.086 Uiso 1 1 calc R U . . .
H9B H 0.313153 0.311969 0.346310 0.086 Uiso 1 1 calc R U . . .
H9C H 0.446297 0.308480 0.465256 0.086 Uiso 1 1 calc R U . . .
C10 C 0.6035(12) 0.3053(4) 0.1126(18) 0.076(4) Uani 1 1 d . . . . .
H10A H 0.580000 0.282911 0.169210 0.091 Uiso 1 1 calc R U . . .
H10B H 0.692266 0.303435 0.110287 0.091 Uiso 1 1 calc R U . . .
C11 C 0.5269(11) 0.3061(5) -0.0862(17) 0.085(5) Uani 1 1 d . . . . .
H11A H 0.447439 0.293904 -0.091966 0.128 Uiso 1 1 calc R U . . .
H11B H 0.574032 0.293143 -0.160535 0.128 Uiso 1 1 calc R U . . .
H11C H 0.513717 0.331558 -0.124479 0.128 Uiso 1 1 calc R U . . .
C12 C 0.6146(10) 0.3747(3) 0.1368(16) 0.059(3) Uani 1 1 d . . . . .
H12A H 0.601768 0.395314 0.212450 0.070 Uiso 1 1 calc R U . . .
H12B H 0.555635 0.377781 0.027426 0.070 Uiso 1 1 calc R U . . .
C13 C 0.7515(9) 0.3778(3) 0.0977(15) 0.052(3) Uani 1 1 d . . . . .
H13A H 0.810135 0.381229 0.205505 0.077 Uiso 1 1 calc R U . . .
H13B H 0.756054 0.398871 0.022298 0.077 Uiso 1 1 calc R U . . .
H28 H 0.771726 0.355314 0.041480 0.077 Uiso 1 1 calc R U . . .
C14 C 0.6704(10) 0.3332(3) 0.3954(14) 0.052(3) Uani 1 1 d . . . . .
H14A H 0.755979 0.331775 0.376647 0.063 Uiso 1 1 calc R U . . .
H14B H 0.650814 0.309577 0.445761 0.063 Uiso 1 1 calc R U . . .
Cl1 Cl -0.0933(4) 0.46200(11) 0.8344(6) 0.0968(12) Uani 1 1 d . . . . .
Cl2 Cl 0.6595(4) 0.36861(14) 0.5407(6) 0.1161(15) Uani 1 1 d . . . . .
N1 N 0.0730(7) 0.41689(19) 0.7187(10) 0.0319(19) Uani 1 1 d . . . . .
N2 N 0.5833(7) 0.3386(2) 0.2211(11) 0.038(2) 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 2.9984(10) . ?
Pb1 Br1 2.9985(10) 3_666 ?
Pb1 Br3 3.0407(11) 3_666 ?
Pb1 Br3 3.0407(11) . ?
Pb1 Br2 3.0613(10) 3_666 ?
Pb1 Br2 3.0613(10) . ?
Pb2 Br1 2.9836(11) . ?
Pb2 Br1 2.9837(11) 3_667 ?
Pb2 Br3 3.0473(11) . ?
Pb2 Br3 3.0474(11) 3_667 ?
Pb2 Br2 3.0583(11) 3_667 ?
Pb2 Br2 3.0583(11) . ?
Pb3 Br6 2.9467(10) . ?
Pb3 Br5 2.9683(12) 4_566 ?
Pb3 Br4 3.0069(12) 4_566 ?
Pb3 Br5 3.0292(12) . ?
Pb3 Br4 3.0674(12) . ?
Pb3 Br6 3.1164(10) 4_566 ?
C1 C2 1.537(14) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.534(12) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.524(11) . ?
C3 C4 1.529(13) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 N1 1.501(12) . ?
C5 C6 1.598(13) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N1 1.511(11) . ?
C7 Cl1 1.704(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N2 1.509(13) . ?
C8 C9 1.555(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 N2 1.498(13) . ?
C10 C11 1.612(18) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.512(12) . ?
C12 C13 1.578(14) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H28 0.9600 . ?
C14 N2 1.512(13) . ?
C14 Cl2 1.715(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 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
Br1 Pb1 Br1 180.0 . 3_666 ?
Br1 Pb1 Br3 95.83(3) . 3_666 ?
Br1 Pb1 Br3 84.17(3) 3_666 3_666 ?
Br1 Pb1 Br3 84.17(3) . . ?
Br1 Pb1 Br3 95.83(3) 3_666 . ?
Br3 Pb1 Br3 180.0 3_666 . ?
Br1 Pb1 Br2 95.55(3) . 3_666 ?
Br1 Pb1 Br2 84.46(3) 3_666 3_666 ?
Br3 Pb1 Br2 80.61(3) 3_666 3_666 ?
Br3 Pb1 Br2 99.39(3) . 3_666 ?
Br1 Pb1 Br2 84.45(3) . . ?
Br1 Pb1 Br2 95.54(3) 3_666 . ?
Br3 Pb1 Br2 99.39(3) 3_666 . ?
Br3 Pb1 Br2 80.61(3) . . ?
Br2 Pb1 Br2 180.00(3) 3_666 . ?
Br1 Pb2 Br1 180.0 . 3_667 ?
Br1 Pb2 Br3 84.30(3) . . ?
Br1 Pb2 Br3 95.70(3) 3_667 . ?
Br1 Pb2 Br3 95.70(3) . 3_667 ?
Br1 Pb2 Br3 84.30(3) 3_667 3_667 ?
Br3 Pb2 Br3 180.0 . 3_667 ?
Br1 Pb2 Br2 95.24(3) . 3_667 ?
Br1 Pb2 Br2 84.76(3) 3_667 3_667 ?
Br3 Pb2 Br2 99.45(3) . 3_667 ?
Br3 Pb2 Br2 80.55(3) 3_667 3_667 ?
Br1 Pb2 Br2 84.76(3) . . ?
Br1 Pb2 Br2 95.24(3) 3_667 . ?
Br3 Pb2 Br2 80.55(3) . . ?
Br3 Pb2 Br2 99.45(3) 3_667 . ?
Br2 Pb2 Br2 180.00(3) 3_667 . ?
Br6 Pb3 Br5 94.52(3) . 4_566 ?
Br6 Pb3 Br4 94.27(3) . 4_566 ?
Br5 Pb3 Br4 84.14(4) 4_566 4_566 ?
Br6 Pb3 Br5 84.28(3) . . ?
Br5 Pb3 Br5 98.03(4) 4_566 . ?
Br4 Pb3 Br5 177.47(3) 4_566 . ?
Br6 Pb3 Br4 83.45(3) . . ?
Br5 Pb3 Br4 177.95(4) 4_566 . ?
Br4 Pb3 Br4 95.69(4) 4_566 . ?
Br5 Pb3 Br4 82.10(3) . . ?
Br6 Pb3 Br6 175.10(3) . 4_566 ?
Br5 Pb3 Br6 82.41(3) 4_566 4_566 ?
Br4 Pb3 Br6 81.65(3) 4_566 4_566 ?
Br5 Pb3 Br6 99.90(3) . 4_566 ?
Br4 Pb3 Br6 99.59(3) . 4_566 ?
Pb2 Br1 Pb1 81.19(3) . . ?
Pb2 Br2 Pb1 79.00(2) . . ?
Pb1 Br3 Pb2 79.49(2) . . ?
Pb3 Br4 Pb3 79.71(3) 4_565 . ?
Pb3 Br5 Pb3 80.93(3) 4_565 . ?
Pb3 Br6 Pb3 79.84(2) . 4_565 ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 116.9(8) . . ?
N1 C2 H2A 108.1 . . ?
C1 C2 H2A 108.1 . . ?
N1 C2 H2B 108.1 . . ?
C1 C2 H2B 108.1 . . ?
H2A C2 H2B 107.3 . . ?
N1 C3 C4 115.2(8) . . ?
N1 C3 H3A 108.5 . . ?
C4 C3 H3A 108.5 . . ?
N1 C3 H3B 108.5 . . ?
C4 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 C6 115.3(7) . . ?
N1 C5 H5A 108.4 . . ?
C6 C5 H5A 108.4 . . ?
N1 C5 H5B 108.4 . . ?
C6 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 Cl1 114.1(6) . . ?
N1 C7 H7A 108.7 . . ?
Cl1 C7 H7A 108.7 . . ?
N1 C7 H7B 108.7 . . ?
Cl1 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
N2 C8 C9 116.3(9) . . ?
N2 C8 H8A 108.2 . . ?
C9 C8 H8A 108.2 . . ?
N2 C8 H8B 108.2 . . ?
C9 C8 H8B 108.2 . . ?
H8A C8 H8B 107.4 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C11 115.1(11) . . ?
N2 C10 H10A 108.5 . . ?
C11 C10 H10A 108.5 . . ?
N2 C10 H10B 108.5 . . ?
C11 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C13 116.3(8) . . ?
N2 C12 H12A 108.2 . . ?
C13 C12 H12A 108.2 . . ?
N2 C12 H12B 108.2 . . ?
C13 C12 H12B 108.2 . . ?
H12A C12 H12B 107.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H28 109.5 . . ?
H13A C13 H28 109.5 . . ?
H13B C13 H28 109.5 . . ?
N2 C14 Cl2 112.8(7) . . ?
N2 C14 H14A 109.0 . . ?
Cl2 C14 H14A 109.0 . . ?
N2 C14 H14B 109.0 . . ?
Cl2 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C5 N1 C7 111.1(7) . . ?
C5 N1 C3 111.9(8) . . ?
C7 N1 C3 104.7(7) . . ?
C5 N1 C2 107.5(7) . . ?
C7 N1 C2 111.4(7) . . ?
C3 N1 C2 110.3(7) . . ?
C10 N2 C8 111.4(8) . . ?
C10 N2 C14 105.7(8) . . ?
C8 N2 C14 110.8(8) . . ?
C10 N2 C12 111.2(9) . . ?
C8 N2 C12 107.7(8) . . ?
C14 N2 C12 110.1(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
C6 C5 N1 C7 65.5(10) . . . . ?
C6 C5 N1 C3 -51.2(10) . . . . ?
C6 C5 N1 C2 -172.4(8) . . . . ?
Cl1 C7 N1 C5 62.3(9) . . . . ?
Cl1 C7 N1 C3 -176.7(7) . . . . ?
Cl1 C7 N1 C2 -57.5(10) . . . . ?
C4 C3 N1 C5 -58.1(11) . . . . ?
C4 C3 N1 C7 -178.6(9) . . . . ?
C4 C3 N1 C2 61.5(11) . . . . ?
C1 C2 N1 C5 -174.6(8) . . . . ?
C1 C2 N1 C7 -52.6(11) . . . . ?
C1 C2 N1 C3 63.2(11) . . . . ?
C11 C10 N2 C8 63.6(12) . . . . ?
C11 C10 N2 C14 -176.0(9) . . . . ?
C11 C10 N2 C12 -56.5(12) . . . . ?
C9 C8 N2 C10 63.9(13) . . . . ?
C9 C8 N2 C14 -53.5(12) . . . . ?
C9 C8 N2 C12 -173.9(10) . . . . ?
Cl2 C14 N2 C10 -179.2(8) . . . . ?
Cl2 C14 N2 C8 -58.4(10) . . . . ?
Cl2 C14 N2 C12 60.6(10) . . . . ?
C13 C12 N2 C10 -56.9(13) . . . . ?
C13 C12 N2 C8 -179.2(10) . . . . ?
C13 C12 N2 C14 59.9(12) . . . . ?

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
C1 H1B Br6 0.96 2.94 3.757(9) 143.5 1_456 yes
C3 H3A Br2 0.97 3.13 4.007(11) 151.1 3_667 yes
C3 H3B Br3 0.97 3.10 3.968(10) 149.2 . yes
C4 H4B Br1 0.96 3.11 3.806(10) 130.6 . yes
C5 H5B Br6 0.97 2.96 3.922(10) 173.1 1_455 yes
C6 H6C Br2 0.96 2.99 3.856(9) 150.9 3_666 yes
C7 H7A Br3 0.97 2.92 3.787(9) 149.8 . yes
C7 H7B Br2 0.97 3.05 3.969(11) 157.9 3_667 yes
C11 H11A Br5 0.96 2.72 3.640(12) 161.8 4_465 yes
C11 H11B Br4 0.96 2.84 3.643(11) 141.9 4_565 yes
C12 H12B Br1 0.97 2.96 3.639(10) 127.8 1_554 yes
C13 H13B Br1 0.96 3.05 3.741(10) 130.2 1_554 yes
C14 H14A Br6 0.97 2.86 3.819(11) 168.9 . yes
C14 H14B Br4 0.97 3.11 3.674(11) 118.8 4_566 yes

_refine_diff_density_max         1.869
_refine_diff_density_min         -2.485
_refine_diff_density_rms         0.183

# start Validation Reply Form
_vrf_PLAT972_GSW220829_PbBr2_a   
;
PROBLEM: Check Calcd Resid. Dens.  1.44Ang From Pb3            -2.84 eA-3
RESPONSE: The residual electron density peaks indicated above are close to the 
Pb atom and are assumed to be the result of inadequacies in the absorption 
correction.
;
# end Validation Reply Form

