# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_x2
_database_code_depnum_ccdc_archive 'CCDC 1952538'
loop_
_audit_author_name
_audit_author_address
'bo kou'
;Fujian Institute of Research on the Structure of Matter,Chinese Academy of Sciences
China
;
_audit_update_record             
;
2019-09-10 deposited with the CCDC.	2022-11-21 downloaded from the CCDC.
;
_audit_creation_date             2019-09-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C10 H14 N'
_chemical_formula_sum            'C10 H14 Br3 N Pb'
_chemical_formula_weight         595.14
_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           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   14.8489(16)
_cell_length_b                   7.7744(7)
_cell_length_c                   13.5892(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1568.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1775
_cell_measurement_temperature    420(2)
_cell_measurement_theta_max      22.911
_cell_measurement_theta_min      3.018
_shelx_estimated_absorpt_T_max   0.838
_shelx_estimated_absorpt_T_min   0.710
_exptl_absorpt_coefficient_mu    18.370
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1284 before and 0.0473 after correction. The Ratio of minimum to maximum transmission is 0.4352. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.520
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6455
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.542
_diffrn_reflns_theta_min         3.019
_diffrn_ambient_temperature      419.98
_diffrn_detector                 'Bruker APEX3 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX3 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                690
_reflns_number_total             1001
_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 (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         1001
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0268
_refine_ls_restrained_S_all      1.106
_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)+(0.0205P)²+2.8367P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0623
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5-N1
 1.34 with sigma of 0.02
 C6-N1
 1.47 with sigma of 0.02
 C6-C7 = C8-C7
 1.5 with sigma of 0.02
 C3-C4 = C3-C2 = C2-C1
 1.38 with sigma of 0.02
 C5-C3
 1.48 with sigma of 0.02
 C3-N1 = C6-C5 = N1-C7 = C6-C8
 2.4 with sigma of 0.04
3. Restrained planarity
 C5, C2, C3, C1, C2_$1, C4, C3_$1
 with sigma of 0.1
 C6, N1, C5, C3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C4 \\sim C3 \\sim C7 \\sim C8 \\sim C5 \\sim C6 \\sim N1:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: H3(0.25) C7(0.25) H7a(0.25) H7b(0.25) C8(0.25) H8a(0.25) H8b(0.25)
 H8c(0.25) N1(0.25) H1a(0.25) C5(0.25) H5(0.25) C6(0.25) H6a(0.25) H6b(0.25)
6.a Riding coordinates:
 C3(H3)
6.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C6(H6a,H6b)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), N1(H1a), C5(H5)
6.d Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c)
;
_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 0.500000 1.000000 0.08225(7) Uani 1 4 d S T P . .
Br1 Br 0.000000 0.750000 0.82698(5) 0.1078(3) Uani 1 4 d S T P . .
Br2 Br 0.13842(4) 0.250000 0.92043(5) 0.1183(2) Uani 1 2 d S T P . .
C1 C 0.000000 0.250000 0.6679(8) 0.224(3) Uani 1 4 d DS TU P . .
H1 H 0.000000 0.250000 0.736382 0.269 Uiso 1 4 calc RS T P . .
C2 C 0.0775(6) 0.250000 0.6153(5) 0.231(2) Uani 1 2 d DS TU P . .
H2 H 0.132016 0.250000 0.649068 0.277 Uiso 1 2 calc RS T P . .
C4 C 0.000000 0.250000 0.4663(8) 0.226(3) Uani 1 4 d DS TU P . .
H4 H 0.000000 0.250000 0.397890 0.272 Uiso 1 4 calc RS T P . .
C3 C 0.0790(5) 0.250000 0.5150(4) 0.2326(19) Uani 1 2 d DS TU P . .
H3 H 0.133247 0.250000 0.480784 0.279 Uiso 0.25 1 d RS T P A -1
C7 C 0.2468(12) 0.3038(13) 0.2025(7) 0.217(3) Uani 0.25 1 d D U . B -1
H7A H 0.303211 0.344338 0.175008 0.261 Uiso 0.25 1 calc R . . B -1
H7B H 0.199694 0.319569 0.153841 0.261 Uiso 0.25 1 calc R . . B -1
C8 C 0.254(2) 0.1159(13) 0.2309(16) 0.196(5) Uani 0.25 1 d D U . B -1
H8A H 0.216914 0.093875 0.287216 0.294 Uiso 0.25 1 calc GR . . B -1
H8B H 0.315715 0.089395 0.246639 0.294 Uiso 0.25 1 calc GR . . B -1
H8C H 0.234791 0.045445 0.176948 0.294 Uiso 0.25 1 calc GR . . B -1
N1 N 0.1540(8) 0.3501(18) 0.3565(7) 0.229(2) Uani 0.25 1 d D U . B -1
H1A H 0.101827 0.387380 0.339088 0.274 Uiso 0.25 1 calc R . . B -1
C5 C 0.1540(9) 0.2555(13) 0.4395(7) 0.238(2) Uani 0.25 1 d D U . B -1
H5 H 0.204391 0.187715 0.451463 0.285 Uiso 0.25 1 calc R . . B -1
C6 C 0.2250(9) 0.3986(17) 0.2931(7) 0.223(2) Uani 0.25 1 d D U . B -1
H6A H 0.279427 0.399990 0.332616 0.267 Uiso 0.25 1 calc R . . B -1
H6B H 0.213596 0.516717 0.273759 0.267 Uiso 0.25 1 calc R . . B -1

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 0.07966(14) 0.07807(12) 0.08901(14) 0.00241(13) 0.000 0.000
Br1 0.1019(5) 0.1441(6) 0.0775(4) 0.000 0.000 0.000
Br2 0.0898(3) 0.1409(4) 0.1240(4) 0.000 0.0267(3) 0.000
C1 0.192(5) 0.352(6) 0.130(5) 0.000 0.000 0.000
C2 0.182(4) 0.359(4) 0.151(4) 0.000 -0.024(3) 0.000
C4 0.172(5) 0.371(6) 0.136(5) 0.000 0.000 0.000
C3 0.176(3) 0.369(3) 0.152(3) 0.000 0.016(3) 0.000
C7 0.136(5) 0.346(6) 0.171(5) 0.007(5) -0.008(5) -0.015(5)
C8 0.109(8) 0.316(10) 0.163(10) 0.001(11) -0.021(8) -0.015(11)
N1 0.161(4) 0.360(4) 0.165(4) 0.007(4) 0.004(4) -0.010(4)
C5 0.175(4) 0.372(4) 0.166(4) 0.004(4) 0.009(4) -0.005(4)
C6 0.150(4) 0.350(4) 0.169(4) 0.006(4) -0.005(4) -0.014(4)

_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 3.0505(6) . ?
Pb1 Br1 3.0505(6) 9_567 ?
Pb1 Br2 3.0284(5) 9_567 ?
Pb1 Br2 3.0284(5) 2 ?
Pb1 Br2 3.0284(5) . ?
Pb1 Br2 3.0284(5) 10_567 ?
C1 H1 0.9300 . ?
C1 C2 1.355(9) 2 ?
C1 C2 1.355(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.364(9) . ?
C4 H4 0.9300 . ?
C4 C3 1.346(8) . ?
C4 C3 1.346(8) 2 ?
C3 H3 0.9301 . ?
C3 C5 1.515(11) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.515(13) . ?
C7 C6 1.471(12) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N1 H1A 0.8600 . ?
N1 C5 1.346(12) . ?
N1 C6 1.414(13) . ?
C5 H3 0.6420 . ?
C5 H5 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 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 9_567 . ?
Br2 Pb1 Br1 82.315(13) 2 9_567 ?
Br2 Pb1 Br1 82.315(13) 10_567 . ?
Br2 Pb1 Br1 97.685(13) 10_567 9_567 ?
Br2 Pb1 Br1 82.315(13) 9_567 . ?
Br2 Pb1 Br1 97.685(13) 2 . ?
Br2 Pb1 Br1 97.685(13) 9_567 9_567 ?
Br2 Pb1 Br1 97.685(13) . . ?
Br2 Pb1 Br1 82.315(13) . 9_567 ?
Br2 Pb1 Br2 94.514(19) 10_567 . ?
Br2 Pb1 Br2 180.0 9_567 . ?
Br2 Pb1 Br2 85.486(19) 2 . ?
Br2 Pb1 Br2 180.0 10_567 2 ?
Br2 Pb1 Br2 85.487(19) 10_567 9_567 ?
Br2 Pb1 Br2 94.513(19) 2 9_567 ?
Pb1 Br1 Pb1 79.157(18) 2_565 . ?
Pb1 Br2 Pb1 79.849(15) 2 . ?
C2 C1 H1 121.8 2 . ?
C2 C1 H1 121.8 . . ?
C2 C1 C2 116.3(10) 2 . ?
C1 C2 H2 118.6 . . ?
C1 C2 C3 122.8(8) . . ?
C3 C2 H2 118.6 . . ?
C3 C4 H4 119.4 2 . ?
C3 C4 H4 119.4 . . ?
C3 C4 C3 121.2(10) . 2 ?
C2 C3 H3 120.9 . . ?
C2 C3 C5 133.5(8) . . ?
C4 C3 C2 118.5(8) . . ?
C4 C3 H3 120.6 . . ?
C4 C3 C5 107.9(7) . . ?
C5 C3 H3 12.8 . . ?
H7A C7 H7B 108.6 . . ?
C8 C7 H7A 110.4 . . ?
C8 C7 H7B 110.4 . . ?
C6 C7 H7A 110.4 . . ?
C6 C7 H7B 110.4 . . ?
C6 C7 C8 106.6(12) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 N1 H1A 114.5 . . ?
C5 N1 C6 131.0(12) . . ?
C6 N1 H1A 114.5 . . ?
C3 C5 H3 18.7 . . ?
C3 C5 H5 117.2 . . ?
H3 C5 H5 101.2 . . ?
N1 C5 C3 125.6(10) . . ?
N1 C5 H3 140.3 . . ?
N1 C5 H5 117.2 . . ?
C7 C6 H6A 106.7 . . ?
C7 C6 H6B 106.7 . . ?
N1 C6 C7 122.7(12) . . ?
N1 C6 H6A 106.7 . . ?
N1 C6 H6B 106.7 . . ?
H6A C6 H6B 106.6 . . ?

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
C3 H3 N1 0.93 1.88 2.546(11) 126.1 . yes

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
C1 C2 C3 C4 0.000(2) . . . . ?
C1 C2 C3 C5 177.8(5) . . . . ?
C2 C1 C2 C3 0.000(2) 2 . . . ?
C2 C3 C5 N1 -137.8(10) . . . . ?
C4 C3 C5 N1 40.2(12) . . . . ?
C3 C4 C3 C2 0.000(2) 2 . . . ?
C3 C4 C3 C5 -178.3(4) 2 . . . ?
C8 C7 C6 N1 -51(2) . . . . ?
C5 N1 C6 C7 96.6(17) . . . . ?
C6 N1 C5 C3 163.1(12) . . . . ?

_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_new
_database_code_depnum_ccdc_archive 'CCDC 1952539'
loop_
_audit_author_name
_audit_author_address
'bo kou'
;Fujian Institute of Research on the Structure of Matter,Chinese Academy of Sciences
China
;
_audit_update_record             
;
2019-09-10 deposited with the CCDC.	2022-11-21 downloaded from the CCDC.
;
_audit_creation_date             2019-09-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C10 H14 N'
_chemical_formula_sum            'C10 H14 Br3 N Pb'
_chemical_formula_weight         595.14
_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'
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           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+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   14.4126(7)
_cell_length_b                   7.7413(4)
_cell_length_c                   13.0896(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1460.44(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1775
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.911
_cell_measurement_theta_min      3.018
_shelx_estimated_absorpt_T_max   0.827
_shelx_estimated_absorpt_T_min   0.694
_exptl_absorpt_coefficient_mu    19.732
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1284 before and 0.0473 after correction. The Ratio of minimum to maximum transmission is 0.4352. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.707
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0886
_diffrn_reflns_av_unetI/netI     0.1018
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32011
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         44.375
_diffrn_reflns_theta_min         3.057
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker APEX3 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX3 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.813
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                8204
_reflns_number_total             11587
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         3.277
_refine_diff_density_min         -4.551
_refine_diff_density_rms         0.367
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.491(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         11587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0524
_refine_ls_restrained_S_all      0.987
_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)+(0.0208P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1084
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.509(14)
 0.491(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C00E(H00G,H00H), C00F(H00I,H00J)
3.b Aromatic/amide H refined with riding coordinates:
 C005(H005), C006(H006), C008(H008), C009(H009), C00B(H00D), C00C(H00E),
 N00D(H00F)
3.c Idealised Me refined as rotating group:
 C00A(H00A,H00B,H00C)
;
_atom_sites_solution_hydrogens   geom
_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
Pb01 Pb 0.49394(2) 0.48231(3) 0.24630(2) 0.01421(5) Uani 1 1 d . . . . .
Br02 Br 0.48879(5) 0.26386(10) 0.42814(6) 0.01747(13) Uani 1 1 d . . . . .
Br03 Br 0.35526(5) 0.72894(11) 0.32714(6) 0.01768(14) Uani 1 1 d . . . . .
Br04 Br 0.63515(5) 0.70242(10) 0.34414(6) 0.01632(14) Uani 1 1 d . . . . .
C005 C 0.4810(5) 0.3707(11) 0.7096(6) 0.0214(15) Uani 1 1 d . . . . .
H005 H 0.471867 0.396167 0.639270 0.026 Uiso 1 1 calc R . . . .
C006 C 0.5084(6) 0.2974(11) 0.9163(6) 0.0259(16) Uani 1 1 d . . . . .
H006 H 0.516745 0.273946 0.986948 0.031 Uiso 1 1 calc R . . . .
C007 C 0.5713(5) 0.3528(10) 0.7491(7) 0.0202(13) Uani 1 1 d . . . . .
C008 C 0.4188(6) 0.3147(13) 0.8762(7) 0.0233(16) Uani 1 1 d . . . . .
H008 H 0.366543 0.301264 0.919710 0.028 Uiso 1 1 calc R . . . .
C009 C 0.5847(6) 0.3144(14) 0.8531(7) 0.0233(16) Uani 1 1 d . . . . .
H009 H 0.645530 0.300350 0.879599 0.028 Uiso 1 1 calc R . . . .
C00A C 0.7479(6) 0.1038(12) 0.4690(8) 0.0256(18) Uani 1 1 d . . . . .
H00A H 0.686268 0.080468 0.497533 0.038 Uiso 1 1 calc GR . . . .
H00B H 0.795479 0.072751 0.519136 0.038 Uiso 1 1 calc GR . . . .
H00C H 0.756595 0.035132 0.406800 0.038 Uiso 1 1 calc GR . . . .
C00B C 0.4057(6) 0.3511(12) 0.7738(6) 0.0219(16) Uani 1 1 d . . . . .
H00D H 0.344571 0.362646 0.747431 0.026 Uiso 1 1 calc R . . . .
C00C C 0.6545(5) 0.3726(11) 0.6876(7) 0.0207(15) Uani 1 1 d . . . . .
H00E H 0.711648 0.373024 0.723685 0.025 Uiso 1 1 calc R . . . .
N00D N 0.6598(4) 0.3894(9) 0.5913(5) 0.0188(12) Uani 1 1 d . . . . .
H00F H 0.608047 0.386948 0.555718 0.023 Uiso 1 1 calc R . . . .
C00E C 0.7474(5) 0.4125(11) 0.5362(7) 0.0171(14) Uani 1 1 d . . . . .
H00G H 0.799641 0.388647 0.583280 0.021 Uiso 1 1 calc R . . . .
H00H H 0.752509 0.534356 0.513892 0.021 Uiso 1 1 calc R . . . .
C00F C 0.7560(5) 0.2954(10) 0.4431(6) 0.0173(13) Uani 1 1 d . . . . .
H00I H 0.816681 0.316307 0.409960 0.021 Uiso 1 1 calc R . . . .
H00J H 0.706863 0.326078 0.393452 0.021 Uiso 1 1 calc R . . . .

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 0.01411(8) 0.01267(8) 0.01585(9) -0.00046(9) 0.00003(10) -0.00051(7)
Br02 0.0157(3) 0.0234(3) 0.0134(3) -0.0004(2) -0.0005(2) -0.0026(3)
Br03 0.0143(3) 0.0200(3) 0.0187(3) 0.0001(3) 0.0027(3) 0.0006(2)
Br04 0.0137(3) 0.0176(3) 0.0177(3) -0.0015(3) -0.0021(2) 0.0008(2)
C005 0.022(3) 0.027(4) 0.015(3) -0.001(3) -0.003(3) 0.002(3)
C006 0.031(4) 0.033(4) 0.014(3) -0.001(3) -0.005(3) 0.000(4)
C007 0.019(3) 0.026(3) 0.015(3) -0.004(4) 0.003(3) 0.000(2)
C008 0.026(4) 0.024(4) 0.020(4) -0.004(3) 0.007(3) -0.002(3)
C009 0.020(3) 0.031(4) 0.019(4) -0.003(4) -0.002(3) 0.002(3)
C00A 0.028(4) 0.018(4) 0.031(5) 0.000(4) 0.002(4) -0.001(3)
C00B 0.019(3) 0.032(4) 0.015(3) -0.001(3) 0.001(3) 0.002(3)
C00C 0.016(3) 0.025(4) 0.021(4) -0.002(3) 0.000(3) -0.002(3)
N00D 0.017(3) 0.023(3) 0.016(3) 0.000(2) 0.000(2) 0.001(2)
C00E 0.013(3) 0.019(4) 0.019(4) -0.001(3) 0.003(2) -0.001(2)
C00F 0.018(3) 0.021(3) 0.013(3) 0.000(3) 0.001(2) 0.000(3)

_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 Br02 2.9208(8) . ?
Pb01 Br02 3.1665(8) 4_655 ?
Pb01 Br03 3.0813(8) 4_645 ?
Pb01 Br03 2.9598(8) . ?
Pb01 Br04 2.9471(8) . ?
Pb01 Br04 3.0915(8) 4_645 ?
C005 C007 1.408(10) . ?
C005 C00B 1.381(11) . ?
C006 C008 1.400(12) . ?
C006 C009 1.382(12) . ?
C007 C009 1.406(12) . ?
C007 C00C 1.452(11) . ?
C008 C00B 1.383(12) . ?
C00A C00F 1.525(12) . ?
C00C N00D 1.269(11) . ?
N00D C00E 1.466(9) . ?
C00E C00F 1.524(12) . ?

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
Br02 Pb01 Br02 171.19(2) . 4_655 ?
Br02 Pb01 Br03 93.72(2) . . ?
Br02 Pb01 Br03 84.47(2) . 4_645 ?
Br02 Pb01 Br04 89.89(2) . . ?
Br02 Pb01 Br04 83.74(2) . 4_645 ?
Br03 Pb01 Br02 99.08(2) 4_645 4_655 ?
Br03 Pb01 Br02 82.35(2) . 4_655 ?
Br03 Pb01 Br03 176.837(11) . 4_645 ?
Br03 Pb01 Br04 100.52(2) . 4_645 ?
Br03 Pb01 Br04 81.89(2) 4_645 4_645 ?
Br04 Pb01 Br02 82.02(2) . 4_655 ?
Br04 Pb01 Br02 104.69(2) 4_645 4_655 ?
Br04 Pb01 Br03 86.45(2) . . ?
Br04 Pb01 Br03 90.95(2) . 4_645 ?
Br04 Pb01 Br04 170.82(2) . 4_645 ?
Pb01 Br02 Pb01 78.981(18) . 4_645 ?
Pb01 Br03 Pb01 79.790(17) . 4_655 ?
Pb01 Br04 Pb01 79.816(18) . 4_655 ?
C00B C005 C007 119.5(8) . . ?
C009 C006 C008 120.0(8) . . ?
C005 C007 C00C 123.3(8) . . ?
C009 C007 C005 120.2(7) . . ?
C009 C007 C00C 116.5(7) . . ?
C00B C008 C006 120.6(8) . . ?
C006 C009 C007 119.4(7) . . ?
C005 C00B C008 120.3(8) . . ?
N00D C00C C007 127.7(8) . . ?
C00C N00D C00E 123.6(7) . . ?
N00D C00E C00F 113.0(6) . . ?
C00E C00F C00A 113.3(7) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.509(14)
2 0.491(14)

