# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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_r-1
_database_code_depnum_ccdc_archive 'CCDC 2121694'
loop_
_audit_author_name
_audit_author_address
'Xi-Ming Luo'
;Zhengzhou University
China
;
_audit_update_record             
;
2021-11-12 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_audit_creation_date             2021-11-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H8 N)'
_chemical_formula_sum            'C6 H16 Br4 N2 Pb'
_chemical_formula_weight         643.04
_chemical_absolute_configuration R
_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           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.8337(5)
_cell_length_b                   11.7412(5)
_cell_length_c                   9.9636(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1384.36(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3725
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      29.3170
_cell_measurement_theta_min      2.7250
_shelx_estimated_absorpt_T_max   0.200
_shelx_estimated_absorpt_T_min   0.163
_exptl_absorpt_coefficient_mu    23.698
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.085
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9065
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.341
_diffrn_reflns_theta_min         3.187
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     26.00  72.00   0.50    1.00    --    3.80  57.00  90.00   92
  2  ω    -86.00  32.00   0.50    1.00    --    3.80 -38.00 -30.00  236
  3  ω    -57.00 -28.00   0.50    1.00    --    3.80 -57.00  60.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0090222000
_diffrn_orient_matrix_UB_12      -0.0069446000
_diffrn_orient_matrix_UB_13      -0.0698985000
_diffrn_orient_matrix_UB_21      0.0097912000
_diffrn_orient_matrix_UB_22      0.0593411000
_diffrn_orient_matrix_UB_23      -0.0063794000
_diffrn_orient_matrix_UB_31      0.0584440000
_diffrn_orient_matrix_UB_32      -0.0089281000
_diffrn_orient_matrix_UB_33      0.0118853000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.636
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.749
_reflns_number_gt                2870
_reflns_number_total             3147
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details 
;
 Flack x determined using 1032 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(9)
_refine_ls_extinction_coef       0.00232(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         3147
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0219
_refine_ls_restrained_S_all      1.011
_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)+(0.0103P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0405
_refine_ls_wR_factor_ref         0.0414
_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,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E)
;
_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
Pb1 Pb 0.74760(2) 0.72692(2) 0.49406(2) 0.01328(7) Uani 1 1 d . . . . .
Br1 Br 0.74441(7) 0.71355(5) 0.79159(5) 0.01713(14) Uani 1 1 d . . . . .
Br4 Br 0.50445(5) 0.68109(5) 0.49447(6) 0.02506(15) Uani 1 1 d . . . . .
Br2 Br 0.81987(5) 0.48170(4) 0.47737(6) 0.02000(14) Uani 1 1 d . . . . .
Br3 Br 0.74813(7) 0.70682(5) 0.19650(5) 0.01723(14) Uani 1 1 d . . . . .
C3 C 0.9608(6) 0.4488(6) -0.1437(7) 0.0226(18) Uani 1 1 d . . . . .
H3A H 0.975312 0.402578 -0.222466 0.027 Uiso 1 1 calc R . . . .
H3B H 0.882939 0.474452 -0.147377 0.027 Uiso 1 1 calc R . . . .
C2 C 0.9789(5) 0.3775(4) -0.0175(6) 0.0170(12) Uani 1 1 d . . . . .
H2A H 0.926205 0.314202 -0.017477 0.020 Uiso 1 1 calc R . . . .
H2B H 1.054866 0.346584 -0.018041 0.020 Uiso 1 1 calc R . . . .
C5 C 0.6154(5) 0.4558(4) -0.0114(6) 0.0174(12) Uani 1 1 d . . . . .
H5A H 0.667399 0.391929 -0.011014 0.021 Uiso 1 1 calc R . . . .
H5B H 0.659663 0.525353 -0.010450 0.021 Uiso 1 1 calc R . . . .
C6 C 0.5436(6) 0.4520(6) -0.1402(7) 0.0201(17) Uani 1 1 d . . . . .
H6A H 0.592381 0.459502 -0.217983 0.024 Uiso 1 1 calc R . . . .
H6B H 0.505246 0.379134 -0.146124 0.024 Uiso 1 1 calc R . . . .
C1 C 0.9618(5) 0.4479(5) 0.1088(6) 0.0129(15) Uani 1 1 d . . . . .
H1 H 0.883068 0.473689 0.111481 0.016 Uiso 1 1 calc R . . . .
N1 N 0.9833(5) 0.3730(4) 0.2296(5) 0.0188(12) Uani 1 1 d . . . . .
H1A H 1.052746 0.344249 0.224877 0.023 Uiso 1 1 calc GR . . . .
H1B H 0.933182 0.316407 0.230822 0.023 Uiso 1 1 calc GR . . . .
H1C H 0.976449 0.414111 0.304175 0.023 Uiso 1 1 calc GR . . . .
C4 C 0.5425(5) 0.4511(5) 0.1126(6) 0.0124(15) Uani 1 1 d . . . . .
H4 H 0.501157 0.378793 0.113437 0.015 Uiso 1 1 calc R . . . .
N2 N 0.6180(4) 0.4558(4) 0.2330(5) 0.0172(12) Uani 1 1 d . . . . .
H2C H 0.670070 0.401379 0.226974 0.021 Uiso 1 1 calc GR . . . .
H2D H 0.577099 0.445420 0.306919 0.021 Uiso 1 1 calc GR . . . .
H2E H 0.651751 0.523507 0.236571 0.021 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.9688(6) . ?
Pb1 Br4 2.9273(6) . ?
Pb1 Br4 3.2276(6) 4_566 ?
Pb1 Br2 3.0081(5) . ?
Pb1 Br2 3.1092(6) 3_656 ?
Pb1 Br3 2.9742(6) . ?
C3 C3 1.518(13) 2_765 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.525(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.519(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.540(8) . ?
C5 C4 1.509(8) . ?
C6 C6 1.529(13) 2_665 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C1 C1 1.521(12) 2_765 ?
C1 H1 0.9800 . ?
C1 N1 1.513(8) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C4 C4 1.525(12) 2_665 ?
C4 H4 0.9800 . ?
C4 N2 1.496(8) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?

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 Br4 89.67(2) . 4_566 ?
Br1 Pb1 Br2 90.470(17) . . ?
Br1 Pb1 Br2 87.490(17) . 3_656 ?
Br1 Pb1 Br3 172.395(15) . . ?
Br4 Pb1 Br1 88.65(2) . . ?
Br4 Pb1 Br4 170.786(8) . 4_566 ?
Br4 Pb1 Br2 85.658(17) . 3_656 ?
Br4 Pb1 Br2 95.946(17) . . ?
Br4 Pb1 Br3 89.36(2) . . ?
Br2 Pb1 Br4 93.126(16) . 4_566 ?
Br2 Pb1 Br4 85.218(16) 3_656 4_566 ?
Br2 Pb1 Br2 177.377(8) . 3_656 ?
Br3 Pb1 Br4 93.43(2) . 4_566 ?
Br3 Pb1 Br2 99.678(17) . 3_656 ?
Br3 Pb1 Br2 82.436(17) . . ?
Pb1 Br4 Pb1 149.79(2) . 4_466 ?
Pb1 Br2 Pb1 147.44(2) . 3_646 ?
C3 C3 H3A 109.6 2_765 . ?
C3 C3 H3B 109.6 2_765 . ?
C3 C3 C2 110.4(4) 2_765 . ?
H3A C3 H3B 108.1 . . ?
C2 C3 H3A 109.6 . . ?
C2 C3 H3B 109.6 . . ?
C3 C2 H2A 109.3 . . ?
C3 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
C1 C2 C3 111.4(4) . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C4 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C4 C5 C6 111.5(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C6 C6 C5 110.6(4) 2_665 . ?
C6 C6 H6A 109.5 2_665 . ?
C6 C6 H6B 109.5 2_665 . ?
H6A C6 H6B 108.1 . . ?
C2 C1 C1 111.0(4) . 2_765 ?
C2 C1 H1 108.5 . . ?
C1 C1 H1 108.5 2_765 . ?
N1 C1 C2 108.7(5) . . ?
N1 C1 C1 111.6(4) . 2_765 ?
N1 C1 H1 108.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C5 C4 C4 110.5(4) . 2_665 ?
C5 C4 H4 108.9 . . ?
C4 C4 H4 108.9 2_665 . ?
N2 C4 C5 108.3(5) . . ?
N2 C4 C4 111.5(4) . 2_665 ?
N2 C4 H4 108.9 . . ?
C4 N2 H2C 109.5 . . ?
C4 N2 H2D 109.5 . . ?
C4 N2 H2E 109.5 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 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 C1 56.9(8) 2_765 . . . ?
C3 C2 C1 C1 -55.7(7) . . . 2_765 ?
C3 C2 C1 N1 -178.9(5) . . . . ?
C6 C5 C4 C4 -57.4(6) . . . 2_665 ?
C6 C5 C4 N2 -179.7(5) . . . . ?
C4 C5 C6 C6 56.0(7) . . . 2_665 ?

_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 1.873
_oxdiff_exptl_absorpt_empirical_full_min 0.611
####################################################################### 
# 
# 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_s-1
_database_code_depnum_ccdc_archive 'CCDC 2121695'
loop_
_audit_author_name
_audit_author_address
'Xi-Ming Luo'
;Zhengzhou University
China
;
_audit_update_record             
;
2021-11-12 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_audit_creation_date             2021-11-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H8 N)'
_chemical_formula_sum            'C6 H16 Br4 N2 Pb'
_chemical_formula_weight         643.04
_chemical_absolute_configuration S
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     ' '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 '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           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.87800(10)
_cell_length_b                   11.78320(10)
_cell_length_c                   9.97810(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1396.54(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11948
_cell_measurement_temperature    272.0(10)
_cell_measurement_theta_max      73.3620
_cell_measurement_theta_min      3.7330
_shelx_estimated_absorpt_T_max   0.121
_shelx_estimated_absorpt_T_min   0.096
_exptl_absorpt_coefficient_mu    36.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.058
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            12911
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.478
_diffrn_reflns_theta_max         66.478
_diffrn_reflns_theta_min         4.431
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      272.0(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -28.00  54.00   0.50    0.50    --    0.00  57.00   0.00  164
  2  ω    -27.00  89.00   0.50    0.50    --    0.00  57.00 -90.00  232
  3  ω     55.00  87.00   0.50    0.50    --    0.00  38.00-150.00   64
  4  ω    -12.00  14.00   0.50    0.50    --    0.00  57.00-180.00   52
  5  ω    -25.00  45.00   0.50    0.50    --    0.00  38.00-150.00  140
  6  ω     38.00  71.00   0.50    0.50    --   98.80  15.00-150.00   66
  7  ω     37.00  77.00   0.50    0.50    --   98.80 -82.00-150.00   80
  8  ω     93.00 131.00   0.50    0.50    --   98.80 -82.00  60.00   76
  9  ω      9.00  86.00   0.50    0.50    --   98.80 -15.00-180.00  154
 10  ω      9.00  35.00   0.50    0.50    --   98.80 -30.00 120.00   52
 11  ω     59.00 136.00   0.50    0.50    --   98.80 -82.00-180.00  154
 12  ω     81.00 129.00   0.50    0.50    --   98.80 -82.00-150.00   96
 13  ω     25.00  51.00   0.50    0.50    --   98.80 -30.00-120.00   52
 14  ω     69.00 131.00   0.50    0.50    --   98.80 -30.00-120.00  124
 15  ω     84.00 133.00   0.50    0.50    --   98.80 -82.00 -90.00   98
 16  ω     68.00 100.00   0.50    0.50    --   98.80 -82.00 -30.00   64
 17  ω     10.00  44.00   0.50    0.50    --   98.80 -82.00 -30.00   68
 18  ω    156.00 188.00   0.50    0.50    --   98.80  15.00-150.00   64
 19  ω     18.00 129.00   0.50    0.50    --   98.80 -61.00  60.00  222
 20  ω     40.00 109.00   0.50    0.50    --   98.80 -30.00 120.00  138
 21  ω     89.00 142.00   0.50    0.50    --   98.80  15.00-150.00  106
 22  ω     98.00 156.00   0.50    0.50    --   98.80 -15.00-180.00  116
 23  ω     12.00  66.00   0.50    0.50    --   98.80 -82.00 -90.00  108
 24  ω     10.00  41.00   0.50    0.50    --   98.80 -82.00 120.00   62
 25  ω     76.00 102.00   0.50    0.50    --   98.80 -82.00 120.00   52
 26  ω     44.00  74.00   0.50    0.50    --   98.80 -82.00  60.00   60
 27  ω     17.00 112.00   0.50    0.50    --   98.80 -82.00  30.00  190
 28  ω     79.00 124.00   0.50    0.50    --   98.80  77.00  90.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0616223000
_diffrn_orient_matrix_UB_12      0.1124419000
_diffrn_orient_matrix_UB_13      -0.0286781000
_diffrn_orient_matrix_UB_21      -0.1032917000
_diffrn_orient_matrix_UB_22      -0.0667219000
_diffrn_orient_matrix_UB_23      -0.0500145000
_diffrn_orient_matrix_UB_31      -0.0484676000
_diffrn_orient_matrix_UB_32      -0.0007944000
_diffrn_orient_matrix_UB_33      0.1432472000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.719
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2445
_reflns_number_total             2460
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.614
_refine_diff_density_min         -3.877
_refine_diff_density_rms         0.344
_refine_ls_abs_structure_details 
;
 Flack x determined using 996 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(6)
_refine_ls_extinction_coef       0.00252(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2460
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0375
_refine_ls_restrained_S_all      1.085
_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)+(0.0708P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0922
_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,H,H) groups
2. Rigid bond restraints
 N2, C4, C5, C6
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B)
4.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E)
;
_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
Pb1 Pb 0.74726(2) 0.72702(3) 0.50600(3) 0.0139(2) Uani 1 1 d . . . . .
Br1 Br 0.81935(8) 0.48171(7) 0.52264(11) 0.0240(3) Uani 1 1 d . . . . .
Br2 Br 0.74844(9) 0.70617(9) 0.80366(10) 0.0197(3) Uani 1 1 d . . . . .
Br3 Br 0.74428(8) 0.71465(8) 0.20891(10) 0.0192(3) Uani 1 1 d . . . . .
Br4 Br 0.50428(7) 0.68189(9) 0.50635(9) 0.0312(3) Uani 1 1 d . . . . .
N1 N 0.9835(7) 0.3730(6) 0.7716(6) 0.0186(15) Uani 1 1 d . . . . .
H1A H 0.976098 0.413713 0.697024 0.022 Uiso 1 1 calc GR . . . .
H1B H 0.934312 0.316022 0.770729 0.022 Uiso 1 1 calc GR . . . .
H1C H 1.053074 0.345316 0.776366 0.022 Uiso 1 1 calc GR . . . .
C1 C 0.9615(7) 0.4472(7) 0.8912(9) 0.0124(19) Uani 1 1 d . . . . .
H1 H 0.882941 0.472655 0.888018 0.015 Uiso 1 1 calc R . . . .
C2 C 0.9784(8) 0.3778(7) 1.0171(8) 0.0215(18) Uani 1 1 d . . . . .
H2A H 1.054035 0.346781 1.017479 0.026 Uiso 1 1 calc R . . . .
H2B H 0.925816 0.314827 1.017353 0.026 Uiso 1 1 calc R . . . .
C3 C 0.9610(8) 0.4485(9) 1.1428(9) 0.025(3) Uani 1 1 d . U . . .
H3A H 0.975934 0.402382 1.221344 0.030 Uiso 1 1 calc R . . . .
H3B H 0.883316 0.473762 1.147145 0.030 Uiso 1 1 calc R . . . .
N2 N 0.6180(6) 0.4566(7) 0.7665(7) 0.0192(15) Uani 1 1 d . U . . .
H2C H 0.578095 0.444065 0.692448 0.023 Uiso 1 1 calc GR . . . .
H2D H 0.671644 0.404168 0.773654 0.023 Uiso 1 1 calc GR . . . .
H2E H 0.649437 0.525067 0.762113 0.023 Uiso 1 1 calc GR . . . .
C4 C 0.5417(6) 0.4506(7) 0.8869(8) 0.0106(18) Uani 1 1 d . U . . .
H4 H 0.500092 0.378792 0.885279 0.013 Uiso 1 1 calc R . . . .
C5 C 0.6144(7) 0.4550(8) 1.0120(8) 0.0211(17) Uani 1 1 d . U . . .
H5A H 0.659297 0.523765 1.010582 0.025 Uiso 1 1 calc R . . . .
H5B H 0.665426 0.390776 1.012120 0.025 Uiso 1 1 calc R . . . .
C6 C 0.5430(8) 0.4528(9) 1.1404(9) 0.023(2) Uani 1 1 d . U . . .
H6A H 0.504802 0.380238 1.147312 0.028 Uiso 1 1 calc R . . . .
H6B H 0.591837 0.460775 1.217800 0.028 Uiso 1 1 calc R . . . .


_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 3.0192(8) . ?
Pb1 Br1 3.1169(9) 3_656 ?
Pb1 Br2 2.9803(10) . ?
Pb1 Br3 2.9681(10) . ?
Pb1 Br4 2.9347(9) . ?
Pb1 Br4 3.2384(10) 4_566 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.502(10) . ?
C1 C1 1.544(16) 2_765 ?
C1 H1 0.9800 . ?
C1 C2 1.513(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.520(12) . ?
C3 C3 1.53(2) 2_765 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N2 C4 1.507(10) . ?
C4 C4 1.529(16) 2_665 ?
C4 H4 0.9800 . ?
C4 C5 1.518(10) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.537(11) . ?
C6 C6 1.511(19) 2_665 ?
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 177.275(12) . 3_656 ?
Br1 Pb1 Br4 92.98(3) . 4_566 ?
Br1 Pb1 Br4 85.22(3) 3_656 4_566 ?
Br2 Pb1 Br1 99.90(3) . 3_656 ?
Br2 Pb1 Br1 82.24(3) . . ?
Br2 Pb1 Br4 93.49(3) . 4_566 ?
Br3 Pb1 Br1 90.65(3) . . ?
Br3 Pb1 Br1 87.29(3) . 3_656 ?
Br3 Pb1 Br2 172.45(4) . . ?
Br3 Pb1 Br4 89.40(3) . 4_566 ?
Br4 Pb1 Br1 96.05(3) . . ?
Br4 Pb1 Br1 85.69(3) . 3_656 ?
Br4 Pb1 Br2 89.34(3) . . ?
Br4 Pb1 Br3 88.89(3) . . ?
Br4 Pb1 Br4 170.824(14) . 4_566 ?
Pb1 Br1 Pb1 147.65(4) . 3_646 ?
Pb1 Br4 Pb1 150.11(4) . 4_466 ?
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 C1 111.4(5) . 2_765 ?
N1 C1 H1 108.6 . . ?
N1 C1 C2 108.8(7) . . ?
C1 C1 H1 108.6 2_765 . ?
C2 C1 C1 110.9(6) . 2_765 ?
C2 C1 H1 108.6 . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
C1 C2 C3 111.8(7) . . ?
H2A C2 H2B 107.9 . . ?
C3 C2 H2A 109.3 . . ?
C3 C2 H2B 109.3 . . ?
C2 C3 C3 110.7(6) . 2_765 ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C3 C3 H3A 109.5 2_765 . ?
C3 C3 H3B 109.5 2_765 . ?
H3A C3 H3B 108.1 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
C4 N2 H2C 109.5 . . ?
C4 N2 H2D 109.5 . . ?
C4 N2 H2E 109.5 . . ?
N2 C4 C4 110.7(6) . 2_665 ?
N2 C4 H4 109.3 . . ?
N2 C4 C5 108.2(6) . . ?
C4 C4 H4 109.3 2_665 . ?
C5 C4 C4 110.0(6) . 2_665 ?
C5 C4 H4 109.3 . . ?
C4 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C4 C5 C6 111.8(7) . . ?
H5A C5 H5B 107.9 . . ?
C6 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C5 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
C6 C6 C5 111.1(7) 2_665 . ?
C6 C6 H6A 109.4 2_665 . ?
C6 C6 H6B 109.4 2_665 . ?
H6A C6 H6B 108.0 . . ?

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 C1 C2 C3 178.3(7) . . . . ?
C1 C1 C2 C3 55.4(11) 2_765 . . . ?
C1 C2 C3 C3 -56.5(12) . . . 2_765 ?
N2 C4 C5 C6 178.4(8) . . . . ?
C4 C4 C5 C6 57.3(10) 2_665 . . . ?
C4 C5 C6 C6 -55.3(12) . . . 2_665 ?

_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 5.628
_oxdiff_exptl_absorpt_empirical_full_min 0.677
