# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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 2163383'
loop_
_audit_author_name
_audit_author_address
'Zhenhong Wei'
;CCDC
China
;
_audit_update_record             
;
2022-03-30 deposited with the CCDC.	2022-05-02 downloaded from the CCDC.
;
_audit_creation_date             2022-03-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C6 H13 N2'
_chemical_formula_sum            'C6 H13 Br3 N2 Pb'
_chemical_formula_weight         560.08
_chemical_absolute_configuration ?
_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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   7.8703(3)
_cell_length_b                   10.4757(4)
_cell_length_c                   15.2771(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1259.55(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4154
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.9770
_cell_measurement_theta_min      2.3450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.87
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.954
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.804
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7457
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.749
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.876
_diffrn_reflns_theta_min         2.357
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.804
_diffrn_measurement_device_type  'multiwire proportional'
_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         0.629
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.675
_reflns_number_gt                2494
_reflns_number_total             3969
_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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details 
;
 Flack x determined using 898 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(11)
_refine_ls_extinction_coef       0.00444(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2971
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0222
_refine_ls_restrained_S_all      1.040
_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)+(0.0215P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0512
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 N1(H1)
1.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C1(H1A,H1B), C4(H4A,H4B), C2(H2A,H2B), C5(H5A,H5B), C3(H3A,H3B)
;
_atom_sites_solution_hydrogens   geom
_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
Pb01 Pb 0.51503(3) 0.24547(2) 0.49989(2) 0.04045(9) Uani 1 1 d . . . . .
Br3 Br 0.30146(10) 0.46153(6) 0.44853(4) 0.04711(18) Uani 1 1 d . . . . .
Br2 Br 0.72309(10) 0.41061(7) 0.60358(5) 0.0546(2) Uani 1 1 d . . . . .
Br1 Br 0.27798(11) 0.21536(8) 0.64850(4) 0.0561(2) Uani 1 1 d . . . . .
N2 N 0.1890(10) 0.7348(6) 0.6002(4) 0.0629(17) Uani 1 1 d . . . . .
N1 N 0.3314(9) 0.6509(6) 0.6225(4) 0.0546(17) Uani 1 1 d . . . . .
H1 H 0.345389 0.588711 0.575073 0.066 Uiso 1 1 calc R U . . .
C6 C 0.4883(11) 0.7364(9) 0.6243(7) 0.075(3) Uani 1 1 d . . . . .
H6A H 0.568157 0.708539 0.668789 0.090 Uiso 1 1 calc R U . . .
H6B H 0.544960 0.737319 0.567955 0.090 Uiso 1 1 calc R U . . .
C1 C 0.2936(14) 0.5816(8) 0.7027(5) 0.072(2) Uani 1 1 d . . . . .
H1A H 0.343333 0.623556 0.753168 0.087 Uiso 1 1 calc R U . . .
H1B H 0.335251 0.494526 0.699748 0.087 Uiso 1 1 calc R U . . .
C4 C 0.2460(16) 0.8638(10) 0.6091(9) 0.110(4) Uani 1 1 d . . . . .
H4A H 0.171213 0.910558 0.648135 0.133 Uiso 1 1 calc R U . . .
H4B H 0.245977 0.905993 0.552607 0.133 Uiso 1 1 calc R U . . .
C2 C 0.1062(14) 0.5847(11) 0.7066(6) 0.089(3) Uani 1 1 d . . . . .
H2A H 0.058498 0.511609 0.676423 0.106 Uiso 1 1 calc R U . . .
H2B H 0.067780 0.583429 0.766943 0.106 Uiso 1 1 calc R U . . .
C5 C 0.4192(16) 0.8603(11) 0.6452(10) 0.112(4) Uani 1 1 d . . . . .
H5A H 0.488155 0.927063 0.619315 0.134 Uiso 1 1 calc R U . . .
H5B H 0.416530 0.872705 0.708092 0.134 Uiso 1 1 calc R U . . .
C3 C 0.0565(17) 0.6981(13) 0.6657(10) 0.120(5) Uani 1 1 d . . . . .
H3A H 0.043737 0.765231 0.708909 0.144 Uiso 1 1 calc R U . . .
H3B H -0.051960 0.686041 0.636671 0.144 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb01 0.02677(13) 0.04902(15) 0.04556(14) -0.00453(10) -0.00112(10) 0.00111(10)
Br3 0.0491(4) 0.0472(4) 0.0450(3) -0.0004(3) -0.0055(3) 0.0029(3)
Br2 0.0450(5) 0.0616(4) 0.0572(4) -0.0177(3) -0.0021(3) -0.0045(4)
Br1 0.0539(5) 0.0718(5) 0.0425(3) 0.0049(3) 0.0004(3) -0.0080(4)
N2 0.066(5) 0.063(4) 0.060(4) -0.004(3) -0.018(3) 0.003(4)
N1 0.065(5) 0.054(4) 0.045(3) -0.012(3) -0.009(3) 0.012(3)
C6 0.047(5) 0.094(7) 0.084(7) 0.003(5) 0.009(4) -0.005(6)
C1 0.091(7) 0.060(5) 0.065(5) 0.010(4) -0.012(5) -0.009(5)
C4 0.112(12) 0.060(6) 0.160(11) 0.014(6) -0.036(9) 0.008(6)
C2 0.081(8) 0.116(9) 0.069(6) 0.021(6) -0.009(5) -0.032(7)
C5 0.076(8) 0.082(8) 0.178(13) -0.016(8) 0.029(9) -0.017(7)
C3 0.075(9) 0.119(10) 0.167(13) 0.020(10) 0.044(9) 0.004(8)

_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 Br3 3.2257(8) 4_556 ?
Pb01 Br3 2.9264(7) . ?
Pb01 Br2 3.2329(8) 4_456 ?
Pb01 Br2 2.8607(8) . ?
Pb01 Br1 2.9554(8) . ?
Pb01 Br1 3.0968(8) 4_556 ?
N2 N1 1.465(9) . ?
N2 C4 1.431(12) . ?
N2 C3 1.496(13) . ?
N1 H1 0.9800 . ?
N1 C6 1.526(10) . ?
N1 C1 1.456(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.442(14) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.476(13) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.471(16) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.398(16) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 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
Br3 Pb01 Br3 170.70(2) . 4_556 ?
Br3 Pb01 Br2 81.48(2) . 4_456 ?
Br3 Pb01 Br2 106.027(19) 4_556 4_456 ?
Br3 Pb01 Br1 85.75(2) . . ?
Br3 Pb01 Br1 94.88(2) . 4_556 ?
Br2 Pb01 Br3 90.54(2) . . ?
Br2 Pb01 Br3 82.60(2) . 4_556 ?
Br2 Pb01 Br2 169.56(3) . 4_456 ?
Br2 Pb01 Br1 90.03(2) . . ?
Br2 Pb01 Br1 86.72(2) . 4_556 ?
Br1 Pb01 Br3 100.47(2) . 4_556 ?
Br1 Pb01 Br3 78.514(19) 4_556 4_556 ?
Br1 Pb01 Br2 82.70(2) . 4_456 ?
Br1 Pb01 Br2 100.60(2) 4_556 4_456 ?
Br1 Pb01 Br1 176.69(2) . 4_556 ?
Pb01 Br3 Pb01 79.395(16) . 4_456 ?
Pb01 Br2 Pb01 80.223(16) . 4_556 ?
Pb01 Br1 Pb01 81.103(17) . 4_456 ?
N1 N2 C3 102.9(7) . . ?
C4 N2 N1 107.7(8) . . ?
C4 N2 C3 113.4(9) . . ?
N2 N1 H1 108.3 . . ?
N2 N1 C6 105.8(6) . . ?
C6 N1 H1 108.3 . . ?
C1 N1 N2 109.8(7) . . ?
C1 N1 H1 108.3 . . ?
C1 N1 C6 116.2(7) . . ?
N1 C6 H6A 111.1 . . ?
N1 C6 H6B 111.1 . . ?
H6A C6 H6B 109.1 . . ?
C5 C6 N1 103.1(8) . . ?
C5 C6 H6A 111.1 . . ?
C5 C6 H6B 111.1 . . ?
N1 C1 H1A 111.1 . . ?
N1 C1 H1B 111.1 . . ?
N1 C1 C2 103.1(8) . . ?
H1A C1 H1B 109.1 . . ?
C2 C1 H1A 111.1 . . ?
C2 C1 H1B 111.1 . . ?
N2 C4 H4A 110.2 . . ?
N2 C4 H4B 110.2 . . ?
N2 C4 C5 107.6(9) . . ?
H4A C4 H4B 108.5 . . ?
C5 C4 H4A 110.2 . . ?
C5 C4 H4B 110.2 . . ?
C1 C2 H2A 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
C3 C2 C1 106.3(9) . . ?
C3 C2 H2A 110.5 . . ?
C3 C2 H2B 110.5 . . ?
C6 C5 C4 106.9(10) . . ?
C6 C5 H5A 110.3 . . ?
C6 C5 H5B 110.3 . . ?
C4 C5 H5A 110.3 . . ?
C4 C5 H5B 110.3 . . ?
H5A C5 H5B 108.6 . . ?
N2 C3 H3A 109.9 . . ?
N2 C3 H3B 109.9 . . ?
C2 C3 N2 108.8(10) . . ?
C2 C3 H3A 109.9 . . ?
C2 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?

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
N2 N1 C6 C5 26.5(10) . . . . ?
N2 N1 C1 C2 22.7(9) . . . . ?
N2 C4 C5 C6 22.9(16) . . . . ?
N1 N2 C4 C5 -5.4(14) . . . . ?
N1 N2 C3 C2 -12.6(13) . . . . ?
N1 C6 C5 C4 -29.9(13) . . . . ?
N1 C1 C2 C3 -30.3(12) . . . . ?
C6 N1 C1 C2 142.6(8) . . . . ?
C1 N1 C6 C5 -95.6(11) . . . . ?
C1 C2 C3 N2 27.2(15) . . . . ?
C4 N2 N1 C6 -13.0(10) . . . . ?
C4 N2 N1 C1 113.1(9) . . . . ?
C4 N2 C3 C2 -128.7(11) . . . . ?
C3 N2 N1 C6 -133.2(9) . . . . ?
C3 N2 N1 C1 -7.0(10) . . . . ?
C3 N2 C4 C5 107.9(14) . . . . ?

_shelx_res_file                  
;
TITL 1_a.res in P2(1)2(1)2(1)
    1.res
    created by SHELXL-2017/1 at 20:51:18 on 17-Mar-2022
REM Old TITL 1 in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.120, Rweak 0.011, Alpha 0.002, Orientation as input
REM Flack x = 0.021 ( 0.014 ) from Parsons' quotients
REM Formula found by SHELXT: C3 N Br3 Pb
CELL 0.71073 7.8703 10.4757 15.2771 90 90 90
ZERR 4 0.0003 0.0004 0.0006 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N Br Pb O
UNIT 12 12 12 12 12 1

L.S. 60
PLAN  33
CONF
BOND $H
Htab
list 4
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\1.hkl">
REM </olex2.extras>

WGHT    0.021500
EXTI    0.004440
FVAR       0.30473
PB01  5    0.515031    0.245472    0.499893    11.00000    0.02677    0.04902 =
         0.04556   -0.00453   -0.00112    0.00111
BR3   4    0.301460    0.461535    0.448532    11.00000    0.04914    0.04722 =
         0.04498   -0.00037   -0.00554    0.00287
BR2   4    0.723086    0.410614    0.603584    11.00000    0.04499    0.06159 =
         0.05721   -0.01768   -0.00215   -0.00453
BR1   4    0.277976    0.215361    0.648503    11.00000    0.05387    0.07177 =
         0.04253    0.00488    0.00040   -0.00801
N2    3    0.188953    0.734794    0.600190    11.00000    0.06579    0.06256 =
         0.06030   -0.00404   -0.01821    0.00326
N1    3    0.331404    0.650898    0.622452    11.00000    0.06540    0.05394 =
         0.04455   -0.01210   -0.00854    0.01245
AFIX  13
H1    2    0.345389    0.588711    0.575073    11.00000   -1.20000
AFIX   0
C6    1    0.488335    0.736418    0.624348    11.00000    0.04693    0.09441 =
         0.08394    0.00281    0.00875   -0.00455
AFIX  23
H6A   2    0.568157    0.708539    0.668789    11.00000   -1.20000
H6B   2    0.544960    0.737319    0.567955    11.00000   -1.20000
AFIX   0
C1    1    0.293604    0.581567    0.702709    11.00000    0.09075    0.06016 =
         0.06543    0.01001   -0.01220   -0.00866
AFIX  23
H1A   2    0.343333    0.623556    0.753168    11.00000   -1.20000
H1B   2    0.335251    0.494526    0.699748    11.00000   -1.20000
AFIX   0
C4    1    0.245984    0.863829    0.609136    11.00000    0.11226    0.05953 =
         0.15965    0.01388   -0.03570    0.00813
AFIX  23
H4A   2    0.171213    0.910558    0.648135    11.00000   -1.20000
H4B   2    0.245977    0.905993    0.552607    11.00000   -1.20000
AFIX   0
C2    1    0.106217    0.584746    0.706622    11.00000    0.08080    0.11554 =
         0.06919    0.02117   -0.00947   -0.03178
AFIX  23
H2A   2    0.058498    0.511609    0.676423    11.00000   -1.20000
H2B   2    0.067780    0.583429    0.766943    11.00000   -1.20000
AFIX   0
C5    1    0.419171    0.860250    0.645190    11.00000    0.07563    0.08227 =
         0.17770   -0.01618    0.02853   -0.01657
AFIX  23
H5A   2    0.488155    0.927063    0.619315    11.00000   -1.20000
H5B   2    0.416530    0.872705    0.708092    11.00000   -1.20000
AFIX   0
C3    1    0.056476    0.698058    0.665703    11.00000    0.07467    0.11910 =
         0.16680    0.02047    0.04391    0.00418
AFIX  23
H3A   2    0.043737    0.765231    0.708909    11.00000   -1.20000
H3B   2   -0.051960    0.686041    0.636671    11.00000   -1.20000
AFIX   0
HKLF 4




REM  1_a.res in P2(1)2(1)2(1)
REM R1 =  0.0222 for    2494 Fo > 4sig(Fo)  and  0.0301 for all    2971 data
REM    110 parameters refined using      0 restraints

END

WGHT      0.0215      0.0000

REM Instructions for potential hydrogen bonds
HTAB N1 Br3
EQIV $3 -x+1, y+1/2, -z+3/2
HTAB C6 Br1_$3
HTAB C1 Br1
EQIV $4 x-1/2, -y+3/2, -z+1
HTAB C4 Br2_$4
EQIV $5 x-1, y, z
HTAB C2 Br2_$5
EQIV $6 -x+1/2, -y+1, z+1/2
HTAB C2 Br3_$6
EQIV $7 x+1/2, -y+3/2, -z+1
HTAB C5 Br3_$7
HTAB C5 Br2_$3

REM Highest difference peak  0.738,  deepest hole -0.720,  1-sigma level  0.107
Q1    1   0.4383  0.1848  0.5002  11.00000  0.05    0.74
Q2    1   0.5861  0.1792  0.4995  11.00000  0.05    0.71
Q3    1   0.4434  0.3120  0.4996  11.00000  0.05    0.68
Q4    1   0.5939  0.3069  0.5000  11.00000  0.05    0.60
Q5    1   0.2122  0.2826  0.6478  11.00000  0.05    0.52
Q6    1   0.7083  0.4597  0.5524  11.00000  0.05    0.40
Q7    1   0.8580  0.3802  0.5302  11.00000  0.05    0.39
Q8    1   0.3734  0.2209  0.4274  11.00000  0.05    0.39
Q9    1   0.3878  0.2138  0.5672  11.00000  0.05    0.39
Q10   1   0.1790  0.2866  0.5862  11.00000  0.05    0.38
Q11   1   0.2172  0.5181  0.4627  11.00000  0.05    0.38
Q12   1   0.3961  0.8328  0.5784  11.00000  0.05    0.36
Q13   1   0.5036  0.2502  0.4178  11.00000  0.05    0.35
Q14   1   0.2128  0.4671  0.4913  11.00000  0.05    0.34
Q15   1   0.3625  0.7202  0.7382  11.00000  0.05    0.34
Q16   1   0.2243  0.6648  0.6476  11.00000  0.05    0.34
Q17   1   0.2330  0.8416  0.6554  11.00000  0.05    0.34
Q18   1   0.7953  0.3329  0.5982  11.00000  0.05    0.33
Q19   1   0.2752  0.7911  0.5819  11.00000  0.05    0.32
Q20   1   0.3582  0.2692  0.6073  11.00000  0.05    0.32
Q21   1  -0.1219  0.4322  0.6771  11.00000  0.05    0.32
Q22   1   0.3629  0.3756  0.5213  11.00000  0.05    0.31
Q23   1  -0.0577  0.3534  0.6737  11.00000  0.05    0.31
Q24   1   0.3898  0.9613  0.5415  11.00000  0.05    0.31
Q25   1   0.5804  0.8515  0.6404  11.00000  0.05    0.30
Q26   1   0.6404  0.2742  0.4480  11.00000  0.05    0.30
Q27   1  -0.1176  0.5830  0.8184  11.00000  0.05    0.30
Q28   1   0.3582  0.3841  0.4743  11.00000  0.05    0.30
Q29   1   0.4965  0.5323  0.7607  11.00000  0.05    0.30
Q30   1   0.6741  0.3772  0.5273  11.00000  0.05    0.30
Q31   1   0.5015  0.2442  0.5934  11.00000  0.05    0.30
Q32   1   0.3793  0.1800  0.7177  11.00000  0.05    0.30
Q33   1   0.5086  0.2618  0.5571  11.00000  0.05    0.29
;
_shelx_res_checksum              70478
_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_t
_database_code_depnum_ccdc_archive 'CCDC 2163392'
loop_
_audit_author_name
_audit_author_address
'Zhenhong Wei'
;CCDC
China
;
_audit_update_record             
;
2022-03-30 deposited with the CCDC.	2022-05-02 downloaded from the CCDC.
;
_audit_creation_date             2022-03-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C3 N), Br3 Pb'
_chemical_formula_sum            'C6 Br3 N2 Pb'
_chemical_formula_weight         546.98
_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'
Br Br -0.2901 2.4595 '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'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, x-y, z'

_cell_length_a                   9.7659(16)
_cell_length_b                   9.7659(16)
_cell_length_c                   7.9042(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     652.8(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    473
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2560
_cell_measurement_theta_min      2.4070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.058
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            color
_exptl_crystal_density_diffrn    2.782
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2622
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.688
_diffrn_reflns_theta_min         2.408
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'multiwire proportional'
_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                156
_reflns_number_total             419
_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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.430
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.3405
_refine_ls_R_factor_gt           0.1935
_refine_ls_restrained_S_all      1.430
_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)+(0.0599P)²+11.3213P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3019
_refine_ls_wR_factor_ref         0.3389
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: N1(0.16667) C1(0.33333)
;
_atom_sites_solution_hydrogens   .
_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 1.000000 1.000000 0.500000 0.183(3) Uani 1 12 d S T P . .
Br1 Br 0.7316(14) 0.8658(7) 0.750000 0.286(7) Uani 1 4 d S T P . .
N1 N 0.270(9) 0.730(9) 1.250000 0.35(10) Uiso 0.6667 4 d S . P . .
C1 C 0.408(8) 0.816(16) 1.102(14) 0.34(7) Uiso 0.6667 2 d S . P . .
C2 C 0.333333 0.666667 1.04(3) 0.41(13) Uiso 1 6 d S . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.238(5) 0.238(5) 0.072(2) 0.000 0.000 0.119(2)
Br1 0.229(11) 0.419(16) 0.148(6) 0.000 0.000 0.114(6)

_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 3.010(9) 14_677 ?
Pb1 Br1 3.010(9) 15_566 ?
Pb1 Br1 3.010(9) 13_776 ?
Pb1 Br1 3.010(9) 3_765 ?
Pb1 Br1 3.010(9) . ?
Pb1 Br1 3.010(9) 2_654 ?
N1 N1 1.9(3) 14_568 ?
N1 N1 1.9(3) 3_665 ?
N1 C1 1.66(10) 3_665 ?
N1 C1 1.66(10) 18_668 ?
N1 C1 1.66(10) . ?
N1 C1 1.66(10) 16_558 ?
N1 C2 1.9(2) . ?
N1 C2 1.9(2) 14_568 ?
C1 C2 1.34(15) . ?

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 14_677 2_654 ?
Br1 Pb1 Br1 98.4(2) 2_654 . ?
Br1 Pb1 Br1 98.4(2) 14_677 15_566 ?
Br1 Pb1 Br1 98.4(2) . 15_566 ?
Br1 Pb1 Br1 180.0 13_776 . ?
Br1 Pb1 Br1 81.6(2) . 3_765 ?
Br1 Pb1 Br1 81.6(2) 14_677 3_765 ?
Br1 Pb1 Br1 98.4(2) 14_677 13_776 ?
Br1 Pb1 Br1 98.4(2) 13_776 3_765 ?
Br1 Pb1 Br1 98.4(2) 2_654 3_765 ?
Br1 Pb1 Br1 180.0 15_566 3_765 ?
Br1 Pb1 Br1 81.6(2) 2_654 13_776 ?
Br1 Pb1 Br1 81.6(2) 2_654 15_566 ?
Br1 Pb1 Br1 81.6(2) 13_776 15_566 ?
Br1 Pb1 Br1 81.6(2) 14_677 . ?
Pb1 Br1 Pb1 82.1(3) 2_655 . ?
N1 N1 N1 60.00(6) 3_665 14_568 ?
N1 N1 C2 62(5) 3_665 . ?
N1 N1 C2 62(5) 14_568 14_568 ?
N1 N1 C2 62(5) 3_665 14_568 ?
N1 N1 C2 62(5) 14_568 . ?
C1 N1 N1 56(6) 16_558 14_568 ?
C1 N1 N1 56(6) 18_668 3_665 ?
C1 N1 N1 96(7) 16_558 3_665 ?
C1 N1 N1 96(7) 18_668 14_568 ?
C1 N1 N1 56(6) . 14_568 ?
C1 N1 N1 96(7) . 3_665 ?
C1 N1 N1 96(7) 3_665 14_568 ?
C1 N1 N1 56(6) 3_665 3_665 ?
C1 N1 C1 82(9) 16_558 18_668 ?
C1 N1 C1 90(7) 3_665 18_668 ?
C1 N1 C1 82(9) . 3_665 ?
C1 N1 C1 90(7) 16_558 . ?
C1 N1 C1 149(10) . 18_668 ?
C1 N1 C1 149(10) 16_558 3_665 ?
C1 N1 C2 43(5) . . ?
C1 N1 C2 116(7) 18_668 . ?
C1 N1 C2 116(7) 3_665 14_568 ?
C1 N1 C2 43(5) 18_668 14_568 ?
C1 N1 C2 116(7) . 14_568 ?
C1 N1 C2 116(7) 16_558 . ?
C1 N1 C2 43(5) 16_558 14_568 ?
C1 N1 C2 43(5) 3_665 . ?
C2 N1 C2 113(10) . 14_568 ?
N1 C1 N1 68(10) . 14_568 ?
C2 C1 N1 80(10) . 14_568 ?
C2 C1 N1 80(10) . . ?
N1 C2 N1 57(9) . 3_665 ?
N1 C2 N1 57(9) 14_568 3_665 ?
N1 C2 N1 57(9) . 14_568 ?
C1 C2 N1 57(10) . . ?
C1 C2 N1 57(10) 3_665 3_665 ?
C1 C2 N1 57(10) . 14_568 ?
C1 C2 N1 103(10) . 3_665 ?
C1 C2 N1 57(10) 3_665 . ?
C1 C2 N1 57(10) 5_565 3_665 ?
C1 C2 N1 103(10) 5_565 . ?
C1 C2 N1 103(10) 3_665 14_568 ?
C1 C2 N1 57(10) 5_565 14_568 ?
C1 C2 C1 109(10) . 3_665 ?
C1 C2 C1 109(10) . 5_565 ?
C1 C2 C1 109(10) 3_665 5_565 ?

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
N1 N1 C1 N1 -48(4) 3_665 . . 14_568 ?
N1 N1 C1 C2 83(8) 14_568 . . . ?
N1 N1 C1 C2 36(8) 3_665 . . . ?
N1 C1 C2 N1 69(10) 14_568 . . . ?
N1 C1 C2 N1 -69(10) . . . 14_568 ?
N1 C1 C2 N1 34(5) 14_568 . . 3_665 ?
N1 C1 C2 N1 -34(5) . . . 3_665 ?
N1 C1 C2 C1 -25(18) 14_568 . . 5_565 ?
N1 C1 C2 C1 94(17) 14_568 . . 3_665 ?
N1 C1 C2 C1 -94(17) . . . 5_565 ?
N1 C1 C2 C1 25(18) . . . 3_665 ?
C1 N1 C1 N1 -102(4) 3_665 . . 14_568 ?
C1 N1 C1 N1 -26(3) 18_668 . . 14_568 ?
C1 N1 C1 N1 48(10) 16_558 . . 14_568 ?
C1 N1 C1 C2 57(7) 18_668 . . . ?
C1 N1 C1 C2 -19(10) 3_665 . . . ?
C1 N1 C1 C2 131(10) 16_558 . . . ?
C2 N1 C1 N1 13(10) 14_568 . . 14_568 ?
C2 N1 C1 N1 -83(8) . . . 14_568 ?
C2 N1 C1 C2 97(12) 14_568 . . . ?

_shelx_res_file                  
;
TITL t R = New: P63/mmc
    t.res
    created by SHELXL-2017/1 at 21:57:40 on 23-Mar-2022
CELL 0.71073 9.7659 9.7659 7.9042 90 90 120
ZERR 2 0.0016 0.0016 0.0007 0 0 0
LATT 1
SYMM -Y+X,+X,0.5+Z
SYMM -Y,+X-Y,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y-X,-X,+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y,-X,0.5-Z
SYMM -Y+X,-Y,-Z
SYMM +X,+X-Y,0.5-Z
SYMM +Y,+X,-Z
SYMM +Y-X,+Y,0.5-Z
SYMM -X,-X+Y,-Z
SFAC C Br N Pb
UNIT 16 6 6 2

L.S. 15
PLAN  2
CONF
fmap 2
acta
MORE -1
REM <olex2.extras>
REM <HklSrc "%.\\t.hkl">
REM </olex2.extras>

WGHT    0.059900   11.321301
FVAR       0.52540
PB1   4    1.000000    1.000000    0.500000    10.08333    0.23814    0.23814 =
         0.07181    0.00000    0.00000    0.11907
BR1   2    0.731610    0.865805    0.750000    10.25000    0.22854    0.41900 =
         0.14781    0.00000    0.00000    0.11427
N1    3    0.270161    0.729839    1.250000    10.16667    0.35156
C1    1    0.407804    0.815607    1.102076    10.33333    0.34413
C2    1    0.333333    0.666667    1.044236    10.16667    0.41445
HKLF 4




REM  t R = New: P63/mmc
REM R1 =  0.1935 for     156 Fo > 4sig(Fo)  and  0.3405 for all     385 data
REM     14 parameters refined using      0 restraints

END

WGHT      0.0599     11.3203

REM Highest difference peak  0.716,  deepest hole -0.688,  1-sigma level  0.125
Q1    1   1.0000  1.0000  0.6527  10.16667  0.05    0.72
Q2    1   1.0531  0.9469  0.5987  10.50000  0.05    0.64
;
_shelx_res_checksum              29800
_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_t_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2163391'
loop_
_audit_author_name
_audit_author_address
'Zhenhong Wei'
;CCDC
China
;
_audit_update_record             
;
2022-03-30 deposited with the CCDC.	2022-05-02 downloaded from the CCDC.
;
_audit_creation_date             2022-03-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'Br7 Pb2, 4(C3 N)'
_chemical_formula_sum            'C12 Br7 N4 Pb2'
_chemical_formula_weight         1173.86
_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'
N N 0.0061 0.0033 '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'

_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      orthorhombic
_space_group_IT_number           57
_space_group_name_H-M_alt        'P b c m'
_space_group_name_Hall           '-P 2c 2b'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y-1/2, z'

_cell_length_a                   10.1747(9)
_cell_length_b                   15.8777(17)
_cell_length_c                   7.9470(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1283.8(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1359
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.4830
_cell_measurement_theta_min      2.0060
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.994
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            color
_exptl_crystal_density_diffrn    3.037
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1018.0
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5349
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.002
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                664
_reflns_number_total             1222
_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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         6.759
_refine_diff_density_min         -1.852
_refine_diff_density_rms         0.595
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.598
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1221
_refine_ls_number_restraints     110
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.1243
_refine_ls_restrained_S_all      1.533
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3871
_refine_ls_wR_factor_ref         0.4280
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N1A-N2A
 1.55 with sigma of 0.05
 N1A-C1
 1.55 with sigma of 0.05
 C1-C2A
 1.55 with sigma of 0.05
 C3-C2A
 1.55 with sigma of 0.05
 N2A-C3
 1.55 with sigma of 0.05
 N2A-C2A
 2.5 with sigma of 0.05
 N1A-C2A
 2.5 with sigma of 0.05
 N1-N2
 1.55 with sigma of 0.05
 N1-C1
 1.55 with sigma of 0.05
 C1-C2
 1.55 with sigma of 0.05
 C3-C2
 1.55 with sigma of 0.05
 C3-N2
 1.55 with sigma of 0.05
 N1-C2
 2.5 with sigma of 0.05
2. Rigid bond restraints
 N1, N2, C2, N1A, N2A, C2A, C3, C1
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
3. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C2 \\sim N1A \\sim N2A \\sim C2A \\sim C3 \\sim C1: within 2A
with sigma of 0.05 and sigma for terminal atoms of 0.1 within 2A
4. Others
 Sof(C2A)=1-FVAR(1)
 Sof(N1A)=Sof(N2A)=0.5*(1-FVAR(2))
 Sof(N1)=Sof(N2)=0.5*FVAR(2)
 Sof(C2)=FVAR(1)
 Fixed Sof: Br2(0.25)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.18999(7) 0.250000 0.500000 0.0820(3) Uani 1 2 d S T P . .
Br1 Br -0.0036(3) 0.1790(3) 0.250000 0.1852(15) Uani 1 2 d S T P . .
Br2 Br 0.4316(5) 0.250000 0.000000 0.0842(14) Uani 0.5 2 d S T P . .
Br3 Br 0.1916(4) 0.3934(3) 0.250000 0.1567(18) Uani 1 2 d S T P . .
Br4 Br 0.3832(3) 0.1739(2) 0.250000 0.1458(12) Uani 1 2 d S T P . .
N1 N 0.285(2) 0.835(2) 0.250000 0.250(9) Uani 0.58(3) 2 d DS TU P A 1
N2 N 0.146(3) 0.867(2) 0.250000 0.258(10) Uani 0.58(3) 2 d DS TU P A 1
C2 C 0.335(3) 0.932(2) 0.477(3) 0.259(8) Uani 0.58(3) 1 d D U P A 1
N1A N 0.387(3) 0.9801(16) 0.250000 0.264(9) Uani 0.42(3) 2 d DS TU P A 2
N2A N 0.237(3) 0.990(2) 0.250000 0.257(10) Uani 0.42(3) 2 d DS TU P A 2
C2A C 0.298(3) 0.8711(16) 0.448(3) 0.254(8) Uani 0.42(3) 1 d D U P A 2
C1 C 0.402(2) 0.8895(13) 0.316(2) 0.258(7) Uani 1 1 d D U . . .
C3 C 0.192(2) 0.9322(15) 0.389(3) 0.252(7) Uani 1 1 d D U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0905(6) 0.1014(7) 0.0541(6) 0.0000(4) 0.000 0.000
Br1 0.155(2) 0.285(4) 0.116(2) 0.000 0.000 -0.122(2)
Br2 0.099(3) 0.104(3) 0.050(2) 0.0049(19) 0.000 0.000
Br3 0.244(5) 0.097(2) 0.129(3) 0.000 0.000 0.006(2)
Br4 0.129(2) 0.197(3) 0.112(2) 0.000 0.000 0.0620(19)
N1 0.350(15) 0.234(16) 0.166(16) 0.000 0.000 0.054(14)
N2 0.364(15) 0.24(2) 0.169(18) 0.000 0.000 0.073(17)
C2 0.361(14) 0.242(15) 0.174(13) -0.010(12) 0.016(12) 0.032(14)
N1A 0.361(14) 0.248(15) 0.183(17) 0.000 0.000 0.028(16)
N2A 0.356(17) 0.244(19) 0.172(19) 0.000 0.000 0.028(17)
C2A 0.359(14) 0.235(14) 0.167(14) -0.007(12) 0.009(13) 0.036(13)
C1 0.368(11) 0.229(12) 0.175(13) -0.014(11) 0.011(11) 0.036(12)
C3 0.357(12) 0.248(13) 0.150(13) -0.010(11) 0.009(11) 0.037(11)

_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 3.017(3) 7_566 ?
Pb1 Br1 3.017(3) . ?
Pb1 Br2 2.459(5) 6_556 ?
Pb1 Br3 3.022(3) 7_566 ?
Pb1 Br3 3.022(3) . ?
Pb1 Br4 3.046(2) 7_566 ?
Pb1 Br4 3.046(2) . ?
Br2 Br4 2.377(2) 7_565 ?
Br2 Br4 2.377(2) . ?
N1 N2 1.51(3) . ?
N1 C1 1.56(3) 6_556 ?
N1 C1 1.56(3) . ?
N2 C3 1.58(3) 6_556 ?
N2 C3 1.58(3) . ?
C2 C1 1.60(3) . ?
C2 C3 1.61(3) . ?
N1A N2A 1.53(3) . ?
N1A C1 1.54(3) 6_556 ?
N1A C1 1.54(3) . ?
N2A C3 1.50(3) . ?
N2A C3 1.50(3) 6_556 ?
C2A C1 1.52(3) . ?
C2A C3 1.52(3) . ?
C1 C1 1.04(4) 6_556 ?

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 98.47(12) 7_566 . ?
Br1 Pb1 Br3 98.91(9) . 7_566 ?
Br1 Pb1 Br3 81.51(9) . . ?
Br1 Pb1 Br3 81.51(9) 7_566 7_566 ?
Br1 Pb1 Br3 98.91(9) 7_566 . ?
Br1 Pb1 Br4 80.99(8) 7_566 7_566 ?
Br1 Pb1 Br4 178.57(10) . 7_566 ?
Br1 Pb1 Br4 81.00(8) . . ?
Br1 Pb1 Br4 178.57(10) 7_566 . ?
Br2 Pb1 Br1 130.77(6) 6_556 . ?
Br2 Pb1 Br1 130.77(6) 6_556 7_566 ?
Br2 Pb1 Br3 89.68(7) 6_556 . ?
Br2 Pb1 Br3 89.68(7) 6_556 7_566 ?
Br2 Pb1 Br4 49.79(5) 6_556 7_566 ?
Br2 Pb1 Br4 49.79(5) 6_556 . ?
Br3 Pb1 Br3 179.36(15) . 7_566 ?
Br3 Pb1 Br4 82.33(8) 7_566 7_566 ?
Br3 Pb1 Br4 97.25(8) . 7_566 ?
Br3 Pb1 Br4 97.25(8) 7_566 . ?
Br3 Pb1 Br4 82.33(8) . . ?
Br4 Pb1 Br4 99.57(11) 7_566 . ?
Pb1 Br1 Pb1 82.39(8) 6_556 . ?
Br4 Br2 Pb1 78.05(13) 7_565 6_556 ?
Br4 Br2 Pb1 78.05(13) . 6_556 ?
Br4 Br2 Br4 156.1(3) 7_565 . ?
Pb1 Br3 Pb1 82.22(10) 6_556 . ?
Pb1 Br4 Pb1 81.44(8) . 6_556 ?
Br2 Br4 Pb1 118.49(15) 6_556 6_556 ?
Br2 Br4 Pb1 118.49(15) . . ?
Br2 Br4 Pb1 52.17(12) . 6_556 ?
Br2 Br4 Pb1 52.17(12) 6_556 . ?
Br2 Br4 Br2 113.39(17) 6_556 . ?
N2 N1 C1 122(2) . 6_556 ?
N2 N1 C1 122(2) . . ?
C1 N1 C1 39.0(15) 6_556 . ?
N1 N2 C3 86.5(19) . 6_556 ?
N1 N2 C3 86.5(19) . . ?
C3 N2 C3 88(2) 6_556 . ?
C1 C2 C3 92.3(17) . . ?
C1 N1A N2A 101(2) 6_556 . ?
C1 N1A N2A 101(2) . . ?
C1 N1A C1 39.6(15) . 6_556 ?
C3 N2A N1A 104.0(17) 6_556 . ?
C3 N2A N1A 104.0(17) . . ?
C3 N2A C3 94(2) . 6_556 ?
C1 C2A C3 98.9(18) . . ?
N1 C1 C2 99.8(17) . . ?
C2A C1 N1A 110.0(18) . . ?
C1 C1 N1 70.5(8) 6_556 . ?
C1 C1 C2 143.1(14) 6_556 . ?
C1 C1 N1A 70.2(8) 6_556 . ?
C1 C1 C2A 133.7(14) 6_556 . ?
N2 C3 C2 125(2) . . ?
N2A C3 C2A 114(2) . . ?

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
N1 N2 C3 C2 -7(3) . . . . ?
N2 N1 C1 C2 40(2) . . . . ?
N2 N1 C1 C1 -102.8(14) . . . 6_556 ?
N1A N2A C3 C2A -14(3) . . . . ?
N2A N1A C1 C2A -36.4(19) . . . . ?
N2A N1A C1 C1 94.1(8) . . . 6_556 ?
C1 N1 N2 C3 67.5(16) . . . 6_556 ?
C1 N1 N2 C3 -21.1(18) . . . . ?
C1 N1 N2 C3 21.1(18) 6_556 . . 6_556 ?
C1 N1 N2 C3 -67.5(16) 6_556 . . . ?
C1 N1 C1 C2 143.1(15) 6_556 . . . ?
C1 C2 C3 N2 28(3) . . . . ?
C1 N1A N2A C3 -69.4(16) . . . 6_556 ?
C1 N1A N2A C3 -28.9(18) 6_556 . . 6_556 ?
C1 N1A N2A C3 69.4(16) 6_556 . . . ?
C1 N1A N2A C3 28.9(18) . . . . ?
C1 N1A C1 C2A -130.5(15) 6_556 . . . ?
C1 C2A C3 N2A -7(3) . . . . ?
C3 N2 C3 C2 -94(3) 6_556 . . . ?
C3 C2 C1 N1 -32(2) . . . . ?
C3 C2 C1 C1 39(3) . . . 6_556 ?
C3 N2A C3 C2A 91(2) 6_556 . . . ?
C3 C2A C1 N1A 27(2) . . . . ?
C3 C2A C1 C1 -54(2) . . . 6_556 ?

_shelx_res_file                  
;
TITL t in Pbcm
    t.res
    created by SHELXL-2017/1 at 17:43:00 on 26-Mar-2022
CELL 0.71073 10.1747 15.8777 7.947 90 90 90
ZERR 12 0.0009 0.0017 0.0005 0 0 0
LATT 1
SYMM -X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM +X,0.5-Y,-Z
SFAC C H N Br Pb
UNIT 12 12 12 12 12
DFIX 1.55 0.05 N1A N2A
DFIX 1.55 0.05 N1A C1
DFIX 1.55 0.05 C1 C2A
DFIX 1.55 0.05 C3 C2A
DFIX 1.55 0.05 N2A C3
DFIX 2.5 0.05 N2A C2A
DFIX 2.5 0.05 N1A C2A
DFIX 1.55 0.05 N1 N2
DFIX 1.55 0.05 N1 C1
DFIX 1.55 0.05 C1 C2
DFIX 1.55 0.05 C3 C2
DFIX 1.55 0.05 C3 N2
DFIX 2.5 0.05 N1 C2
SIMU 0.05 0.1 2 N1 N2 C2 N1A N2A C2A C3 C1
DELU 0.05 0.05 N1 N2 C2 N1A N2A C2A C3 C1

L.S. 35
PLAN  16
CONF
BOND
damp 2000
fmap 2
acta
MORE -1
OMIT -3 50
REM <olex2.extras>
REM <HklSrc "%.\\330_210921_398K_auto.hkl">
REM </olex2.extras>

WGHT    0.200000
FVAR       0.76744   0.58472
PB1   5    0.189993    0.250000    0.500000    10.50000    0.09049    0.10142 =
         0.05414    0.00004    0.00000    0.00000
BR1   4   -0.003596    0.178953    0.250000    10.50000    0.15478    0.28457 =
         0.11634    0.00000    0.00000   -0.12214
BR2   4    0.431637    0.250000    0.000000    10.25000    0.09928    0.10386 =
         0.04959    0.00491    0.00000    0.00000
BR3   4    0.191647    0.393374    0.250000    10.50000    0.24408    0.09666 =
         0.12941    0.00000    0.00000    0.00599
BR4   4    0.383249    0.173855    0.250000    10.50000    0.12900    0.19661 =
         0.11169    0.00000    0.00000    0.06199
PART 1
N1    3    0.285020    0.835174    0.250000    20.50000    0.35031    0.23411 =
         0.16642    0.00000    0.00000    0.05433
N2    3    0.145647    0.867436    0.250000    20.50000    0.36366    0.24203 =
         0.16855    0.00000    0.00000    0.07289
C2    1    0.334646    0.931851    0.476936    21.00000    0.36058    0.24215 =
         0.17425   -0.01043    0.01622    0.03192
PART 2
N1A   3    0.386721    0.980088    0.250000   -20.50000    0.36096    0.24845 =
         0.18299    0.00000    0.00000    0.02811
N2A   3    0.237009    0.989605    0.250000   -20.50000    0.35633    0.24401 =
         0.17177    0.00000    0.00000    0.02759
C2A   1    0.297978    0.871065    0.448031   -21.00000    0.35866    0.23516 =
         0.16728   -0.00720    0.00920    0.03560
PART 0
C1    1    0.402406    0.889478    0.315655    11.00000    0.36836    0.22945 =
         0.17499   -0.01419    0.01053    0.03569
C3    1    0.192363    0.932224    0.388518    11.00000    0.35666    0.24838 =
         0.14998   -0.01023    0.00867    0.03691
HKLF 4




REM  t in Pbcm
REM R1 =  0.1243 for     664 Fo > 4sig(Fo)  and  0.1625 for all    1221 data
REM     90 parameters refined using    110 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  6.759,  deepest hole -1.852,  1-sigma level  0.595
Q1    1   0.2454  0.1735  0.2500  10.50000  0.05    6.76
Q2    1   0.3656  0.6871  0.2500  10.50000  0.05    5.50
Q3    1   0.5659  0.8955  0.2500  10.50000  0.05    5.02
Q4    1   0.3068  0.9117  0.5080  11.00000  0.05    1.40
Q5    1   0.1975  0.9023  0.2500  10.50000  0.05    1.26
Q6    1   0.1330  0.9656  0.2500  10.50000  0.05    0.99
Q7    1   0.1852  0.9340  0.4334  11.00000  0.05    0.85
Q8    1   0.0212  0.7961  0.2500  10.50000  0.05    0.85
Q9    1   0.2924  0.7500  0.5000  10.50000  0.05    0.79
Q10   1   0.4259  0.9472  0.4277  11.00000  0.05    0.72
Q11   1   0.3359  0.8308  0.4730  11.00000  0.05    0.59
Q12   1   0.1789  1.1013  0.2500  10.50000  0.05    0.56
Q13   1   0.3932  0.8499  0.4581  11.00000  0.05    0.55
Q14   1   0.2489  0.5336  0.2500  10.50000  0.05    0.54
Q15   1   0.3625  0.9509  0.2500  10.50000  0.05    0.54
Q16   1   0.0118  0.9651  0.2500  10.50000  0.05    0.50
;
_shelx_res_checksum              26836
_olex2_submission_special_instructions 'No special instructions were received'
