# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_exp_5218_auto_corr
_database_code_depnum_ccdc_archive 'CCDC 2231790'
loop_
_audit_author_name
_audit_author_address
'PENG WANG'
;FUJIAN INSTITUTE OF RESEARCH ON THE STRUCTURE
China
;
_audit_update_record             
;
2022-12-20 deposited with the CCDC.	2024-03-04 downloaded from the CCDC.
;
_audit_creation_date             2022-12-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br10 Pb3, C4 H14 N2, 2(C H6 N)'
_chemical_formula_sum            'C6 H26 Br10 N4 Pb3'
_chemical_formula_weight         1574.98
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNPbBr
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'
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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   8.3682(5)
_cell_length_b                   43.331(3)
_cell_length_c                   8.3003(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3009.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6977
_cell_measurement_temperature    297.34(10)
_cell_measurement_theta_max      30.5390
_cell_measurement_theta_min      2.5070
_shelx_estimated_absorpt_T_max   0.140
_shelx_estimated_absorpt_T_min   0.040
_exptl_absorpt_coefficient_mu    30.018
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.454
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.476
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2744
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 -35 6 0.0418
-8 35 -6 0.1448
-7 -7 9 0.0975
7 7 -9 0.0595
0 61 0 0.0916
0 -61 0 0.0166

_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.108
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7.8919 -34.5148 5.6801 0.1763 0.7299 -0.6605
-7.8919 34.5148 -5.6801 -0.1763 -0.7299 0.6605
-7.2383 -6.7312 9.1534 0.1568 0.6651 0.7301
7.2383 6.7312 -9.1534 -0.1568 -0.6651 -0.7301
-0.0708 61.1468 0.1222 -0.9120 -0.2704 0.3085
0.0708 -61.1468 -0.1222 0.9120 0.2704 -0.3085

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.802
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15044
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.802
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.447
_diffrn_reflns_theta_min         2.498
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.34(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.802
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -36.00  10.36   0.38    1.39    --   -5.06 101.00  69.00  122
  2  ω     -9.00  57.12   0.38    1.39    --    6.70  31.00-125.00  174
  3  ω    -18.00  27.22   0.38    1.39    --   -5.06 -99.00  90.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0301630000
_diffrn_orient_matrix_UB_12      -0.0149145000
_diffrn_orient_matrix_UB_13      -0.0176884000
_diffrn_orient_matrix_UB_21      0.0144259000
_diffrn_orient_matrix_UB_22      -0.0045660000
_diffrn_orient_matrix_UB_23      0.0807074000
_diffrn_orient_matrix_UB_31      -0.0778902000
_diffrn_orient_matrix_UB_32      0.0049113000
_diffrn_orient_matrix_UB_33      0.0217847000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2891
_reflns_number_total             3702
_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       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.312
_refine_diff_density_min         -3.365
_refine_diff_density_rms         0.435
_refine_ls_extinction_coef       0.00052(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         3702
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0611
_refine_ls_restrained_S_all      1.077
_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)+(0.0767P)²+45.9624P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1562
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2D,H2E)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), C1(H1D,H1E,H1F)
;
_atom_sites_solution_hydrogens   geom
_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 0.61470(5) 0.60898(2) 0.50014(4) 0.02000(17) Uani 1 1 d . . . . .
Pb2 Pb 0.62745(7) 0.750000 0.48864(7) 0.02161(18) Uani 1 2 d S T P . .
Br1 Br 0.4276(2) 0.750000 0.7981(2) 0.0416(5) Uani 1 2 d S T P . .
Br6 Br 0.6001(2) 0.54456(3) 0.56264(18) 0.0477(4) Uani 1 1 d . . . . .
Br2 Br 0.8123(3) 0.750000 0.1800(3) 0.0480(5) Uani 1 2 d S T P . .
Br4 Br 0.84266(18) 0.61614(4) 0.77209(19) 0.0497(4) Uani 1 1 d . . . . .
Br5 Br 0.88160(16) 0.59937(4) 0.26787(18) 0.0487(4) Uani 1 1 d . . . . .
Br3 Br 0.6053(2) 0.68171(3) 0.50582(18) 0.0474(5) Uani 1 1 d . . . . .
C3 C 1.0167(16) 0.5083(3) 0.4230(15) 0.040(3) Uani 1 1 d . . . . .
H3A H 0.921660 0.519571 0.391520 0.048 Uiso 1 1 calc R U . . .
H3B H 1.038141 0.493095 0.339789 0.048 Uiso 1 1 calc R U . . .
N1 N 1.1892(18) 0.6888(3) 0.5786(19) 0.065(4) Uani 1 1 d . . . . .
H1A H 1.276615 0.695431 0.528487 0.078 Uiso 1 1 calc R U . . .
H1B H 1.216695 0.675637 0.656283 0.078 Uiso 1 1 calc R U . . .
H1C H 1.137597 0.704744 0.621501 0.078 Uiso 1 1 calc R U . . .
N2 N 1.1251(18) 0.5576(3) 0.5307(17) 0.057(4) Uani 1 1 d . . . . .
H2A H 1.089403 0.572922 0.469281 0.069 Uiso 1 1 calc R U . . .
H2B H 1.214781 0.563390 0.579759 0.069 Uiso 1 1 calc R U . . .
H2C H 1.051727 0.552837 0.604273 0.069 Uiso 1 1 calc R U . . .
C1 C 1.088(3) 0.6736(5) 0.467(3) 0.091(8) Uani 1 1 d . . . . .
H1D H 1.104835 0.682173 0.361256 0.137 Uiso 1 1 calc R U . . .
H1E H 0.978751 0.676471 0.497738 0.137 Uiso 1 1 calc R U . . .
H1F H 1.112845 0.651993 0.465097 0.137 Uiso 1 1 calc R U . . .
C2 C 1.1570(18) 0.5307(3) 0.431(2) 0.047(4) Uani 1 1 d . . . . .
H2D H 1.249639 0.519971 0.473090 0.056 Uiso 1 1 calc R U . . .
H2E H 1.182529 0.537541 0.322585 0.056 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 Br6 2.8415(14) . ?
Pb1 Br4 2.9716(14) . ?
Pb1 Br4 2.9755(13) 6_557 ?
Pb1 Br5 2.9797(13) . ?
Pb1 Br5 2.9877(14) 6_556 ?
Pb1 Br3 3.1531(14) . ?
Pb2 Br1 3.0649(19) . ?
Pb2 Br1 3.0730(19) 6_657 ?
Pb2 Br2 2.986(2) 6_556 ?
Pb2 Br2 2.9924(19) . ?
Pb2 Br3 2.9682(13) 7_575 ?
Pb2 Br3 2.9682(13) . ?
C3 C3 1.49(3) 5_766 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.526(19) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.42(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C2 1.453(19) . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 H1F 0.9600 . ?
C2 H2D 0.9700 . ?
C2 H2E 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
Br6 Pb1 Br4 89.51(5) . . ?
Br6 Pb1 Br4 87.34(5) . 6_557 ?
Br6 Pb1 Br5 90.75(5) . . ?
Br6 Pb1 Br5 88.35(5) . 6_556 ?
Br6 Pb1 Br3 167.97(5) . . ?
Br4 Pb1 Br4 89.862(13) . 6_557 ?
Br4 Pb1 Br5 91.43(5) . . ?
Br4 Pb1 Br5 177.69(5) 6_557 . ?
Br4 Pb1 Br5 177.74(5) . 6_556 ?
Br4 Pb1 Br5 89.32(5) 6_557 6_556 ?
Br4 Pb1 Br3 82.36(5) 6_557 . ?
Br4 Pb1 Br3 84.27(4) . . ?
Br5 Pb1 Br5 89.324(14) . 6_556 ?
Br5 Pb1 Br3 99.67(5) . . ?
Br5 Pb1 Br3 97.70(5) 6_556 . ?
Br1 Pb2 Br1 87.892(19) . 6_657 ?
Br2 Pb2 Br1 94.05(6) . 6_657 ?
Br2 Pb2 Br1 172.78(6) 6_556 6_657 ?
Br2 Pb2 Br1 84.89(6) 6_556 . ?
Br2 Pb2 Br1 178.06(6) . . ?
Br2 Pb2 Br2 93.16(2) 6_556 . ?
Br3 Pb2 Br1 85.74(3) . . ?
Br3 Pb2 Br1 91.34(4) . 6_657 ?
Br3 Pb2 Br1 91.34(4) 7_575 6_657 ?
Br3 Pb2 Br1 85.74(3) 7_575 . ?
Br3 Pb2 Br2 94.21(3) . . ?
Br3 Pb2 Br2 88.13(4) . 6_556 ?
Br3 Pb2 Br2 88.13(4) 7_575 6_556 ?
Br3 Pb2 Br2 94.21(3) 7_575 . ?
Br3 Pb2 Br3 170.97(7) . 7_575 ?
Pb2 Br1 Pb2 158.24(8) . 6_557 ?
Pb2 Br2 Pb2 149.08(9) 6_656 . ?
Pb1 Br4 Pb1 164.34(7) . 6_657 ?
Pb1 Br5 Pb1 162.12(7) . 6_656 ?
Pb2 Br3 Pb1 173.83(7) . . ?
C3 C3 H3A 108.7 5_766 . ?
C3 C3 H3B 108.7 5_766 . ?
C3 C3 C2 114.4(15) 5_766 . ?
H3A C3 H3B 107.6 . . ?
C2 C3 H3A 108.7 . . ?
C2 C3 H3B 108.7 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C2 N2 H2A 109.5 . . ?
C2 N2 H2B 109.5 . . ?
C2 N2 H2C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
N1 C1 H1E 109.5 . . ?
N1 C1 H1F 109.5 . . ?
H1D C1 H1E 109.5 . . ?
H1D C1 H1F 109.5 . . ?
H1E C1 H1F 109.5 . . ?
C3 C2 H2D 108.9 . . ?
C3 C2 H2E 108.9 . . ?
N2 C2 C3 113.2(13) . . ?
N2 C2 H2D 108.9 . . ?
N2 C2 H2E 108.9 . . ?
H2D C2 H2E 107.8 . . ?

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
C3 C3 C2 N2 -69(2) 5_766 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.438
_oxdiff_exptl_absorpt_empirical_full_min 0.418
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_20220716mazuihaogao_0m
_database_code_depnum_ccdc_archive 'CCDC 2231791'
loop_
_audit_author_name
_audit_author_address
'PENG WANG'
;FUJIAN INSTITUTE OF RESEARCH ON THE STRUCTURE
China
;
_audit_update_record             
;
2022-12-20 deposited with the CCDC.	2024-03-04 downloaded from the CCDC.
;
_audit_creation_date             2022-12-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br10 Pb3, C4 H14 N2, 2(C H6 N)'
_chemical_formula_sum            'C6 H26 Br10 N4 Pb3'
_chemical_formula_weight         1574.98
_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'
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'
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      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   8.3213(4)
_cell_length_b                   8.4780(6)
_cell_length_c                   42.894(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3026.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4069
_cell_measurement_temperature    343.02
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.85
_shelx_estimated_absorpt_T_max   0.138
_shelx_estimated_absorpt_T_min   0.112
_exptl_absorpt_coefficient_mu    29.855
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1592 before and 0.0743 after correction.
The Ratio of minimum to maximum transmission is 0.2655.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.457
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            12113
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_min         3.560
_diffrn_ambient_temperature      343.02
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_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                1329
_reflns_number_total             1879
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.874
_refine_diff_density_min         -2.718
_refine_diff_density_rms         0.425
_refine_ls_extinction_coef       0.00085(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1879
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0592
_refine_ls_restrained_S_all      1.100
_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)+(0.0987P)²+43.8536P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1851
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C2 = C2-C3
 1.5 with sigma of 0.02
 C3-C3_$1
 1.5 with sigma of 0.02
 N1-C1
 1.5 with sigma of 0.02
 H1A-H1D
 2.12 with sigma of 0.01
 C3-N2
 2.5 with sigma of 0.04
3. Rigid bond restraints
 N1, C1, C3, C2, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Br4(0.5) N2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) C2(0.5) H2D(0.5) H2E(0.5) N1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C1(0.5)
 H1D(0.5) H1E(0.5) H1F(0.5)
6.a Riding coordinates:
 C3(H3A,H3B)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2D,H2E)
6.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N1(H1A,H1B,H1C), C1(H1D,H1E,H1F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.500000 0.37634(10) 0.750000 0.0380(3) Uani 1 4 d S T P . .
Pb2 Pb 0.500000 0.37462(8) 0.60902(2) 0.0391(3) Uani 1 2 d S T P . .
Br2 Br 0.500000 0.3765(5) 0.68112(6) 0.127(2) Uani 1 2 d S T P A .
Br1 Br 0.2493(5) 0.1266(3) 0.750000 0.1263(16) Uani 1 2 d S T P . .
Br3 Br 0.2530(3) 0.1218(2) 0.60861(8) 0.1314(14) Uani 1 1 d . . . . .
Br4 Br 0.4405(5) 0.4015(5) 0.54338(8) 0.0860(12) Uani 0.5 1 d . . P A -1
N2 N 0.545(4) -0.150(3) 0.5602(7) 0.113(12) Uani 0.5 1 d D U P B -1
H2A H 0.646163 -0.158078 0.553510 0.136 Uiso 0.5 1 calc R U P B -1
H2B H 0.527387 -0.223041 0.574775 0.136 Uiso 0.5 1 calc R U P B -1
H2C H 0.528886 -0.054917 0.568162 0.136 Uiso 0.5 1 calc R U P B -1
C3 C 0.428(5) -0.021(4) 0.5166(3) 0.129(14) Uani 0.5 1 d D U P B -1
H3A H 0.523297 0.032980 0.523845 0.154 Uiso 0.5 1 d R U P B -1
H3B H 0.332957 0.034390 0.523865 0.154 Uiso 0.5 1 d R U P B -1
C2 C 0.433(5) -0.176(4) 0.5334(10) 0.124(13) Uani 0.5 1 d D U P B -1
H2D H 0.326480 -0.205431 0.540830 0.149 Uiso 0.5 1 calc R U P B -1
H2E H 0.472133 -0.259274 0.519816 0.149 Uiso 0.5 1 calc R U P B -1
N1 N 0.539(9) -0.069(6) 0.6814(10) 0.20(3) Uani 0.5 1 d D U P C -1
H1A H 0.577237 -0.057515 0.662178 0.244 Uiso 0.5 1 calc DR U P C -1
H1B H 0.619611 -0.082584 0.694673 0.244 Uiso 0.5 1 calc R U P C -1
H1C H 0.483947 0.017529 0.686683 0.244 Uiso 0.5 1 calc R U P C -1
C1 C 0.430(7) -0.208(7) 0.6825(13) 0.17(3) Uani 0.5 1 d D U P C -1
H1D H 0.444089 -0.270537 0.664023 0.262 Uiso 0.5 1 calc DR U P C -1
H1E H 0.320220 -0.173535 0.683789 0.262 Uiso 0.5 1 calc R U P C -1
H1F H 0.455003 -0.271181 0.700509 0.262 Uiso 0.5 1 calc R U P C -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 Br2 2.954(3) 10_557 ?
Pb1 Br2 2.954(3) . ?
Pb1 Br1 2.973(3) . ?
Pb1 Br1 2.967(3) 7_556 ?
Pb1 Br1 2.967(3) 5 ?
Pb1 Br1 2.973(3) 3_656 ?
Pb2 Br2 3.093(3) . ?
Pb2 Br3 2.969(2) . ?
Pb2 Br3 2.971(2) 16 ?
Pb2 Br3 2.9695(19) 12_655 ?
Pb2 Br3 2.971(2) 5 ?
Pb2 Br4 2.868(4) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C2 1.499(19) . ?
C3 C3 1.47(2) 4_556 ?
C3 H3A 0.9699 . ?
C3 H3B 0.9696 . ?
C3 C2 1.503(19) . ?
C2 H2D 0.9700 . ?
C2 H2E 0.9700 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.49(2) . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 H1F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br2 179.94(17) 10_557 . ?
Br2 Pb1 Br1 89.98(6) . 7_556 ?
Br2 Pb1 Br1 90.02(6) 10_557 3_656 ?
Br2 Pb1 Br1 89.98(6) 10_557 5 ?
Br2 Pb1 Br1 90.02(6) . . ?
Br2 Pb1 Br1 89.98(6) . 5 ?
Br2 Pb1 Br1 90.02(6) . 3_656 ?
Br2 Pb1 Br1 89.98(6) 10_557 7_556 ?
Br2 Pb1 Br1 90.02(6) 10_557 . ?
Br1 Pb1 Br1 91.069(5) 7_556 . ?
Br1 Pb1 Br1 179.78(16) 5 . ?
Br1 Pb1 Br1 91.069(5) 5 3_656 ?
Br1 Pb1 Br1 179.78(17) 7_556 3_656 ?
Br1 Pb1 Br1 88.71(16) 5 7_556 ?
Br1 Pb1 Br1 89.15(16) . 3_656 ?
Br3 Pb2 Br2 90.56(8) 12_655 . ?
Br3 Pb2 Br2 90.56(9) . . ?
Br3 Pb2 Br2 90.13(9) 5 . ?
Br3 Pb2 Br2 90.13(9) 16 . ?
Br3 Pb2 Br3 178.50(13) . 5 ?
Br3 Pb2 Br3 91.067(5) 12_655 5 ?
Br3 Pb2 Br3 87.59(11) . 12_655 ?
Br3 Pb2 Br3 90.26(11) 5 16 ?
Br3 Pb2 Br3 178.50(13) 12_655 16 ?
Br3 Pb2 Br3 91.067(5) . 16 ?
Br4 Pb2 Br2 168.91(9) . . ?
Br4 Pb2 Br3 79.38(10) . 16 ?
Br4 Pb2 Br3 99.85(11) . 12_655 ?
Br4 Pb2 Br3 93.47(10) . 5 ?
Br4 Pb2 Br3 86.10(10) . . ?
Pb1 Br2 Pb2 179.67(16) . . ?
Pb1 Br1 Pb1 179.78(16) 5_445 . ?
Pb2 Br3 Pb2 178.50(13) . 5_445 ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C2 N2 H2A 109.5 . . ?
C2 N2 H2B 109.5 . . ?
C2 N2 H2C 109.5 . . ?
C3 C3 H3A 101.3 4_556 . ?
C3 C3 H3B 101.2 4_556 . ?
C3 C3 C2 133(5) 4_556 . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3A 103.7 . . ?
C2 C3 H3B 107.0 . . ?
N2 C2 C3 105(2) . . ?
N2 C2 H2D 110.8 . . ?
N2 C2 H2E 110.8 . . ?
C3 C2 H2D 110.8 . . ?
C3 C2 H2E 110.8 . . ?
H2D C2 H2E 108.9 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
N1 C1 H1E 109.5 . . ?
N1 C1 H1F 109.5 . . ?
H1D C1 H1E 109.5 . . ?
H1D C1 H1F 109.5 . . ?
H1E C1 H1F 109.5 . . ?

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
C3 C3 C2 N2 139(2) 4_556 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
