# 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_(TEMA)PbBr3_295K
_database_code_depnum_ccdc_archive 'CCDC 2329832'
loop_
_audit_author_name
_audit_author_address
'Zhi-Jie Wang'
;southeast university
China
;
_audit_update_record             
;
2024-01-30 deposited with the CCDC.	2024-03-11 downloaded from the CCDC.
;
_audit_creation_date             2023-10-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, 0.5(C14 H36 N2)'
_chemical_formula_sum            'C7 H18 Br3 N Pb'
_chemical_formula_weight         563.14
_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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   10.2305(10)
_cell_length_b                   10.2305(10)
_cell_length_c                   7.8573(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     712.19(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    679
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      20.4520
_cell_measurement_theta_min      2.3110
_shelx_estimated_absorpt_T_max   0.498
_shelx_estimated_absorpt_T_min   0.107
_exptl_absorpt_coefficient_mu    20.222
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.626
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3342
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.730
_diffrn_reflns_theta_min         2.299
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  15.00   0.50    2.00    --    4.87 -11.00 -53.00   80
  2  ω    -66.00 -40.00   0.50    2.00    --    4.87 -11.00 -53.00   52
  3  ω    -14.00  35.00   0.50    2.00    --    4.87 -99.00 -30.00   98
  4  ω    -17.00  12.00   0.50    2.00    --   -5.57 -99.00-150.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0697557000
_diffrn_orient_matrix_UB_12      0.0678111000
_diffrn_orient_matrix_UB_13      -0.0115715000
_diffrn_orient_matrix_UB_21      -0.0388769000
_diffrn_orient_matrix_UB_22      0.0409456000
_diffrn_orient_matrix_UB_23      -0.0065713000
_diffrn_orient_matrix_UB_31      0.0061538000
_diffrn_orient_matrix_UB_32      0.0116878000
_diffrn_orient_matrix_UB_33      0.0892622000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                220
_reflns_number_total             398
_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 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.013(3)
_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   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         398
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.1607
_refine_ls_R_factor_gt           0.0818
_refine_ls_restrained_S_all      0.849
_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)+(0.0758P)²+9.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.2101
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5-C2 = C6-C3 = C7-C4
 1.54 with sigma of 0.01
 N1-C1 = N1-C2 = N1-C3 = N1-C4
 1.5 with sigma of 0.01
 C5-N1 = C6-N1 = C7-N1
 2.483 with sigma of 0.001
 N1-C2 \\sim N1-C3 \\sim N1-C4 \\sim N1-C1
 with sigma of 0.02
 C3-C2 \\sim C4-C2 \\sim C1-C2 \\sim C1-C4 \\sim C1-C3 \\sim C4-C3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) = Uanis(N1) = Uanis(C2) = Uanis(C3) = Uanis(C1) = Uanis(C5) =
Uanis(C6) = Uanis(C7)
4. Rigid body (RIGU) restrains
 C4, N1, C2, C3, C1, C5, C6, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: N1(0.083333) C2(0.083333) H2A(0.083333) H2B(0.083333) C5(0.083333)
 H5A(0.083333) H5B(0.083333) H5C(0.083333) C3(0.083333) H3A(0.083333)
 H3B(0.083333) C6(0.083333) H6A(0.083333) H6B(0.083333) H6C(0.083333)
 C4(0.083333) H4A(0.083333) H4B(0.083333) C7(0.083333) H7A(0.083333)
 H7B(0.083333) H7C(0.083333) C1(0.083333) H1A(0.083333) H1B(0.083333)
 H1C(0.083333)
6.a Riding coordinates:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C1(H1A,H1B,H1C)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
;
_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 1.000000 1.000000 0.500000 0.1226(15) Uani 1 12 d S T P . .
Br1 Br 0.7404(5) 0.8702(2) 0.750000 0.188(2) Uani 1 4 d S T P . .
N1 N 0.342(4) 0.683(4) 0.262(3) 0.141(17) Uani 0.0833 1 d D U P A -1
C2 C 0.385(11) 0.595(10) 0.379(5) 0.141(17) Uani 0.0833 1 d D U P A -1
H2A H 0.490464 0.626182 0.362268 0.169 Uiso 0.0833 1 calc R U P A -1
H2B H 0.325032 0.488466 0.352711 0.169 Uiso 0.0833 1 calc R U P A -1
C5 C 0.358(14) 0.623(11) 0.565(3) 0.141(17) Uani 0.0833 1 d D U P A -1
H5A H 0.445326 0.716956 0.596488 0.211 Uiso 0.0833 1 d R U P A -1
H5B H 0.348296 0.544556 0.639088 0.211 Uiso 0.0833 1 d R U P A -1
H5C H 0.269596 0.632936 0.573728 0.211 Uiso 0.0833 1 d R U P A -1
C3 C 0.257(5) 0.587(9) 0.113(5) 0.141(17) Uani 0.0833 1 d D U P A -1
H3A H 0.290762 0.515598 0.088591 0.169 Uiso 0.0833 1 calc R U P A -1
H3B H 0.275508 0.649536 0.012740 0.169 Uiso 0.0833 1 calc R U P A -1
C6 C 0.086(4) 0.501(11) 0.153(9) 0.141(17) Uani 0.0833 1 d D U P A -1
H6A H 0.066115 0.414944 0.221744 0.211 Uiso 0.0833 1 d R U P A -1
H6B H 0.035465 0.466604 0.045684 0.211 Uiso 0.0833 1 d R U P A -1
H6C H 0.050725 0.559634 0.210434 0.211 Uiso 0.0833 1 d R U P A -1
C4 C 0.481(7) 0.822(7) 0.202(8) 0.141(17) Uani 0.0833 1 d D U P A -1
H4A H 0.563691 0.801576 0.193557 0.169 Uiso 0.0833 1 calc R U P A -1
H4B H 0.508824 0.903228 0.282625 0.169 Uiso 0.0833 1 calc R U P A -1
C7 C 0.451(17) 0.869(5) 0.026(5) 0.141(17) Uani 0.0833 1 d D U P A -1
H7A H 0.523174 0.974451 0.014249 0.211 Uiso 0.0833 1 d R U P A -1
H7B H 0.351324 0.855131 0.033379 0.211 Uiso 0.0833 1 d R U P A -1
H7C H 0.457424 0.815121 -0.070611 0.211 Uiso 0.0833 1 d R U P A -1
C1 C 0.242(9) 0.729(10) 0.355(7) 0.141(17) Uani 0.0833 1 d D U P A -1
H1A H 0.159086 0.703776 0.280319 0.211 Uiso 0.0833 1 d R U P A -1
H1B H 0.291616 0.833986 0.382999 0.211 Uiso 0.0833 1 d R U P A -1
H1C H 0.206146 0.669926 0.457549 0.211 Uiso 0.0833 1 d R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.025(3) 14_566 ?
Pb1 Br1 3.025(3) 15_656 ?
Pb1 Br1 3.025(3) 13_776 ?
Pb1 Br1 3.025(3) . ?
Pb1 Br1 3.025(3) 3_675 ?
Pb1 Br1 3.025(3) 2_765 ?
N1 C2 1.499(9) . ?
N1 C3 1.500(9) . ?
N1 C4 1.498(9) . ?
N1 C1 1.500(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C5 1.541(10) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9601 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C6 1.542(10) . ?
C6 H6A 0.9599 . ?
C6 H6B 0.9599 . ?
C6 H6C 0.9599 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C7 1.540(10) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9601 . ?
C7 H7C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9599 . ?
C1 H1C 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
Br1 Pb1 Br1 180.0 14_566 2_765 ?
Br1 Pb1 Br1 82.38(8) 3_675 . ?
Br1 Pb1 Br1 97.62(8) 3_675 13_776 ?
Br1 Pb1 Br1 97.62(8) 15_656 . ?
Br1 Pb1 Br1 97.62(8) 2_765 13_776 ?
Br1 Pb1 Br1 82.38(8) 15_656 13_776 ?
Br1 Pb1 Br1 180.0 . 13_776 ?
Br1 Pb1 Br1 82.38(8) 14_566 15_656 ?
Br1 Pb1 Br1 82.38(8) 2_765 3_675 ?
Br1 Pb1 Br1 82.38(8) 14_566 13_776 ?
Br1 Pb1 Br1 180.00(14) 15_656 3_675 ?
Br1 Pb1 Br1 97.62(8) 2_765 15_656 ?
Br1 Pb1 Br1 97.62(8) 14_566 . ?
Br1 Pb1 Br1 82.38(8) 2_765 . ?
Br1 Pb1 Br1 97.62(8) 14_566 3_675 ?
Pb1 Br1 Pb1 80.99(11) 4_775 . ?
C2 N1 C3 109.3(10) . . ?
C2 N1 C1 109.6(10) . . ?
C4 N1 C2 109.5(10) . . ?
C4 N1 C3 109.8(10) . . ?
C4 N1 C1 109.4(10) . . ?
C1 N1 C3 109.1(10) . . ?
N1 C2 H2A 109.8 . . ?
N1 C2 H2B 109.8 . . ?
N1 C2 C5 109.5(7) . . ?
H2A C2 H2B 108.2 . . ?
C5 C2 H2A 109.8 . . ?
C5 C2 H2B 109.8 . . ?
C2 C5 H5A 105.6 . . ?
C2 C5 H5B 112.0 . . ?
C2 C5 H5C 110.8 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C3 H3A 109.8 . . ?
N1 C3 H3B 109.8 . . ?
N1 C3 C6 109.4(7) . . ?
H3A C3 H3B 108.2 . . ?
C6 C3 H3A 109.8 . . ?
C6 C3 H3B 109.8 . . ?
C3 C6 H6A 107.7 . . ?
C3 C6 H6B 106.2 . . ?
C3 C6 H6C 114.4 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C4 H4A 109.7 . . ?
N1 C4 H4B 109.7 . . ?
N1 C4 C7 109.6(7) . . ?
H4A C4 H4B 108.2 . . ?
C7 C4 H4A 109.7 . . ?
C7 C4 H4B 109.7 . . ?
C4 C7 H7A 106.2 . . ?
C4 C7 H7B 105.3 . . ?
C4 C7 H7C 116.7 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C1 H1A 105.5 . . ?
N1 C1 H1B 113.7 . . ?
N1 C1 H1C 109.0 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 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
C2 N1 C3 C6 91(8) . . . . ?
C2 N1 C4 C7 152(7) . . . . ?
C3 N1 C2 C5 -138(7) . . . . ?
C3 N1 C4 C7 32(7) . . . . ?
C4 N1 C2 C5 102(7) . . . . ?
C4 N1 C3 C6 -149(8) . . . . ?
C1 N1 C2 C5 -18(7) . . . . ?
C1 N1 C3 C6 -29(8) . . . . ?
C1 N1 C4 C7 -87(7) . . . . ?

_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 2.076
_oxdiff_exptl_absorpt_empirical_full_min 0.562
####################################################################### 
# 
# 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 
# 
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# Please retain this information to preserve the provenance of 
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data_(TEMA)PbBr3_198K
_database_code_depnum_ccdc_archive 'CCDC 2329833'
loop_
_audit_author_name
_audit_author_address
'Zhi-Jie Wang'
;southeast university
China
;
_audit_update_record             
;
2024-01-30 deposited with the CCDC.	2024-03-11 downloaded from the CCDC.
;
_audit_creation_date             2024-01-30
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Br3 Pb), 2(C7 H18 N)'
_chemical_formula_sum            'C14 H36 Br6 N2 Pb2'
_chemical_formula_weight         1126.29
_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.4048(11)
_cell_length_b                   16.8153(9)
_cell_length_c                   7.9462(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.425(5)
_cell_angle_gamma                90
_cell_volume                     2724.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7979
_cell_measurement_temperature    198.00(10)
_cell_measurement_theta_max      29.9930
_cell_measurement_theta_min      2.0750
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.149
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.746
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod-shaped
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1115
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            30387
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.570
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      198.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  76.00   0.50    1.50    --    6.50  38.00 -30.00  160
  2  ω      4.00  72.00   0.50    1.50    --    6.50  38.00  60.00  136
  3  ω    -38.00 -11.00   0.50    1.50    --    6.50 -57.00 150.00   54
  4  ω    -18.00   8.00   0.50    1.50    --    6.50 -99.00  60.00   52
  5  ω    -82.00  10.00   0.50    1.50    --   -7.20 -19.00   0.00  184
  6  ω    -17.00  27.00   0.50    1.50    --   -7.20 -99.00-120.00   88
  7  ω    -24.00  64.00   0.50    1.50    --   -7.20  38.00-180.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0175346000
_diffrn_orient_matrix_UB_12      -0.0361635000
_diffrn_orient_matrix_UB_13      0.0112226000
_diffrn_orient_matrix_UB_21      -0.0300203000
_diffrn_orient_matrix_UB_22      -0.0208563000
_diffrn_orient_matrix_UB_23      0.0060313000
_diffrn_orient_matrix_UB_31      -0.0013178000
_diffrn_orient_matrix_UB_32      -0.0060647000
_diffrn_orient_matrix_UB_33      -0.0884253000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3489
_reflns_number_total             4755
_reflns_odcompleteness_completeness 99.97
_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 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         5.382
_refine_diff_density_min         -4.400
_refine_diff_density_rms         0.466
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         4755
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.0941
_refine_ls_restrained_S_all      1.190
_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)+(0.0825P)²+259.5694P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2293
_refine_ls_wR_factor_ref         0.2451
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C12
 1.5 with sigma of 0.01
 C4-C3
 1.5 with sigma of 0.01
 C13-C12 = C4-C3 = C6-C5 = C2-C1 = C11-C10 = C9-C8
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C13) = Uanis(C10) = Uanis(C14) = Uanis(C8) = Uanis(C9) =
Uanis(C12) = Uanis(C11)
Uanis(N2) = Uanis(C4) = Uanis(C3) = Uanis(C5) = Uanis(C7) = Uanis(C6) =
Uanis(C2) = Uanis(C1)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C9(H9A,H9B), C10(H10A,H10B), C13(H13A,
 H13B)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C)
;
_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
Br1 Br 0.45386(14) 0.66909(18) 0.3462(4) 0.0314(7) Uani 1 1 d . . . . .
Br2 Br 0.25950(14) 0.6943(2) 0.3231(4) 0.0354(7) Uani 1 1 d . . . . .
Br3 Br 0.37059(16) 0.88538(18) 0.3320(4) 0.0375(8) Uani 1 1 d . . . . .
Pb1 Pb 0.36223(5) 0.75011(7) 0.57398(12) 0.0236(3) Uani 1 1 d . . . . .
Br4 Br 0.03664(13) 0.19074(18) 0.3831(4) 0.0304(7) Uani 1 1 d . . . . .
Br5 Br 0.15419(14) 0.38535(17) 0.3874(3) 0.0283(7) Uani 1 1 d . . . . .
Br6 Br 0.22996(14) 0.16853(19) 0.4006(4) 0.0330(7) Uani 1 1 d . . . . .
Pb2 Pb 0.13963(5) 0.24919(7) 0.62871(12) 0.0226(3) Uani 1 1 d . . . . .
C1 C 0.9128(15) 0.3508(18) 0.526(3) 0.034(3) Uani 1 1 d D . . . .
H1A H 0.954450 0.379337 0.541101 0.051 Uiso 1 1 calc R U . . .
H1B H 0.916020 0.299271 0.583104 0.051 Uiso 1 1 calc R U . . .
H1C H 0.877582 0.382206 0.573134 0.051 Uiso 1 1 calc R U . . .
C2 C 0.8975(15) 0.3374(18) 0.336(3) 0.034(3) Uani 1 1 d D . . . .
H2A H 0.937821 0.319104 0.283383 0.041 Uiso 1 1 calc R U . . .
H2B H 0.864302 0.294672 0.322686 0.041 Uiso 1 1 calc R U . . .
C3 C 0.8646(15) 0.3887(15) 0.056(4) 0.034(3) Uani 1 1 d D . . . .
H3A H 0.906940 0.367413 0.019261 0.041 Uiso 1 1 calc R U . . .
H3B H 0.831335 0.346128 0.042040 0.041 Uiso 1 1 calc R U . . .
C4 C 0.8444(15) 0.4593(15) -0.054(4) 0.034(3) Uani 1 1 d D . . . .
H4A H 0.839655 0.442154 -0.171669 0.051 Uiso 1 1 calc R U . . .
H4B H 0.878041 0.500773 -0.043103 0.051 Uiso 1 1 calc R U . . .
H4C H 0.802487 0.480364 -0.017817 0.051 Uiso 1 1 calc R U . . .
C5 C 0.9881(11) 0.4666(18) 0.234(4) 0.034(3) Uani 1 1 d D . . . .
H5A H 0.989939 0.447123 0.117881 0.051 Uiso 1 1 calc R U . . .
H5B H 1.006324 0.426255 0.311607 0.051 Uiso 1 1 calc R U . . .
H5C H 1.013630 0.515698 0.246185 0.051 Uiso 1 1 calc R U . . .
C6 C 0.9163(11) 0.4832(18) 0.274(4) 0.034(3) Uani 1 1 d D . . . .
H6A H 0.914588 0.499331 0.393956 0.041 Uiso 1 1 calc R U . . .
H6B H 0.899853 0.528141 0.204298 0.041 Uiso 1 1 calc R U . . .
C7 C 0.8076(15) 0.4360(18) 0.302(4) 0.034(3) Uani 1 1 d . . . . .
H7A H 0.774836 0.395787 0.268642 0.051 Uiso 1 1 calc R U . . .
H7B H 0.795063 0.487299 0.251707 0.051 Uiso 1 1 calc R U . . .
H7C H 0.809883 0.441018 0.425140 0.051 Uiso 1 1 calc R U . . .
N2 N 0.8718(12) 0.4121(15) 0.244(3) 0.034(3) Uani 1 1 d . . . . .
C8 C 0.5520(14) 0.5871(16) 0.956(3) 0.026(2) Uani 1 1 d D . . . .
H8A H 0.572592 0.639437 0.971774 0.039 Uiso 1 1 calc R U . . .
H8B H 0.576164 0.547817 1.025890 0.039 Uiso 1 1 calc R U . . .
H8C H 0.506478 0.589605 0.990459 0.039 Uiso 1 1 calc R U . . .
C9 C 0.5534(14) 0.5628(16) 0.770(3) 0.026(2) Uani 1 1 d D . . . .
H9A H 0.540721 0.506184 0.759019 0.032 Uiso 1 1 calc R U . . .
H9B H 0.520851 0.594833 0.704066 0.032 Uiso 1 1 calc R U . . .
C10 C 0.6104(12) 0.5531(16) 0.514(3) 0.026(2) Uani 1 1 d D . . . .
H10A H 0.572222 0.583134 0.466023 0.032 Uiso 1 1 calc R U . . .
H10B H 0.600223 0.495735 0.503881 0.032 Uiso 1 1 calc R U . . .
C11 C 0.6708(12) 0.5718(16) 0.411(3) 0.026(2) Uani 1 1 d D . . . .
H11A H 0.672586 0.534513 0.316098 0.039 Uiso 1 1 calc R U . . .
H11B H 0.710673 0.566534 0.482781 0.039 Uiso 1 1 calc R U . . .
H11C H 0.667505 0.626296 0.367183 0.039 Uiso 1 1 calc R U . . .
C12 C 0.6051(13) 0.7235(14) 0.654(4) 0.026(2) Uani 1 1 d D . . . .
H12A H 0.596656 0.715177 0.533140 0.039 Uiso 1 1 calc R U . . .
H12B H 0.627158 0.774671 0.672786 0.039 Uiso 1 1 calc R U . . .
H12C H 0.563416 0.723411 0.711144 0.039 Uiso 1 1 calc R U . . .
C13 C 0.6486(13) 0.6569(13) 0.725(4) 0.026(2) Uani 1 1 d D . . . .
H13A H 0.691599 0.660041 0.671970 0.032 Uiso 1 1 calc R U . . .
H13B H 0.656360 0.665799 0.847253 0.032 Uiso 1 1 calc R U . . .
C14 C 0.6676(14) 0.5159(16) 0.778(3) 0.026(2) Uani 1 1 d . . . . .
H14A H 0.660199 0.512484 0.898706 0.039 Uiso 1 1 calc R U . . .
H14B H 0.712807 0.532802 0.761263 0.039 Uiso 1 1 calc R U . . .
H14C H 0.660145 0.463632 0.725860 0.039 Uiso 1 1 calc R U . . .
N1 N 0.6214(12) 0.5747(13) 0.699(3) 0.026(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Pb1 2.986(3) . ?
Br1 Pb1 3.111(3) 4_575 ?
Br2 Pb1 2.982(3) . ?
Br2 Pb1 3.088(3) 4_575 ?
Br3 Pb1 2.988(3) . ?
Br3 Pb1 3.065(3) 4_575 ?
Br4 Pb2 3.144(3) 4_565 ?
Br4 Pb2 2.974(3) . ?
Br5 Pb2 3.009(3) . ?
Br5 Pb2 3.063(3) 4_565 ?
Br6 Pb2 3.105(3) 4_565 ?
Br6 Pb2 2.968(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.539(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 N2 1.54(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.521(7) . ?
C3 N2 1.54(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5 C6 1.537(10) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 N2 1.51(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 N2 1.46(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 C9 1.535(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 N1 1.54(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.539(10) . ?
C10 N1 1.52(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 C13 1.521(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 N1 1.50(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14 N1 1.49(3) . ?

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
Pb1 Br1 Pb1 81.31(7) . 4_575 ?
Pb1 Br2 Pb1 81.75(7) . 4_575 ?
Pb1 Br3 Pb1 82.04(8) . 4_575 ?
Br1 Pb1 Br1 104.33(10) . 4_576 ?
Br1 Pb1 Br2 170.43(10) . 4_576 ?
Br1 Pb1 Br3 92.74(9) . 4_576 ?
Br1 Pb1 Br3 84.44(9) . . ?
Br2 Pb1 Br1 170.70(9) . 4_576 ?
Br2 Pb1 Br1 83.79(9) . . ?
Br2 Pb1 Br1 80.00(8) 4_576 4_576 ?
Br2 Pb1 Br2 92.67(9) . 4_576 ?
Br2 Pb1 Br3 103.36(9) . 4_576 ?
Br2 Pb1 Br3 82.35(9) . . ?
Br3 Pb1 Br1 93.78(9) . 4_576 ?
Br3 Pb1 Br1 81.06(8) 4_576 4_576 ?
Br3 Pb1 Br2 103.95(9) . 4_576 ?
Br3 Pb1 Br2 79.40(9) 4_576 4_576 ?
Br3 Pb1 Br3 173.35(12) . 4_576 ?
Pb2 Br4 Pb2 80.95(7) . 4_565 ?
Pb2 Br5 Pb2 81.73(7) . 4_565 ?
Pb2 Br6 Pb2 81.70(7) . 4_565 ?
Br4 Pb2 Br4 93.16(9) . 4_566 ?
Br4 Pb2 Br5 104.01(9) . 4_566 ?
Br4 Pb2 Br5 85.38(8) . . ?
Br4 Pb2 Br6 170.41(9) . 4_566 ?
Br5 Pb2 Br4 104.60(8) . 4_566 ?
Br5 Pb2 Br4 81.62(8) 4_566 4_566 ?
Br5 Pb2 Br5 168.61(12) . 4_566 ?
Br5 Pb2 Br6 91.87(8) . 4_566 ?
Br5 Pb2 Br6 79.88(8) 4_566 4_566 ?
Br6 Pb2 Br4 171.52(9) . 4_566 ?
Br6 Pb2 Br4 83.57(9) . . ?
Br6 Pb2 Br4 78.62(8) 4_566 4_566 ?
Br6 Pb2 Br5 91.56(9) . 4_566 ?
Br6 Pb2 Br5 82.99(9) . . ?
Br6 Pb2 Br6 105.24(10) . 4_566 ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
N2 C2 C1 114(2) . . ?
N2 C2 H2A 108.9 . . ?
N2 C2 H2B 108.9 . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C4 C3 N2 112(2) . . ?
N2 C3 H3A 109.3 . . ?
N2 C3 H3B 109.3 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
C5 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
H6A C6 H6B 107.8 . . ?
N2 C6 C5 113(2) . . ?
N2 C6 H6A 108.9 . . ?
N2 C6 H6B 108.9 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
C2 N2 C3 106(2) . . ?
C6 N2 C2 112(2) . . ?
C6 N2 C3 113(2) . . ?
C7 N2 C2 111(2) . . ?
C7 N2 C3 109(2) . . ?
C7 N2 C6 106(2) . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
C8 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
N1 C9 C8 112(2) . . ?
N1 C9 H9A 109.2 . . ?
N1 C9 H9B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C11 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
N1 C10 H10A 109.2 . . ?
N1 C10 H10B 109.2 . . ?
N1 C10 C11 112(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
C12 C13 H13A 108.6 . . ?
C12 C13 H13B 108.6 . . ?
H13A C13 H13B 107.5 . . ?
N1 C13 C12 115(2) . . ?
N1 C13 H13A 108.6 . . ?
N1 C13 H13B 108.6 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
C10 N1 C9 103.3(18) . . ?
C13 N1 C9 114(2) . . ?
C13 N1 C10 113(2) . . ?
C14 N1 C9 109(2) . . ?
C14 N1 C10 108(2) . . ?
C14 N1 C13 109(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 N2 C3 176(2) . . . . ?
C1 C2 N2 C6 52(3) . . . . ?
C1 C2 N2 C7 -66(3) . . . . ?
C4 C3 N2 C2 -176(2) . . . . ?
C4 C3 N2 C6 -53(3) . . . . ?
C4 C3 N2 C7 65(3) . . . . ?
C5 C6 N2 C2 54(3) . . . . ?
C5 C6 N2 C3 -66(3) . . . . ?
C5 C6 N2 C7 175(2) . . . . ?
C8 C9 N1 C10 -176(2) . . . . ?
C8 C9 N1 C13 -53(3) . . . . ?
C8 C9 N1 C14 69(3) . . . . ?
C11 C10 N1 C9 172(2) . . . . ?
C11 C10 N1 C13 49(3) . . . . ?
C11 C10 N1 C14 -72(3) . . . . ?
C12 C13 N1 C9 -57(3) . . . . ?
C12 C13 N1 C10 61(3) . . . . ?
C12 C13 N1 C14 -178(2) . . . . ?

_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 7.156
_oxdiff_exptl_absorpt_empirical_full_min 0.563

# start Validation Reply Form
_vrf_PLAT971_TEMAPbBr3_198K      
;
PROBLEM: Check Calcd Resid. Dens.  0.84Ang From Pb2             6.20 eA-3  
RESPONSE: This density residual is very close to the heavy metal that 
has a high electron density.
;
_vrf_PLAT972_TEMAPbBr3_198K      
;
PROBLEM: Check Calcd Resid. Dens.  1.51Ang From Pb1            -4.93 eA-3  
RESPONSE: This density residual is very close to the heavy metal that 
has a high electron density.
;
_vrf_PLAT342_TEMAPbBr3_198K      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03333 Ang.  
RESPONSE: : The quality of this crystal was poor.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_(TEBA)PbBr3_284K
_database_code_depnum_ccdc_archive 'CCDC 2329834'
loop_
_audit_author_name
_audit_author_address
'Zhi-Jie Wang'
;southeast university
China
;
_audit_update_record             
;
2024-01-30 deposited with the CCDC.	2024-03-11 downloaded from the CCDC.
;
_audit_creation_date             2024-01-30
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Br3 Pb), 2(C7 H17 Br N)'
_chemical_formula_sum            'C14 H34 Br8 N2 Pb2'
_chemical_formula_weight         1284.09
_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.9245(5)
_cell_length_b                   35.8983(18)
_cell_length_c                   7.8168(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.353(5)
_cell_angle_gamma                90
_cell_volume                     3005.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10645
_cell_measurement_temperature    284(1)
_cell_measurement_theta_max      28.7190
_cell_measurement_theta_min      2.2050
_shelx_estimated_absorpt_T_max   0.408
_shelx_estimated_absorpt_T_min   0.138
_exptl_absorpt_coefficient_mu    21.829
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.838
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0469
_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       -12
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            31044
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.901
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      284(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -18.00   7.00   0.50    1.00    --    4.71 -99.00  30.00   50
  2  ω    -16.00  34.00   0.50    1.00    --    4.71 -99.00   0.00  100
  3  ω     -8.00  68.00   0.50    1.00    --    4.71  38.00 120.00  152
  4  ω     13.00  70.00   0.50    1.00    --    4.71  38.00 -30.00  114
  5  ω    -13.00  77.00   0.50    1.00    --    4.71  77.00-180.00  180
  6  ω     41.00  66.00   0.50    1.00    --   -5.49  38.00   0.00   50
  7  ω    -17.00   8.00   0.50    1.00    --   -5.49  38.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0644206000
_diffrn_orient_matrix_UB_12      0.0014260000
_diffrn_orient_matrix_UB_13      -0.0022401000
_diffrn_orient_matrix_UB_21      -0.0103932000
_diffrn_orient_matrix_UB_22      0.0178784000
_diffrn_orient_matrix_UB_23      -0.0387881000
_diffrn_orient_matrix_UB_31      0.0113259000
_diffrn_orient_matrix_UB_32      0.0082898000
_diffrn_orient_matrix_UB_33      0.0840105000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4308
_reflns_number_total             5306
_reflns_odcompleteness_completeness 99.97
_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 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         6.417
_refine_diff_density_min         -2.386
_refine_diff_density_rms         0.341
_refine_ls_extinction_coef       0.00031(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   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         5306
_refine_ls_number_restraints     125
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0709
_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)+(0.0696P)²+144.6369P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1713
_refine_ls_wR_factor_ref         0.1809
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C13 = N2-C12 = N2-C9 = N2-C10
 1.5 with sigma of 0.001
 C2-C1 = C6-C5 = C4-C3
 1.54 with sigma of 0.001
 C9-C8 = C12-C11 = C14-C13
 1.54 with sigma of 0.001
 N1-C5 = N1-C2 = N1-C7 = N1-C4
 1.5 with sigma of 0.001
 N1-C1 = N1-C6 = N1-C3
 2.483 with sigma of 0.001
 N2-C11 = N2-C14 = N2-C8
 2.483 with sigma of 0.001
 N2-C10 \\sim N2-C12 \\sim N2-C9 \\sim N2-C13
 with sigma of 0.02
 C9-C13 \\sim C13-C12 \\sim C13-C10 \\sim C9-C12 \\sim C12-C10 \\sim C9-C10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C6 \\sim C5 \\sim C7: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N2 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C1) = Uanis(C6) = Uanis(C3)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,
 H10B), C12(H12A,H12B), C13(H13A,H13B)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C11(H11A,
 H11B,H11C), C14(H14A,H14B,H14C)
;
_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 1.000000 0.500000 1.000000 0.0312(3) Uani 1 2 d S . P . .
Pb2 Pb 1.000000 0.500000 0.500000 0.0312(3) Uani 1 2 d S . P . .
Br3 Br 0.79286(17) 0.52102(5) 0.6931(3) 0.0421(5) Uani 1 1 d . . . . .
Br4 Br 1.05240(19) 0.43885(5) 0.7676(3) 0.0414(5) Uani 1 1 d . . . . .
Br5 Br 1.14847(19) 0.54868(6) 0.7912(3) 0.0446(5) Uani 1 1 d . . . . .
Pb3 Pb 0.48035(6) 0.75040(2) 0.41258(8) 0.0297(2) Uani 1 1 d . . . . .
Br6 Br 0.48465(19) 0.68528(5) 0.6414(2) 0.0383(5) Uani 1 1 d . . . . .
Br7 Br 0.2962(2) 0.71775(6) 0.1218(3) 0.0506(5) Uani 1 1 d . . . . .
Br8 Br 0.6694(2) 0.71766(7) 0.2248(3) 0.0575(6) Uani 1 1 d . . . . .
Br1 Br 0.8436(3) 0.62770(10) 0.4566(4) 0.0884(10) Uani 1 1 d . . . . .
N1 N 0.9162(9) 0.6635(3) 0.7887(12) 0.046(3) Uani 1 1 d D U . . .
C1 C 1.0871(13) 0.6927(5) 0.668(2) 0.050(3) Uani 1 1 d D U . . .
H1A H 1.052758 0.688968 0.546176 0.075 Uiso 1 1 calc R U . . .
H1B H 1.176448 0.694137 0.684767 0.075 Uiso 1 1 calc R U . . .
H1C H 1.055065 0.715385 0.706476 0.075 Uiso 1 1 calc R U . . .
C2 C 1.0504(10) 0.6597(4) 0.774(2) 0.051(4) Uani 1 1 d D U . . .
H2A H 1.062423 0.636474 0.715906 0.061 Uiso 1 1 calc R U . . .
H2B H 1.103128 0.659441 0.888942 0.061 Uiso 1 1 calc R U . . .
C3 C 0.7565(12) 0.6263(5) 0.899(2) 0.050(3) Uani 1 1 d D U . . .
H3A H 0.701457 0.620816 0.790546 0.075 Uiso 1 1 calc R U . . .
H3B H 0.735185 0.650090 0.941288 0.075 Uiso 1 1 calc R U . . .
H3C H 0.748290 0.607401 0.983173 0.075 Uiso 1 1 calc R U . . .
C4 C 0.8922(11) 0.6272(3) 0.872(3) 0.048(4) Uani 1 1 d D U . . .
H4A H 0.949204 0.624565 0.983040 0.058 Uiso 1 1 calc R U . . .
H4B H 0.906309 0.606713 0.797308 0.058 Uiso 1 1 calc R U . . .
C6 C 0.9612(19) 0.6937(5) 1.0801(14) 0.050(3) Uani 1 1 d D U . . .
H6A H 1.048863 0.695509 1.080267 0.075 Uiso 1 1 calc R U . . .
H6B H 0.943900 0.670263 1.129451 0.075 Uiso 1 1 calc R U . . .
H6C H 0.936972 0.713648 1.148360 0.075 Uiso 1 1 calc R U . . .
C5 C 0.8870(18) 0.6965(4) 0.8914(16) 0.053(4) Uani 1 1 d D U . . .
H5A H 0.798260 0.697162 0.891561 0.064 Uiso 1 1 calc R U . . .
H5B H 0.909092 0.719272 0.838046 0.064 Uiso 1 1 calc R U . . .
C7 C 0.8282(16) 0.6672(6) 0.6163(17) 0.046(4) Uani 1 1 d D U . . .
H7A H 0.843667 0.690769 0.563629 0.055 Uiso 1 1 calc R U . . .
H7B H 0.743225 0.667649 0.635807 0.055 Uiso 1 1 calc R U . . .
Br2 Br 0.6027(2) 0.53825(7) 0.1670(4) 0.0623(7) Uani 1 1 d . . . . .
N2 N 0.4187(7) 0.5845(2) 0.2867(10) 0.034(3) Uani 1 1 d D U . . .
C8 C 0.4069(18) 0.6194(4) 0.0095(13) 0.051(5) Uani 1 1 d D U . . .
H8A H 0.439315 0.599322 -0.049391 0.076 Uiso 1 1 calc R U . . .
H8B H 0.426878 0.642724 -0.038610 0.076 Uiso 1 1 calc R U . . .
H8C H 0.317919 0.616997 -0.005566 0.076 Uiso 1 1 calc R U . . .
C9 C 0.4657(13) 0.6181(3) 0.2053(13) 0.043(4) Uani 1 1 d D U . . .
H9A H 0.555893 0.616988 0.220563 0.051 Uiso 1 1 calc R U . . .
H9B H 0.443973 0.640525 0.262063 0.051 Uiso 1 1 calc R U . . .
C10 C 0.4406(13) 0.5498(3) 0.1900(19) 0.035(3) Uani 1 1 d D U . . .
H10A H 0.389801 0.551528 0.073533 0.042 Uiso 1 1 calc R U . . .
H10B H 0.409112 0.528964 0.247326 0.042 Uiso 1 1 calc R U . . .
C11 C 0.4428(16) 0.5528(4) 0.5737(13) 0.043(4) Uani 1 1 d D U . . .
H11A H 0.446409 0.529261 0.516637 0.065 Uiso 1 1 calc R U . . .
H11B H 0.357765 0.558274 0.580081 0.065 Uiso 1 1 calc R U . . .
H11C H 0.492481 0.551672 0.689446 0.065 Uiso 1 1 calc R U . . .
C12 C 0.4935(11) 0.5836(3) 0.4694(12) 0.038(4) Uani 1 1 d D U . . .
H12A H 0.488190 0.607501 0.525151 0.045 Uiso 1 1 calc R U . . .
H12B H 0.580520 0.578737 0.467059 0.045 Uiso 1 1 calc R U . . .
C13 C 0.2806(7) 0.5866(3) 0.2790(19) 0.037(3) Uani 1 1 d D U . . .
H13A H 0.252970 0.564445 0.331659 0.044 Uiso 1 1 calc R U . . .
H13B H 0.237078 0.587711 0.158359 0.044 Uiso 1 1 calc R U . . .
C14 C 0.2501(12) 0.6215(4) 0.377(3) 0.050(5) Uani 1 1 d D U . . .
H14A H 0.162081 0.626373 0.347425 0.075 Uiso 1 1 calc R U . . .
H14B H 0.295210 0.642412 0.345067 0.075 Uiso 1 1 calc R U . . .
H14C H 0.273904 0.617320 0.500727 0.075 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 Br3 3.051(2) 3_767 ?
Pb1 Br3 3.051(2) . ?
Pb1 Br4 2.976(2) 3_767 ?
Pb1 Br4 2.976(2) . ?
Pb1 Br5 3.065(2) 3_767 ?
Pb1 Br5 3.064(2) . ?
Pb2 Br3 3.052(2) . ?
Pb2 Br3 3.052(2) 3_766 ?
Pb2 Br4 3.0085(19) 3_766 ?
Pb2 Br4 3.0085(19) . ?
Pb2 Br5 3.068(2) 3_766 ?
Pb2 Br5 3.068(2) . ?
Pb3 Br6 3.141(2) 4_575 ?
Pb3 Br6 2.9381(19) . ?
Pb3 Br7 2.964(2) . ?
Pb3 Br7 3.054(2) 4_576 ?
Pb3 Br8 2.999(2) . ?
Pb3 Br8 3.091(2) 4_576 ?
Br1 C7 1.918(19) . ?
N1 C2 1.4999(11) . ?
N1 C4 1.5001(10) . ?
N1 C5 1.5000(10) . ?
N1 C7 1.5000(10) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.5399(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C4 1.5397(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6 C5 1.5400(10) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
Br2 C10 1.862(13) . ?
N2 C9 1.5000(10) . ?
N2 C10 1.5002(10) . ?
N2 C12 1.4999(10) . ?
N2 C13 1.4998(10) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8 C9 1.5396(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C11 C12 1.5396(10) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.5396(10) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 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
Br3 Pb1 Br3 180.0 3_767 . ?
Br3 Pb1 Br5 80.13(5) . . ?
Br3 Pb1 Br5 99.87(5) 3_767 . ?
Br3 Pb1 Br5 80.13(5) 3_767 3_767 ?
Br3 Pb1 Br5 99.87(5) . 3_767 ?
Br4 Pb1 Br3 84.53(6) . . ?
Br4 Pb1 Br3 84.52(6) 3_767 3_767 ?
Br4 Pb1 Br3 95.47(6) . 3_767 ?
Br4 Pb1 Br3 95.47(6) 3_767 . ?
Br4 Pb1 Br4 180.00(5) 3_767 . ?
Br4 Pb1 Br5 84.84(6) 3_767 3_767 ?
Br4 Pb1 Br5 84.84(6) . . ?
Br4 Pb1 Br5 95.16(6) 3_767 . ?
Br4 Pb1 Br5 95.16(6) . 3_767 ?
Br5 Pb1 Br5 180.0 . 3_767 ?
Br3 Pb2 Br3 180.00(4) 3_766 . ?
Br3 Pb2 Br5 99.95(5) . 3_766 ?
Br3 Pb2 Br5 80.05(5) 3_766 3_766 ?
Br3 Pb2 Br5 80.05(5) . . ?
Br3 Pb2 Br5 99.95(5) 3_766 . ?
Br4 Pb2 Br3 83.95(5) . . ?
Br4 Pb2 Br3 83.95(5) 3_766 3_766 ?
Br4 Pb2 Br3 96.05(5) . 3_766 ?
Br4 Pb2 Br3 96.05(5) 3_766 . ?
Br4 Pb2 Br4 180.00(5) 3_766 . ?
Br4 Pb2 Br5 84.22(6) 3_766 3_766 ?
Br4 Pb2 Br5 84.22(6) . . ?
Br4 Pb2 Br5 95.78(6) . 3_766 ?
Br4 Pb2 Br5 95.78(6) 3_766 . ?
Br5 Pb2 Br5 180.00(6) . 3_766 ?
Pb1 Br3 Pb2 79.65(5) . . ?
Pb1 Br4 Pb2 81.55(5) . . ?
Pb1 Br5 Pb2 79.18(5) . . ?
Br6 Pb3 Br6 174.32(6) . 4_575 ?
Br6 Pb3 Br7 84.56(6) . 4_576 ?
Br6 Pb3 Br7 94.54(6) . . ?
Br6 Pb3 Br8 83.47(6) . 4_576 ?
Br6 Pb3 Br8 93.21(6) . . ?
Br7 Pb3 Br6 100.67(6) 4_576 4_575 ?
Br7 Pb3 Br6 82.61(6) . 4_575 ?
Br7 Pb3 Br7 98.01(8) . 4_576 ?
Br7 Pb3 Br8 84.19(7) . . ?
Br7 Pb3 Br8 81.17(7) 4_576 4_576 ?
Br7 Pb3 Br8 177.90(7) . 4_576 ?
Br8 Pb3 Br6 81.64(6) . 4_575 ?
Br8 Pb3 Br6 99.43(6) 4_576 4_575 ?
Br8 Pb3 Br7 176.97(6) . 4_576 ?
Br8 Pb3 Br8 96.56(8) . 4_576 ?
Pb3 Br6 Pb3 79.95(4) . 4_576 ?
Pb3 Br7 Pb3 80.98(5) . 4_575 ?
Pb3 Br8 Pb3 79.84(5) . 4_575 ?
C2 N1 C4 102.3(8) . . ?
C2 N1 C5 115.3(12) . . ?
C2 N1 C7 113.6(12) . . ?
C5 N1 C4 112.3(11) . . ?
C7 N1 C4 109.3(12) . . ?
C7 N1 C5 104.2(11) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N1 C2 C1 109.59(10) . . ?
N1 C2 H2A 109.8 . . ?
N1 C2 H2B 109.8 . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
N1 C4 C3 109.57(10) . . ?
N1 C4 H4A 109.8 . . ?
N1 C4 H4B 109.8 . . ?
C3 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
N1 C5 C6 109.53(10) . . ?
N1 C5 H5A 109.8 . . ?
N1 C5 H5B 109.8 . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
Br1 C7 H7A 108.9 . . ?
Br1 C7 H7B 108.9 . . ?
N1 C7 Br1 113.4(11) . . ?
N1 C7 H7A 108.9 . . ?
N1 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C9 N2 C10 110.6(7) . . ?
C12 N2 C9 104.7(5) . . ?
C12 N2 C10 110.5(7) . . ?
C13 N2 C9 111.6(7) . . ?
C13 N2 C10 106.2(6) . . ?
C13 N2 C12 113.2(7) . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
N2 C9 C8 109.58(10) . . ?
N2 C9 H9A 109.8 . . ?
N2 C9 H9B 109.8 . . ?
C8 C9 H9A 109.8 . . ?
C8 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
Br2 C10 H10A 107.6 . . ?
Br2 C10 H10B 107.6 . . ?
N2 C10 Br2 118.8(8) . . ?
N2 C10 H10A 107.6 . . ?
N2 C10 H10B 107.6 . . ?
H10A C10 H10B 107.0 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
N2 C12 C11 109.59(10) . . ?
N2 C12 H12A 109.8 . . ?
N2 C12 H12B 109.8 . . ?
C11 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?
N2 C13 H13A 109.8 . . ?
N2 C13 H13B 109.8 . . ?
N2 C13 C14 109.58(10) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 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
C2 N1 C4 C3 179.5(15) . . . . ?
C2 N1 C5 C6 -61.1(18) . . . . ?
C2 N1 C7 Br1 54.4(16) . . . . ?
C4 N1 C2 C1 172.5(15) . . . . ?
C4 N1 C5 C6 55.5(19) . . . . ?
C4 N1 C7 Br1 -59.1(15) . . . . ?
C5 N1 C2 C1 -65.2(17) . . . . ?
C5 N1 C4 C3 55.3(18) . . . . ?
C5 N1 C7 Br1 -179.3(13) . . . . ?
C7 N1 C2 C1 54.9(19) . . . . ?
C7 N1 C4 C3 -59.8(18) . . . . ?
C7 N1 C5 C6 173.6(16) . . . . ?
C9 N2 C10 Br2 57.3(12) . . . . ?
C9 N2 C12 C11 173.3(12) . . . . ?
C9 N2 C13 C14 -59.8(14) . . . . ?
C10 N2 C9 C8 54.1(14) . . . . ?
C10 N2 C12 C11 -67.6(13) . . . . ?
C10 N2 C13 C14 179.5(13) . . . . ?
C12 N2 C9 C8 173.1(13) . . . . ?
C12 N2 C10 Br2 -58.2(11) . . . . ?
C12 N2 C13 C14 58.1(14) . . . . ?
C13 N2 C9 C8 -64.0(14) . . . . ?
C13 N2 C10 Br2 178.6(10) . . . . ?
C13 N2 C12 C11 51.4(13) . . . . ?

_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 2.196
_oxdiff_exptl_absorpt_empirical_full_min 0.662

# start Validation Reply Form
_vrf_PLAT971_TEBAPbBr3_284K      
;
PROBLEM: Check Calcd Resid. Dens.  0.36Ang From C1              6.84 eA-3  
RESPONSE: Due to the minor disorder of the crystal. The density residual
is very close to the heavy metal that has a high electron density.
;
_vrf_PLAT972_TEBAPbBr3_284K      
;
PROBLEM: Check Calcd Resid. Dens.  1.43Ang From Pb3            -2.68 eA-3  
RESPONSE: This density residual is very close to the heavy metal that 
has a high electron density.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_(TECA)PbBr3_300K
_database_code_depnum_ccdc_archive 'CCDC 2329835'
loop_
_audit_author_name
_audit_author_address
'Zhi-Jie Wang'
;southeast university
China
;
_audit_update_record             
;
2024-01-30 deposited with the CCDC.	2024-03-11 downloaded from the CCDC.
;
_audit_creation_date             2024-01-28
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Br3 Pb), 2(C7 H17 Cl N)'
_chemical_formula_sum            'C14 H34 Br6 Cl2 N2 Pb2'
_chemical_formula_weight         1195.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.8700(5)
_cell_length_b                   35.6974(15)
_cell_length_c                   7.7943(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.977(2)
_cell_angle_gamma                90
_cell_volume                     2969.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.22
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.585
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4053
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1208 before and 0.0754 after correction.
The Ratio of minimum to maximum transmission is 0.5436.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.674
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod-shaped
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1260
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            66050
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_min         1.908
_diffrn_ambient_temperature      300.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_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
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4493
_reflns_number_total             6806
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.837
_refine_diff_density_min         -1.663
_refine_diff_density_rms         0.241
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         6806
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0350
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0375P)²+1.9244P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0990
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C13(H13A,H13B), C14(H14A,H14B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C)
;
_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
Br1 Br 0.51195(8) 0.31507(2) -0.63552(10) 0.0479(2) Uani 1 1 d . . . . .
Br2 Br 0.69811(9) 0.28247(3) -0.11361(12) 0.0623(2) Uani 1 1 d . . . . .
Br3 Br 0.32290(10) 0.28171(3) -0.21305(12) 0.0705(3) Uani 1 1 d . . . . .
Pb1 Pb 0.51414(3) 0.24953(2) -0.40518(3) 0.03921(9) Uani 1 1 d . . . . .
Br4 Br 0.15187(8) 0.54811(2) 0.79081(11) 0.0538(2) Uani 1 1 d . . . . .
Br5 Br 0.04977(9) 0.43811(2) 0.76479(11) 0.0537(2) Uani 1 1 d . . . . .
Br6 Br 0.20735(8) 0.47837(2) 1.30558(11) 0.0527(2) Uani 1 1 d . . . . .
Pb2 Pb 0.000000 0.500000 0.500000 0.03977(11) Uani 1 2 d S . P . .
Pb3 Pb 0.000000 0.500000 1.000000 0.03990(11) Uani 1 2 d S . P . .
C1 C 0.5490(7) 0.44834(18) -0.5921(8) 0.0366(16) Uani 1 1 d . . . . .
H1A H 0.483580 0.453591 -0.690524 0.055 Uiso 1 1 calc R U . . .
H1B H 0.620886 0.438704 -0.632447 0.055 Uiso 1 1 calc R U . . .
H1C H 0.571469 0.470957 -0.527011 0.055 Uiso 1 1 calc R U . . .
C2 C 0.5004(8) 0.4178(2) -0.4685(10) 0.050(2) Uani 1 1 d . . . . .
H2A H 0.413313 0.422966 -0.465323 0.060 Uiso 1 1 calc R U . . .
H2B H 0.504144 0.393206 -0.520436 0.060 Uiso 1 1 calc R U . . .
C3 C 0.7559(7) 0.3790(2) -0.3680(11) 0.056(2) Uani 1 1 d . . . . .
H3A H 0.725066 0.381128 -0.491503 0.084 Uiso 1 1 calc R U . . .
H3B H 0.723751 0.356540 -0.325212 0.084 Uiso 1 1 calc R U . . .
H3C H 0.845757 0.378116 -0.345612 0.084 Uiso 1 1 calc R U . . .
C4 C 0.7125(7) 0.4132(2) -0.2745(10) 0.0461(18) Uani 1 1 d . . . . .
H4A H 0.753972 0.412344 -0.152778 0.055 Uiso 1 1 calc R U . . .
H4B H 0.740947 0.435634 -0.325113 0.055 Uiso 1 1 calc R U . . .
C5 C 0.5779(8) 0.3785(2) 0.0052(8) 0.048(2) Uani 1 1 d . . . . .
H5A H 0.667787 0.377865 0.024999 0.072 Uiso 1 1 calc R U . . .
H5B H 0.547225 0.355638 0.046326 0.072 Uiso 1 1 calc R U . . .
H5C H 0.551240 0.399326 0.067072 0.072 Uiso 1 1 calc R U . . .
C6 C 0.5249(8) 0.38294(19) -0.1948(11) 0.054(2) Uani 1 1 d . . . . .
H6A H 0.544423 0.360417 -0.253857 0.065 Uiso 1 1 calc R U . . .
H6B H 0.434335 0.384849 -0.212037 0.065 Uiso 1 1 calc R U . . .
C7 C 0.5606(7) 0.4525(2) -0.1855(10) 0.0484(19) Uani 1 1 d . . . . .
H7A H 0.591249 0.473068 -0.246965 0.058 Uiso 1 1 calc R U . . .
H7B H 0.612470 0.451125 -0.069697 0.058 Uiso 1 1 calc R U . . .
Cl1 Cl 0.4072(3) 0.46199(9) -0.1652(4) 0.1029(10) Uani 1 1 d . . . . .
N1 N 0.5742(6) 0.41662(16) -0.2812(7) 0.0388(14) Uani 1 1 d . . . . .
C8 C 0.2488(8) 0.3774(2) 0.0987(11) 0.060(2) Uani 1 1 d . . . . .
H8A H 0.259562 0.358711 0.014285 0.090 Uiso 1 1 calc R U . . .
H8B H 0.308367 0.373261 0.204863 0.090 Uiso 1 1 calc R U . . .
H8C H 0.262044 0.401806 0.053493 0.090 Uiso 1 1 calc R U . . .
C9 C 0.1153(9) 0.3750(2) 0.1362(12) 0.067(3) Uani 1 1 d . . . . .
H9A H 0.103230 0.395614 0.212302 0.080 Uiso 1 1 calc R U . . .
H9B H 0.056373 0.378298 0.026999 0.080 Uiso 1 1 calc R U . . .
C10 C 0.0313(9) 0.3048(4) -0.0791(13) 0.103(4) Uani 1 1 d . . . . .
H10A H 0.073515 0.288982 -0.148979 0.154 Uiso 1 1 calc R U . . .
H10B H 0.027374 0.329892 -0.124380 0.154 Uiso 1 1 calc R U . . .
H10C H -0.052093 0.295608 -0.082538 0.154 Uiso 1 1 calc R U . . .
C11 C 0.1045(10) 0.3048(3) 0.1131(12) 0.075(3) Uani 1 1 d . . . . .
H11A H 0.080913 0.282580 0.170934 0.089 Uiso 1 1 calc R U . . .
H11B H 0.193334 0.302859 0.111599 0.089 Uiso 1 1 calc R U . . .
C12 C -0.1006(8) 0.3082(2) 0.3427(12) 0.064(2) Uani 1 1 d . . . . .
H12A H -0.114007 0.286653 0.267559 0.096 Uiso 1 1 calc R U . . .
H12B H -0.178044 0.315065 0.376390 0.096 Uiso 1 1 calc R U . . .
H12C H -0.039442 0.302290 0.445166 0.096 Uiso 1 1 calc R U . . .
C13 C -0.0537(8) 0.3407(3) 0.2461(12) 0.068(3) Uani 1 1 d . . . . .
H13A H -0.063715 0.363556 0.309025 0.082 Uiso 1 1 calc R U . . .
H13B H -0.107293 0.342652 0.131735 0.082 Uiso 1 1 calc R U . . .
C14 C 0.1706(8) 0.3322(2) 0.3919(10) 0.060(2) Uani 1 1 d . . . . .
H14A H 0.256058 0.330511 0.372764 0.072 Uiso 1 1 calc R U . . .
H14B H 0.149848 0.308623 0.441055 0.072 Uiso 1 1 calc R U . . .
Cl2 Cl 0.1607(4) 0.36869(10) 0.5423(4) 0.1232(12) Uani 1 1 d . . . . .
N2 N 0.0840(6) 0.33856(17) 0.2203(8) 0.0477(16) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Pb1 2.9464(8) . ?
Br1 Pb1 3.1233(8) 4_565 ?
Br2 Pb1 2.9691(9) . ?
Br2 Pb1 3.0299(9) 4_566 ?
Br3 Pb1 3.0115(9) . ?
Br3 Pb1 3.0698(10) 4_566 ?
Br4 Pb2 3.0640(8) . ?
Br4 Pb3 3.0592(8) . ?
Br5 Pb2 3.0012(8) . ?
Br5 Pb3 2.9852(8) . ?
Br6 Pb2 3.0452(8) 1_556 ?
Br6 Pb3 3.0504(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.610(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 N1 1.526(9) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C4 1.539(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 N1 1.499(9) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C5 C6 1.564(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 N1 1.524(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 Cl1 1.737(8) . ?
C7 N1 1.504(9) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8 C9 1.536(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 N2 1.524(9) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 C11 1.557(13) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 N2 1.508(10) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C12 C13 1.523(12) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 N2 1.549(10) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 Cl2 1.769(9) . ?
C14 N2 1.499(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Pb1 Br1 Pb1 79.838(18) . 4_565 ?
Pb1 Br2 Pb1 81.02(2) . 4_566 ?
Pb1 Br3 Pb1 79.71(2) . 4_566 ?
Br1 Pb1 Br1 174.95(2) . 4_566 ?
Br1 Pb1 Br2 84.39(2) . 4_565 ?
Br1 Pb1 Br2 94.48(2) . . ?
Br1 Pb1 Br3 83.48(3) . 4_565 ?
Br1 Pb1 Br3 94.24(3) . . ?
Br2 Pb1 Br1 82.40(2) . 4_566 ?
Br2 Pb1 Br1 99.95(2) 4_565 4_566 ?
Br2 Pb1 Br2 98.20(3) . 4_565 ?
Br2 Pb1 Br3 82.05(3) 4_565 4_565 ?
Br2 Pb1 Br3 177.91(3) . 4_565 ?
Br2 Pb1 Br3 84.05(3) . . ?
Br3 Pb1 Br1 81.52(2) . 4_566 ?
Br3 Pb1 Br1 99.61(2) 4_565 4_566 ?
Br3 Pb1 Br2 177.44(3) . 4_565 ?
Br3 Pb1 Br3 95.65(4) . 4_565 ?
Pb3 Br4 Pb2 79.056(19) . . ?
Pb3 Br5 Pb2 81.232(19) . . ?
Pb2 Br6 Pb3 79.48(2) 1_556 . ?
Br4 Pb2 Br4 180.0 . 3_566 ?
Br5 Pb2 Br4 84.42(2) 3_566 3_566 ?
Br5 Pb2 Br4 95.58(2) . 3_566 ?
Br5 Pb2 Br4 84.42(2) . . ?
Br5 Pb2 Br4 95.58(2) 3_566 . ?
Br5 Pb2 Br5 180.0 . 3_566 ?
Br5 Pb2 Br6 95.85(2) 3_566 3_567 ?
Br5 Pb2 Br6 84.15(2) 3_566 1_554 ?
Br5 Pb2 Br6 84.15(2) . 3_567 ?
Br5 Pb2 Br6 95.85(2) . 1_554 ?
Br6 Pb2 Br4 99.48(2) 1_554 . ?
Br6 Pb2 Br4 80.52(2) 3_567 . ?
Br6 Pb2 Br4 99.48(2) 3_567 3_566 ?
Br6 Pb2 Br4 80.52(2) 1_554 3_566 ?
Br6 Pb2 Br6 180.0 3_567 1_554 ?
Br4 Pb3 Br4 180.00(2) . 3_567 ?
Br5 Pb3 Br4 95.23(2) . 3_567 ?
Br5 Pb3 Br4 84.77(2) 3_567 3_567 ?
Br5 Pb3 Br4 84.77(2) . . ?
Br5 Pb3 Br4 95.23(2) 3_567 . ?
Br5 Pb3 Br5 180.0 3_567 . ?
Br5 Pb3 Br6 84.33(2) . 3_567 ?
Br5 Pb3 Br6 95.67(2) 3_567 3_567 ?
Br5 Pb3 Br6 84.33(2) 3_567 . ?
Br5 Pb3 Br6 95.67(2) . . ?
Br6 Pb3 Br4 80.51(2) . 3_567 ?
Br6 Pb3 Br4 80.52(2) 3_567 . ?
Br6 Pb3 Br4 99.48(2) 3_567 3_567 ?
Br6 Pb3 Br4 99.49(2) . . ?
Br6 Pb3 Br6 180.00(4) . 3_567 ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
N1 C2 C1 114.7(6) . . ?
N1 C2 H2A 108.6 . . ?
N1 C2 H2B 108.6 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
C3 C4 H4A 108.2 . . ?
C3 C4 H4B 108.2 . . ?
H4A C4 H4B 107.4 . . ?
N1 C4 C3 116.3(6) . . ?
N1 C4 H4A 108.2 . . ?
N1 C4 H4B 108.2 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
C5 C6 H6A 108.5 . . ?
C5 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
N1 C6 C5 115.2(6) . . ?
N1 C6 H6A 108.5 . . ?
N1 C6 H6B 108.5 . . ?
H7A C7 H7B 107.7 . . ?
Cl1 C7 H7A 108.9 . . ?
Cl1 C7 H7B 108.9 . . ?
N1 C7 H7A 108.9 . . ?
N1 C7 H7B 108.9 . . ?
N1 C7 Cl1 113.5(5) . . ?
C4 N1 C2 112.1(6) . . ?
C4 N1 C6 110.8(6) . . ?
C4 N1 C7 104.2(5) . . ?
C6 N1 C2 106.2(6) . . ?
C7 N1 C2 111.6(6) . . ?
C7 N1 C6 112.1(5) . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
C8 C9 H9A 108.5 . . ?
C8 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
N2 C9 C8 115.2(7) . . ?
N2 C9 H9A 108.5 . . ?
N2 C9 H9B 108.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
C10 C11 H11A 108.4 . . ?
C10 C11 H11B 108.4 . . ?
H11A C11 H11B 107.5 . . ?
N2 C11 C10 115.5(8) . . ?
N2 C11 H11A 108.4 . . ?
N2 C11 H11B 108.4 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
C12 C13 H13A 108.1 . . ?
C12 C13 H13B 108.1 . . ?
C12 C13 N2 116.7(7) . . ?
H13A C13 H13B 107.3 . . ?
N2 C13 H13A 108.1 . . ?
N2 C13 H13B 108.1 . . ?
H14A C14 H14B 107.9 . . ?
Cl2 C14 H14A 109.2 . . ?
Cl2 C14 H14B 109.2 . . ?
N2 C14 H14A 109.2 . . ?
N2 C14 H14B 109.2 . . ?
N2 C14 Cl2 111.9(5) . . ?
C9 N2 C13 108.3(6) . . ?
C11 N2 C9 112.0(6) . . ?
C11 N2 C13 111.0(7) . . ?
C14 N2 C9 111.0(7) . . ?
C14 N2 C11 103.9(6) . . ?
C14 N2 C13 110.5(6) . . ?

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 N1 C4 -51.7(8) . . . . ?
C1 C2 N1 C6 -172.8(6) . . . . ?
C1 C2 N1 C7 64.8(8) . . . . ?
C3 C4 N1 C2 -57.5(8) . . . . ?
C3 C4 N1 C6 60.9(8) . . . . ?
C3 C4 N1 C7 -178.4(6) . . . . ?
C5 C6 N1 C2 -174.1(6) . . . . ?
C5 C6 N1 C4 64.0(8) . . . . ?
C5 C6 N1 C7 -52.0(9) . . . . ?
Cl1 C7 N1 C2 61.8(7) . . . . ?
Cl1 C7 N1 C4 -177.0(5) . . . . ?
Cl1 C7 N1 C6 -57.2(8) . . . . ?
C8 C9 N2 C11 -56.3(10) . . . . ?
C8 C9 N2 C13 -179.2(8) . . . . ?
C8 C9 N2 C14 59.3(9) . . . . ?
C10 C11 N2 C9 -56.5(11) . . . . ?
C10 C11 N2 C13 64.8(10) . . . . ?
C10 C11 N2 C14 -176.5(8) . . . . ?
C12 C13 N2 C9 -175.1(8) . . . . ?
C12 C13 N2 C11 61.5(10) . . . . ?
C12 C13 N2 C14 -53.2(10) . . . . ?
Cl2 C14 N2 C9 60.2(8) . . . . ?
Cl2 C14 N2 C11 -179.2(6) . . . . ?
Cl2 C14 N2 C13 -60.0(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
