# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_h3_sqd
_database_code_depnum_ccdc_archive 'CCDC 2235623'
loop_
_audit_author_name
_audit_author_address
ChengAnHu
;Guangdong University of Technology
China
;
_audit_update_record             
;
2023-01-11 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_audit_creation_date             2022-11-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Bi2 Br9, 3(C5 H14 N3)'
_chemical_formula_sum            'C15 H42 Bi2 Br9 N9'
_chemical_formula_weight         1485.72
_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'
Bi Bi -4.1077 10.2566 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9420(8)
_cell_length_b                   12.4124(10)
_cell_length_c                   14.7289(11)
_cell_angle_alpha                71.210(3)
_cell_angle_beta                 88.227(3)
_cell_angle_gamma                85.193(3)
_cell_volume                     1887.1(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7523
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.55
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.862
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0061
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1403 before and 0.0707 after correction.
The Ratio of minimum to maximum transmission is 0.2210.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.615
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_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  0.0693
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33390
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.435
_diffrn_reflns_theta_min         2.547
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6238
_reflns_number_total             7694
_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       H3
_computing_data_collection       ?
_computing_data_reduction        H3
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.307
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         7694
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0319
_refine_ls_restrained_S_all      0.990
_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)+(0.0223P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0739
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a X=CH2 refined with riding coordinates:
 N00D(H00O,H00P), N00E(H00A,H00B), N00M(H00Z,H)
2.b Idealised Me refined as rotating group:
 C00O(H00C,H00D,H00E), C00P(H00,HA,HB), C00Q(H00F,H00G,H00H), C00R(H00I,H00J,
 H00K), C00S(H00L,H00M,H00N), C00T(H0AA,HC,HD), C00U(H1AA,HE,HF), C00V(H00Q,
 H00R,H00S), C00W(H00T,H00U,H00V), C00X(H2AA,HG,HH), C00Y(H00W,H00X,H00Y),
 C1(H1A,H1B,H1C)
;
_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
Bi01 Bi 0.77962(2) 0.20156(2) 0.17529(2) 0.02983(7) Uani 1 1 d . . . . .
Bi02 Bi 0.75029(2) 0.40814(2) 0.33258(2) 0.03188(7) Uani 1 1 d . . . . .
Br03 Br 0.77527(6) 0.15174(6) 0.39080(4) 0.03573(14) Uani 1 1 d . . . . .
Br04 Br 0.99558(6) 0.06621(6) 0.18971(4) 0.03746(15) Uani 1 1 d . . . . .
Br05 Br 0.94087(6) 0.38888(5) 0.17485(4) 0.03621(15) Uani 1 1 d . . . . .
Br06 Br 0.72683(6) 0.64358(6) 0.26193(5) 0.03995(15) Uani 1 1 d . . . . .
Br07 Br 0.56906(6) 0.37225(6) 0.18919(5) 0.04025(16) Uani 1 1 d . . . . .
Br08 Br 0.77653(6) 0.26078(7) -0.02079(4) 0.04354(17) Uani 1 1 d . . . . .
Br09 Br 0.62867(6) 0.03186(6) 0.19616(5) 0.04441(17) Uani 1 1 d . . . . .
Br0A Br 0.93136(7) 0.40822(7) 0.45078(5) 0.04567(17) Uani 1 1 d . . . . .
Br0B Br 0.57647(7) 0.38911(7) 0.46604(5) 0.05124(19) Uani 1 1 d . . . . .
N00C N 0.7055(5) 0.6889(5) -0.0092(4) 0.0378(13) Uani 1 1 d . . . . .
N00D N 1.0864(5) 0.1544(6) 0.3893(4) 0.0562(18) Uani 1 1 d . . . . .
H00O H 1.077997 0.151152 0.331067 0.067 Uiso 1 1 calc R . . . .
H00P H 1.021488 0.154012 0.426237 0.067 Uiso 1 1 calc R . . . .
N00E N 0.9085(5) 0.6803(5) 0.0326(4) 0.0398(13) Uani 1 1 d . . . . .
H00A H 0.919714 0.610359 0.029966 0.048 Uiso 1 1 calc R . . . .
H00B H 0.969930 0.712666 0.047747 0.048 Uiso 1 1 calc R . . . .
N00F N 0.3087(5) 0.7640(5) 0.2798(4) 0.0375(13) Uani 1 1 d . . . . .
N00G N 0.2138(5) 0.6001(5) 0.2879(4) 0.0418(13) Uani 1 1 d . . . . .
N00H N 1.2950(5) 0.1604(5) 0.3663(4) 0.0405(13) Uani 1 1 d . . . . .
N00I N 0.7860(5) 0.8438(5) 0.0173(4) 0.0392(13) Uani 1 1 d . . . . .
N00J N 1.2070(6) 0.1673(5) 0.5093(4) 0.0446(14) Uani 1 1 d . . . . .
C00K C 1.1962(6) 0.1598(5) 0.4214(5) 0.0356(14) Uani 1 1 d . . . . .
C00L C 0.8001(6) 0.7365(6) 0.0140(4) 0.0329(14) Uani 1 1 d . . . . .
N00M N 0.4200(5) 0.6105(5) 0.2558(4) 0.0472(15) Uani 1 1 d . . . . .
H00Z H 0.486177 0.648450 0.246249 0.057 Uiso 1 1 calc R . . . .
H H 0.424331 0.540720 0.252481 0.057 Uiso 1 1 calc R . . . .
C00N C 0.3140(6) 0.6583(6) 0.2750(4) 0.0384(15) Uani 1 1 d . . . . .
C00O C 0.8786(7) 0.8849(6) 0.0676(5) 0.0454(17) Uani 1 1 d . . . . .
H00C H 0.912761 0.821060 0.121454 0.068 Uiso 1 1 calc GR . . . .
H00D H 0.839559 0.944392 0.091598 0.068 Uiso 1 1 calc GR . . . .
H00E H 0.944635 0.916207 0.022765 0.068 Uiso 1 1 calc GR . . . .
C00P C 0.2252(7) 0.8033(7) 0.3444(5) 0.0515(19) Uani 1 1 d . . . . .
H00 H 0.173237 0.742204 0.378613 0.077 Uiso 1 1 calc GR . . . .
HA H 0.173505 0.870317 0.307018 0.077 Uiso 1 1 calc GR . . . .
HB H 0.273032 0.823668 0.390795 0.077 Uiso 1 1 calc GR . . . .
C00Q C 0.7279(7) 0.5848(6) -0.0345(5) 0.0438(17) Uani 1 1 d . . . . .
H00F H 0.802982 0.588944 -0.073091 0.066 Uiso 1 1 calc GR . . . .
H00G H 0.658483 0.576439 -0.071520 0.066 Uiso 1 1 calc GR . . . .
H00H H 0.737271 0.518982 0.024118 0.066 Uiso 1 1 calc GR . . . .
C00R C 0.5795(6) 0.7123(7) 0.0187(5) 0.0475(18) Uani 1 1 d . . . . .
H00I H 0.578317 0.763169 0.057722 0.071 Uiso 1 1 calc GR . . . .
H00J H 0.545679 0.640525 0.056070 0.071 Uiso 1 1 calc GR . . . .
H00K H 0.529843 0.748968 -0.038886 0.071 Uiso 1 1 calc GR . . . .
C00S C 0.7020(7) 0.9332(7) -0.0442(5) 0.0505(18) Uani 1 1 d . . . . .
H00L H 0.748456 0.996617 -0.082674 0.076 Uiso 1 1 calc GR . . . .
H00M H 0.641937 0.960714 -0.004332 0.076 Uiso 1 1 calc GR . . . .
H00N H 0.659308 0.902458 -0.086758 0.076 Uiso 1 1 calc GR . . . .
C00T C 0.0901(6) 0.6544(7) 0.2638(5) 0.0511(19) Uani 1 1 d . . . . .
H0AA H 0.043893 0.649629 0.322855 0.077 Uiso 1 1 calc GR . . . .
HC H 0.048425 0.615360 0.226882 0.077 Uiso 1 1 calc GR . . . .
HD H 0.094946 0.734761 0.225406 0.077 Uiso 1 1 calc GR . . . .
C00U C 0.4129(7) 0.8334(6) 0.2449(6) 0.0515(19) Uani 1 1 d . . . . .
H1AA H 0.482677 0.802107 0.288156 0.077 Uiso 1 1 calc GR . . . .
HE H 0.389908 0.912114 0.243073 0.077 Uiso 1 1 calc GR . . . .
HF H 0.435681 0.832393 0.180340 0.077 Uiso 1 1 calc GR . . . .
C00V C 1.1087(8) 0.1353(7) 0.5825(5) 0.060(2) Uani 1 1 d . . . . .
H00Q H 1.055782 0.203543 0.581066 0.090 Uiso 1 1 calc GR . . . .
H00R H 1.145528 0.101243 0.646168 0.090 Uiso 1 1 calc GR . . . .
H00S H 1.059746 0.079919 0.568549 0.090 Uiso 1 1 calc GR . . . .
C00W C 1.2832(7) 0.1835(7) 0.2637(5) 0.0502(19) Uani 1 1 d . . . . .
H00T H 1.278386 0.111505 0.250448 0.075 Uiso 1 1 calc GR . . . .
H00U H 1.354713 0.221344 0.230675 0.075 Uiso 1 1 calc GR . . . .
H00V H 1.208561 0.233228 0.240745 0.075 Uiso 1 1 calc GR . . . .
C00X C 0.2271(8) 0.4778(8) 0.3031(8) 0.075(3) Uani 1 1 d . . . . .
H2AA H 0.241277 0.464611 0.241358 0.112 Uiso 1 1 calc GR . . . .
HG H 0.152103 0.443506 0.332584 0.112 Uiso 1 1 calc GR . . . .
HH H 0.296853 0.442966 0.345533 0.112 Uiso 1 1 calc GR . . . .
C00Y C 1.4106(7) 0.1004(10) 0.4056(6) 0.078(3) Uani 1 1 d . . . . .
H00W H 1.401751 0.064105 0.474993 0.117 Uiso 1 1 calc GR . . . .
H00X H 1.474062 0.154637 0.393077 0.117 Uiso 1 1 calc GR . . . .
H00Y H 1.434012 0.041895 0.375477 0.117 Uiso 1 1 calc GR . . . .
C1 C 1.3070(10) 0.2219(10) 0.5361(6) 0.083(3) Uani 1 1 d . . . . .
H1A H 1.355195 0.165685 0.587468 0.125 Uiso 1 1 calc GR . . . .
H1B H 1.272967 0.284451 0.558560 0.125 Uiso 1 1 calc GR . . . .
H1C H 1.359819 0.252147 0.480236 0.125 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
Bi01 Br03 3.0318(7) . ?
Bi01 Br04 2.7545(7) . ?
Bi01 Br05 3.0326(7) . ?
Bi01 Br07 3.0448(8) . ?
Bi01 Br08 2.7416(7) . ?
Bi01 Br09 2.7191(7) . ?
Bi02 Br03 3.0082(7) . ?
Bi02 Br05 3.1267(7) . ?
Bi02 Br06 2.7606(8) . ?
Bi02 Br07 3.0991(7) . ?
Bi02 Br0A 2.6780(7) . ?
Bi02 Br0B 2.6613(7) . ?
N00C C00L 1.338(8) . ?
N00C C00Q 1.456(9) . ?
N00C C00R 1.459(8) . ?
N00D C00K 1.319(8) . ?
N00E C00L 1.314(8) . ?
N00F C00N 1.332(9) . ?
N00F C00P 1.466(9) . ?
N00F C00U 1.466(8) . ?
N00G C00N 1.339(8) . ?
N00G C00T 1.462(9) . ?
N00G C00X 1.457(11) . ?
N00H C00K 1.330(8) . ?
N00H C00W 1.452(8) . ?
N00H C00Y 1.449(10) . ?
N00I C00L 1.344(8) . ?
N00I C00O 1.488(8) . ?
N00I C00S 1.459(9) . ?
N00J C00K 1.338(8) . ?
N00J C00V 1.484(9) . ?
N00J C1 1.461(10) . ?
N00M C00N 1.323(9) . ?

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
Br03 Bi01 Br05 84.326(18) . . ?
Br03 Bi01 Br07 80.906(19) . . ?
Br04 Bi01 Br03 90.296(19) . . ?
Br04 Bi01 Br05 85.55(2) . . ?
Br04 Bi01 Br07 167.32(2) . . ?
Br05 Bi01 Br07 84.50(2) . . ?
Br08 Bi01 Br03 176.21(2) . . ?
Br08 Bi01 Br04 92.85(2) . . ?
Br08 Bi01 Br05 93.81(2) . . ?
Br08 Bi01 Br07 95.64(2) . . ?
Br09 Bi01 Br03 89.49(2) . . ?
Br09 Bi01 Br04 96.00(2) . . ?
Br09 Bi01 Br05 173.64(2) . . ?
Br09 Bi01 Br07 93.06(2) . . ?
Br09 Bi01 Br08 92.28(2) . . ?
Br03 Bi02 Br05 83.114(18) . . ?
Br03 Bi02 Br07 80.401(19) . . ?
Br06 Bi02 Br03 174.74(2) . . ?
Br06 Bi02 Br05 93.028(19) . . ?
Br06 Bi02 Br07 95.56(2) . . ?
Br07 Bi02 Br05 82.044(18) . . ?
Br0A Bi02 Br03 91.52(2) . . ?
Br0A Bi02 Br05 90.80(2) . . ?
Br0A Bi02 Br06 92.10(2) . . ?
Br0A Bi02 Br07 169.77(2) . . ?
Br0B Bi02 Br03 87.81(2) . . ?
Br0B Bi02 Br05 169.84(2) . . ?
Br0B Bi02 Br06 95.73(2) . . ?
Br0B Bi02 Br07 91.96(2) . . ?
Br0B Bi02 Br0A 94.02(3) . . ?
Bi02 Br03 Bi01 81.952(17) . . ?
Bi01 Br05 Bi02 80.022(16) . . ?
Bi01 Br07 Bi02 80.275(18) . . ?
C00L N00C C00Q 119.5(6) . . ?
C00L N00C C00R 122.5(6) . . ?
C00Q N00C C00R 115.0(5) . . ?
C00N N00F C00P 123.1(5) . . ?
C00N N00F C00U 119.3(6) . . ?
C00U N00F C00P 114.6(6) . . ?
C00N N00G C00T 123.4(6) . . ?
C00N N00G C00X 119.4(6) . . ?
C00X N00G C00T 115.3(6) . . ?
C00K N00H C00W 120.8(6) . . ?
C00K N00H C00Y 121.5(6) . . ?
C00Y N00H C00W 114.1(6) . . ?
C00L N00I C00O 119.7(6) . . ?
C00L N00I C00S 123.8(6) . . ?
C00S N00I C00O 114.9(6) . . ?
C00K N00J C00V 121.8(6) . . ?
C00K N00J C1 122.8(6) . . ?
C1 N00J C00V 114.9(6) . . ?
N00D C00K N00H 120.5(6) . . ?
N00D C00K N00J 119.2(6) . . ?
N00H C00K N00J 120.2(6) . . ?
N00C C00L N00I 120.3(6) . . ?
N00E C00L N00C 121.0(6) . . ?
N00E C00L N00I 118.8(6) . . ?
N00F C00N N00G 121.3(6) . . ?
N00M C00N N00F 119.4(6) . . ?
N00M C00N N00G 119.3(7) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_h18
_database_code_depnum_ccdc_archive 'CCDC 2235626'
loop_
_audit_author_name
_audit_author_address
ChengAnHu
;Guangdong University of Technology
China
;
_audit_update_record             
;
2023-01-11 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_audit_creation_date             2023-01-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(Bi2 Br10), 2(C5 H9 N2)'
_chemical_formula_sum            'C10 H18 Bi Br5 N4'
_chemical_formula_weight         802.81
_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'
Bi Bi -4.1077 10.2566 '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'

_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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
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'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   14.7839(12)
_cell_length_b                   16.9690(10)
_cell_length_c                   8.5719(6)
_cell_angle_alpha                90
_cell_angle_beta                 113.558(2)
_cell_angle_gamma                90
_cell_volume                     1971.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6761
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      3.01
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.076
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0062
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1421 before and 0.0688 after correction.
The Ratio of minimum to maximum transmission is 0.2246.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.705
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_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  0.0599
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20869
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.397
_diffrn_reflns_theta_min         3.006
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1954
_reflns_number_total             2078
_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 V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.169
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2078
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0277
_refine_ls_restrained_S_all      1.048
_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)+(0.0417P)²+8.4802P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0735
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C1AA(H1AA), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.33922(2) 0.500000 0.45645(3) 0.02753(11) Uani 1 2 d S T P . .
Br3 Br 0.18260(6) 0.500000 0.13793(10) 0.03705(19) Uani 1 2 d S T P . .
Br1 Br 0.52939(5) 0.500000 0.75115(9) 0.03261(17) Uani 1 2 d S T P . .
Br4 Br 0.34187(4) 0.66812(3) 0.47467(6) 0.03454(15) Uani 1 1 d . . . . .
Br2 Br 0.23451(7) 0.500000 0.65529(12) 0.0448(2) Uani 1 2 d S T P . .
N2 N 0.3877(3) 0.7758(3) 1.0997(6) 0.0350(10) Uani 1 1 d . . . . .
N3 N 0.3332(4) 0.7192(3) 0.8553(6) 0.0425(11) Uani 1 1 d . . . . .
H3 H 0.305123 0.711354 0.744655 0.051 Uiso 1 1 calc R . . . .
C0AA C 0.5099(5) 0.8737(4) 1.2749(8) 0.0474(14) Uani 1 1 d . . . . .
H0AA H 0.512927 0.896511 1.172047 0.071 Uiso 1 1 calc GR . . . .
H0AB H 0.560667 0.832897 1.320283 0.071 Uiso 1 1 calc GR . . . .
H0AC H 0.521312 0.915073 1.360390 0.071 Uiso 1 1 calc GR . . . .
C1AA C 0.4140(4) 0.6982(3) 1.1264(7) 0.0362(12) Uani 1 1 d . . . . .
H1AA H 0.450294 0.673969 1.233277 0.043 Uiso 1 1 calc R . . . .
C5 C 0.3376(4) 0.7875(4) 0.9331(7) 0.0377(12) Uani 1 1 d . . . . .
H5 H 0.310114 0.835975 0.879886 0.045 Uiso 1 1 calc R . . . .
C2 C 0.4104(5) 0.8379(3) 1.2319(8) 0.0448(14) Uani 1 1 d . . . . .
H2A H 0.407726 0.814838 1.336079 0.054 Uiso 1 1 calc R . . . .
H2B H 0.359589 0.879739 1.190760 0.054 Uiso 1 1 calc R . . . .
C6 C 0.3798(4) 0.6627(3) 0.9755(7) 0.0379(12) Uani 1 1 d . . . . .
H6 H 0.386208 0.608392 0.954749 0.046 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
Bi1 Br3 2.7861(8) . ?
Bi1 Br1 2.9341(8) . ?
Bi1 Br1 3.1150(8) 5_666 ?
Bi1 Br4 2.8566(5) . ?
Bi1 Br4 2.8566(5) 6_565 ?
Bi1 Br2 2.7223(9) . ?
N2 C1AA 1.367(7) . ?
N2 C5 1.335(7) . ?
N2 C2 1.485(7) . ?
N3 C5 1.325(8) . ?
N3 C6 1.375(7) . ?
C0AA C2 1.495(9) . ?
C1AA C6 1.330(8) . ?

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 Bi1 Br1 168.18(3) . . ?
Br3 Bi1 Br1 84.49(2) . 5_666 ?
Br3 Bi1 Br4 92.376(11) . . ?
Br3 Bi1 Br4 92.377(11) . 6_565 ?
Br1 Bi1 Br1 83.69(2) . 5_666 ?
Br4 Bi1 Br1 91.902(12) . 5_666 ?
Br4 Bi1 Br1 91.901(12) 6_565 5_666 ?
Br4 Bi1 Br1 88.018(11) 6_565 . ?
Br4 Bi1 Br1 88.019(11) . . ?
Br4 Bi1 Br4 174.18(2) . 6_565 ?
Br2 Bi1 Br3 98.96(3) . . ?
Br2 Bi1 Br1 176.55(2) . 5_666 ?
Br2 Bi1 Br1 92.86(3) . . ?
Br2 Bi1 Br4 87.970(12) . 6_565 ?
Br2 Bi1 Br4 87.969(12) . . ?
Bi1 Br1 Bi1 96.31(2) . 5_666 ?
C1AA N2 C2 126.5(5) . . ?
C5 N2 C1AA 108.7(5) . . ?
C5 N2 C2 124.8(5) . . ?
C5 N3 C6 108.9(5) . . ?
C6 C1AA N2 107.5(5) . . ?
N3 C5 N2 107.7(5) . . ?
N2 C2 C0AA 112.1(5) . . ?
C1AA C6 N3 107.2(5) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_0619_11_0m
_database_code_depnum_ccdc_archive 'CCDC 2280228'
loop_
_audit_author_name
_audit_author_address
ChengAnHu
;Guangdong University of Technology
China
;
_audit_update_record             
;
2023-07-08 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_audit_creation_method           
;FinalCif V121 by Daniel Kratzert, Freiburg 2023, 
https://dkratzert.de/finalcif.html
;
_audit_creation_date             2023-06-24
_diffrn_source_power             1.5
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.73(3)
 0.27(3)
2. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 Bi4-Br17 \\sim Bi4-Br16 \\sim Bi4-Br18 \\sim Bi4-Br13 \\sim Bi4-Br15 \\sim
Bi4-Br14 \\sim Bi3-Br14 ~
 Bi3-Br15 \\sim Bi3-Br13 \\sim Bi3-Br11 \\sim Bi3-Br10 \\sim Bi3-Br12
 with sigma of 0.02
 Bi02-Bi01 \\sim Bi4-Bi3
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Br17 \\sim Bi3 \\sim Br10 \\sim Br11 \\sim Br12 \\sim Br13 \\sim Br15 \\sim
Br14 \\sim Bi4 \\sim Br16 \\sim Br18: within 2A with sigma of 0.0001 and sigma
for terminal atoms of 0.0002 within 2A
N1 \\sim C00E \\sim C00J \\sim C00G: within 2A with sigma of 0.004 and sigma
for terminal atoms of 0.008 within 2A
C00L \\sim C00F \\sim N2 \\sim C00O: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N3 \\sim C1 \\sim C00H \\sim C00I: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 Br17, Bi3, Br10, Br11, Br12, Br13, Br15, Br14, Bi4, Br16, Br18
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
 C00E, N1, C00J, C00G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
 N3, C1, C00H, C00I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C00O, C00F, N2, C00L
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(Bi3)=Sof(Br10)=Sof(Br12)=Sof(Br11)=Sof(Bi4)=Sof(Br13)=Sof(Br14)=Sof(Br15)=
 Sof(Br17)=Sof(Br18)=Sof(Br16)=1-FVAR(1)
 Sof(Bi01)=Sof(Bi02)=Sof(Br03)=Sof(Br04)=Sof(Br05)=Sof(Br06)=Sof(Br07)=
 Sof(Br08)=Sof(Br09)=Sof(Br0A)=Sof(Br0B)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 N1(H1), N3(H3), N2(H2)
7.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C00E(H00G,H00H,H00I), C00F(H00P,H00Q,H00R), C00G(H00J,H00K,
 H00L), C00H(H00A,H00B,H00C), C00I(H00D,H00E,H00F), C00J(H00M,H00N,H00O),
 C00L(H00S,H00T,H00U), C00O(H00V,H00W,H00X)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C9 H30 Bi2 Br9 N3'
_chemical_formula_moiety         'Bi2 Br9, 3(C3 H10 N)'
_chemical_formula_weight         1317.51
_chemical_melting_point          ?
_chemical_absolute_configuration ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   17.2323(13)
_cell_length_b                   15.0720(13)
_cell_length_c                   11.4500(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.209(3)
_cell_angle_gamma                90
_cell_volume                     2926.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00
_cell_measurement_reflns_used    5866
_cell_measurement_theta_min      2.401
_cell_measurement_theta_max      26.275
_exptl_crystal_description       needle
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.990
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    24.297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0031
_exptl_absorpt_correction_T_max  0.0277
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1698 before and 0.1060 after correction.
The Ratio of minimum to maximum transmission is 0.1119.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   0.247
_shelx_estimated_absorpt_T_max   0.323
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           ?
_diffrn_ambient_temperature      150.00
_diffrn_ambient_environment      ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_radiation_monochromator  ?
_diffrn_measurement_ambient_temperature_device_make ?
_diffrn_radiation_probe          ?
_diffrn_source                   ?
_diffrn_source_type              ?
_diffrn_source_voltage           50.0
_diffrn_source_current           30.0
_diffrn_detector                 ?
_diffrn_detector_type            ?
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device       ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_measurement_specimen_support ?
_diffrn_reflns_number            24531
_diffrn_reflns_av_unetI/netI     0.0877
_diffrn_reflns_av_R_equivalents  0.1190
_diffrn_reflns_theta_min         1.808
_diffrn_reflns_theta_max         24.972
_diffrn_reflns_theta_full        24.972
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_standards_number         0
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_point_group_measured_fraction_full 0.934
_reflns_number_total             4834
_reflns_number_gt                3742
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_max     0.870
_reflns_Friedel_fraction_full    0.870
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_computing_data_collection       ?
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0481P)²+92.3190P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4834
_refine_ls_number_parameters     318
_refine_ls_number_restraints     285
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1398
_refine_ls_wR_factor_gt          0.1280
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.407
_refine_diff_density_min         -1.971
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_Flack   0.27(3)
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.73(3)
2 0.27(3)

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'
Bi Bi -4.1077 10.2566 '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'

_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_
_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
Bi01 Bi 0.47844(14) 0.2497(3) 0.6024(2) 0.0204(6) Uani 0.830(4) 1 d D . P A 1
Bi02 Bi 0.66066(10) 0.25012(13) 0.42136(16) 0.0214(4) Uani 0.830(4) 1 d D . P A
1
Br03 Br 0.4776(5) 0.2888(5) 0.3469(5) 0.0226(16) Uani 0.830(4) 1 d . . P A 1
Br04 Br 0.5843(6) 0.1003(7) 0.5634(13) 0.0245(19) Uani 0.830(4) 1 d . . P A 1
Br05 Br 0.3931(4) 0.4023(3) 0.6255(7) 0.0286(13) Uani 0.830(4) 1 d . . P A 1
Br06 Br 0.3484(4) 0.1413(4) 0.5381(6) 0.0288(13) Uani 0.830(4) 1 d . . P A 1
Br07 Br 0.6270(5) 0.3557(6) 0.6435(9) 0.0239(16) Uani 0.830(4) 1 d . . P A 1
Br08 Br 0.5012(4) 0.2072(5) 0.8415(5) 0.0284(13) Uani 0.830(4) 1 d . . P A 1
Br09 Br 0.6526(4) 0.1656(6) 0.2140(5) 0.0405(17) Uani 0.830(4) 1 d . . P A 1
Br0A Br 0.8023(3) 0.1844(5) 0.5133(6) 0.0408(17) Uani 0.830(4) 1 d . . P A 1
Br0B Br 0.7184(4) 0.3995(4) 0.3451(6) 0.0400(14) Uani 0.830(4) 1 d . . P A 1
Bi3 Bi 0.3132(7) 0.2499(6) 0.7675(13) 0.031(2) Uani 0.170(4) 1 d D . P A 2
C1 C 0.440(2) 0.104(3) 0.081(3) 0.035(8) Uani 1 1 d . U . . .
H1A H 0.484220 0.063961 0.077767 0.053 Uiso 1 1 calc R U . . .
H1B H 0.455224 0.164987 0.067701 0.053 Uiso 1 1 calc R U . . .
H1C H 0.395018 0.086887 0.019808 0.053 Uiso 1 1 calc R U . . .
C00E C 0.792(2) 0.039(3) 0.792(4) 0.047(6) Uani 1 1 d . U . . .
H00G H 0.816338 0.069673 0.731897 0.071 Uiso 1 1 calc R U . . .
H00H H 0.773874 -0.019488 0.763046 0.071 Uiso 1 1 calc R U . . .
H00I H 0.831448 0.032853 0.865097 0.071 Uiso 1 1 calc R U . . .
C00F C 0.648(2) 0.607(3) 0.501(4) 0.052(10) Uani 1 1 d . U . . .
H00P H 0.686419 0.563414 0.484069 0.078 Uiso 1 1 calc R U . . .
H00Q H 0.668621 0.638358 0.574755 0.078 Uiso 1 1 calc R U . . .
H00R H 0.636090 0.649207 0.435658 0.078 Uiso 1 1 calc R U . . .
C00G C 0.740(3) 0.187(2) 0.843(5) 0.048(6) Uani 1 1 d . U . . .
H00J H 0.772841 0.191270 0.922437 0.071 Uiso 1 1 calc R U . . .
H00K H 0.693828 0.225166 0.839333 0.071 Uiso 1 1 calc R U . . .
H00L H 0.771086 0.206296 0.783632 0.071 Uiso 1 1 calc R U . . .
C00H C 0.457(2) 0.031(2) 0.277(3) 0.041(9) Uani 1 1 d . U . . .
H00A H 0.435633 -0.027095 0.250214 0.061 Uiso 1 1 calc R U . . .
H00B H 0.453356 0.039222 0.360890 0.061 Uiso 1 1 calc R U . . .
H00C H 0.512339 0.034704 0.267688 0.061 Uiso 1 1 calc R U . . .
C00I C 0.331(2) 0.091(3) 0.197(4) 0.043(9) Uani 1 1 d . U . . .
H00D H 0.307060 0.139017 0.144535 0.065 Uiso 1 1 calc R U . . .
H00E H 0.315361 0.098206 0.275192 0.065 Uiso 1 1 calc R U . . .
H00F H 0.312829 0.033858 0.163404 0.065 Uiso 1 1 calc R U . . .
C00J C 0.688(2) 0.056(3) 0.912(4) 0.047(6) Uani 1 1 d . U . . .
H00M H 0.657297 0.004013 0.880283 0.071 Uiso 1 1 calc R U . . .
H00N H 0.654315 0.096852 0.947169 0.071 Uiso 1 1 calc R U . . .
H00O H 0.732476 0.037457 0.972427 0.071 Uiso 1 1 calc R U . . .
N1 N 0.716(2) 0.0987(19) 0.821(3) 0.050(5) Uani 1 1 d . U . . .
H1 H 0.673765 0.097751 0.748739 0.060 Uiso 1 1 calc R U . . .
C00L C 0.520(3) 0.531(3) 0.405(4) 0.053(10) Uani 1 1 d . U . . .
H00S H 0.485647 0.580632 0.374527 0.079 Uiso 1 1 calc R U . . .
H00T H 0.487878 0.479236 0.416469 0.079 Uiso 1 1 calc R U . . .
H00U H 0.554616 0.516504 0.348500 0.079 Uiso 1 1 calc R U . . .
N3 N 0.414(2) 0.096(3) 0.211(3) 0.052(7) Uani 1 1 d . U . . .
H3 H 0.430290 0.153712 0.252091 0.063 Uiso 1 1 calc R U . . .
N2 N 0.567(3) 0.556(3) 0.516(4) 0.060(7) Uani 1 1 d . U . . .
H2 H 0.582737 0.499610 0.561344 0.072 Uiso 1 1 calc R U . . .
C00O C 0.531(3) 0.610(3) 0.589(4) 0.058(10) Uani 1 1 d . U . . .
H00V H 0.566632 0.620492 0.664081 0.087 Uiso 1 1 calc R U . . .
H00W H 0.482605 0.580969 0.605088 0.087 Uiso 1 1 calc R U . . .
H00X H 0.516621 0.666787 0.549084 0.087 Uiso 1 1 calc R U . . .
Br10 Br 0.2515(17) 0.0942(16) 0.851(3) 0.031(4) Uani 0.170(4) 1 d D . P A 2
Br12 Br 0.320(2) 0.334(2) 0.990(2) 0.033(4) Uani 0.170(4) 1 d D . P A 2
Br11 Br 0.1628(16) 0.320(2) 0.678(3) 0.031(4) Uani 0.170(4) 1 d D . P A 2
Bi4 Bi 0.4968(10) 0.2523(17) 0.5920(19) 0.027(3) Uani 0.170(4) 1 d D . P A 2
Br13 Br 0.3502(19) 0.158(2) 0.563(3) 0.030(4) Uani 0.170(4) 1 d D . P A 2
Br14 Br 0.4786(13) 0.207(3) 0.829(3) 0.030(4) Uani 0.170(4) 1 d D . P A 2
Br15 Br 0.383(2) 0.3817(18) 0.635(4) 0.030(4) Uani 0.170(4) 1 d D . P A 2
Br17 Br 0.627(3) 0.370(3) 0.658(6) 0.029(5) Uani 0.170(4) 1 d D . P A 2
Br18 Br 0.594(4) 0.104(3) 0.559(7) 0.029(5) Uani 0.170(4) 1 d D . P A 2
Br16 Br 0.483(3) 0.309(3) 0.352(3) 0.031(5) Uani 0.170(4) 1 d D . P A 2


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
Bi01 Br03 2.981(6) . ?
Bi01 Br04 2.980(7) . ?
Bi01 Br05 2.769(6) . ?
Bi01 Br06 2.765(6) . ?
Bi01 Br07 2.984(7) . ?
Bi01 Br08 2.771(6) . ?
Bi02 Br03 3.172(10) . ?
Bi02 Br04 3.200(12) . ?
Bi02 Br07 3.140(8) . ?
Bi02 Br09 2.677(6) . ?
Bi02 Br0A 2.671(6) . ?
Bi02 Br0B 2.670(6) . ?
Bi3 Br10 2.81(2) . ?
Bi3 Br12 2.83(2) . ?
Bi3 Br11 2.82(2) . ?
Bi3 Br13 2.89(2) . ?
Bi3 Br14 2.89(2) . ?
Bi3 Br15 2.89(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 N3 1.62(5) . ?
C00E H00G 0.9800 . ?
C00E H00H 0.9800 . ?
C00E H00I 0.9800 . ?
C00E N1 1.67(5) . ?
C00F H00P 0.9800 . ?
C00F H00Q 0.9800 . ?
C00F H00R 0.9800 . ?
C00F N2 1.62(6) . ?
C00G H00J 0.9800 . ?
C00G H00K 0.9800 . ?
C00G H00L 0.9800 . ?
C00G N1 1.40(4) . ?
C00H H00A 0.9800 . ?
C00H H00B 0.9800 . ?
C00H H00C 0.9800 . ?
C00H N3 1.37(5) . ?
C00I H00D 0.9800 . ?
C00I H00E 0.9800 . ?
C00I H00F 0.9800 . ?
C00I N3 1.42(5) . ?
C00J H00M 0.9800 . ?
C00J H00N 0.9800 . ?
C00J H00O 0.9800 . ?
C00J N1 1.38(6) . ?
N1 H1 1.0000 . ?
C00L H00S 0.9800 . ?
C00L H00T 0.9800 . ?
C00L H00U 0.9800 . ?
C00L N2 1.43(5) . ?
N3 H3 1.0000 . ?
N2 H2 1.0000 . ?
N2 C00O 1.40(6) . ?
C00O H00V 0.9800 . ?
C00O H00W 0.9800 . ?
C00O H00X 0.9800 . ?
Bi4 Br13 2.87(2) . ?
Bi4 Br14 2.87(2) . ?
Bi4 Br15 2.87(2) . ?
Bi4 Br17 2.86(2) . ?
Bi4 Br18 2.86(2) . ?
Bi4 Br16 2.85(2) . ?

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
Br03 Bi01 Br07 84.5(3) . . ?
Br04 Bi01 Br03 84.2(3) . . ?
Br04 Bi01 Br07 84.1(3) . . ?
Br05 Bi01 Br03 91.1(3) . . ?
Br05 Bi01 Br04 172.6(3) . . ?
Br05 Bi01 Br07 89.7(3) . . ?
Br05 Bi01 Br08 94.7(3) . . ?
Br06 Bi01 Br03 89.6(3) . . ?
Br06 Bi01 Br04 90.1(3) . . ?
Br06 Bi01 Br05 95.6(2) . . ?
Br06 Bi01 Br07 172.1(3) . . ?
Br06 Bi01 Br08 95.3(2) . . ?
Br08 Bi01 Br03 172.0(3) . . ?
Br08 Bi01 Br04 89.4(3) . . ?
Br08 Bi01 Br07 90.0(3) . . ?
Br03 Bi02 Br04 77.7(2) . . ?
Br07 Bi02 Br03 78.9(2) . . ?
Br07 Bi02 Br04 78.1(3) . . ?
Br09 Bi02 Br03 87.5(2) . . ?
Br09 Bi02 Br04 98.8(3) . . ?
Br09 Bi02 Br07 166.4(3) . . ?
Br0A Bi02 Br03 165.85(19) . . ?
Br0A Bi02 Br04 88.2(3) . . ?
Br0A Bi02 Br07 98.9(3) . . ?
Br0A Bi02 Br09 94.2(2) . . ?
Br0B Bi02 Br03 99.7(2) . . ?
Br0B Bi02 Br04 166.5(2) . . ?
Br0B Bi02 Br07 88.3(2) . . ?
Br0B Bi02 Br09 94.3(2) . . ?
Br0B Bi02 Br0A 94.2(2) . . ?
Bi01 Br03 Bi02 82.4(2) . . ?
Bi01 Br04 Bi02 82.0(3) . . ?
Bi01 Br07 Bi02 82.95(16) . . ?
Br10 Bi3 Br12 91.5(10) . . ?
Br10 Bi3 Br11 93.2(11) . . ?
Br10 Bi3 Br13 91.4(11) . . ?
Br10 Bi3 Br14 98.5(11) . . ?
Br10 Bi3 Br15 166.0(12) . . ?
Br12 Bi3 Br13 164.8(12) . . ?
Br12 Bi3 Br14 89.9(12) . . ?
Br12 Bi3 Br15 102.0(12) . . ?
Br11 Bi3 Br12 92.7(11) . . ?
Br11 Bi3 Br13 102.0(12) . . ?
Br11 Bi3 Br14 167.9(12) . . ?
Br11 Bi3 Br15 89.7(12) . . ?
Br14 Bi3 Br13 74.9(11) . . ?
Br14 Bi3 Br15 78.3(11) . . ?
Br15 Bi3 Br13 74.6(11) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N3 C1 H1A 109.5 . . ?
N3 C1 H1B 109.5 . . ?
N3 C1 H1C 109.5 . . ?
H00G C00E H00H 109.5 . . ?
H00G C00E H00I 109.5 . . ?
H00H C00E H00I 109.5 . . ?
N1 C00E H00G 109.5 . . ?
N1 C00E H00H 109.5 . . ?
N1 C00E H00I 109.5 . . ?
H00P C00F H00Q 109.5 . . ?
H00P C00F H00R 109.5 . . ?
H00Q C00F H00R 109.5 . . ?
N2 C00F H00P 109.5 . . ?
N2 C00F H00Q 109.5 . . ?
N2 C00F H00R 109.5 . . ?
H00J C00G H00K 109.5 . . ?
H00J C00G H00L 109.5 . . ?
H00K C00G H00L 109.5 . . ?
N1 C00G H00J 109.5 . . ?
N1 C00G H00K 109.5 . . ?
N1 C00G H00L 109.5 . . ?
H00A C00H H00B 109.5 . . ?
H00A C00H H00C 109.5 . . ?
H00B C00H H00C 109.5 . . ?
N3 C00H H00A 109.5 . . ?
N3 C00H H00B 109.5 . . ?
N3 C00H H00C 109.5 . . ?
H00D C00I H00E 109.5 . . ?
H00D C00I H00F 109.5 . . ?
H00E C00I H00F 109.5 . . ?
N3 C00I H00D 109.5 . . ?
N3 C00I H00E 109.5 . . ?
N3 C00I H00F 109.5 . . ?
H00M C00J H00N 109.5 . . ?
H00M C00J H00O 109.5 . . ?
H00N C00J H00O 109.5 . . ?
N1 C00J H00M 109.5 . . ?
N1 C00J H00N 109.5 . . ?
N1 C00J H00O 109.5 . . ?
C00E N1 H1 108.3 . . ?
C00G N1 C00E 109(3) . . ?
C00G N1 H1 108.3 . . ?
C00J N1 C00E 107(3) . . ?
C00J N1 C00G 116(4) . . ?
C00J N1 H1 108.3 . . ?
H00S C00L H00T 109.5 . . ?
H00S C00L H00U 109.5 . . ?
H00T C00L H00U 109.5 . . ?
N2 C00L H00S 109.5 . . ?
N2 C00L H00T 109.5 . . ?
N2 C00L H00U 109.5 . . ?
C1 N3 H3 106.3 . . ?
C00H N3 C1 111(3) . . ?
C00H N3 C00I 117(4) . . ?
C00H N3 H3 106.3 . . ?
C00I N3 C1 110(3) . . ?
C00I N3 H3 106.3 . . ?
C00F N2 H2 107.4 . . ?
C00L N2 C00F 113(4) . . ?
C00L N2 H2 107.4 . . ?
C00O N2 C00F 106(3) . . ?
C00O N2 C00L 116(4) . . ?
C00O N2 H2 107.4 . . ?
N2 C00O H00V 109.5 . . ?
N2 C00O H00W 109.5 . . ?
N2 C00O H00X 109.5 . . ?
H00V C00O H00W 109.5 . . ?
H00V C00O H00X 109.5 . . ?
H00W C00O H00X 109.5 . . ?
Br13 Bi4 Br15 75.1(11) . . ?
Br14 Bi4 Br13 75.4(11) . . ?
Br14 Bi4 Br15 78.8(11) . . ?
Br17 Bi4 Br13 166.8(17) . . ?
Br17 Bi4 Br14 96.3(17) . . ?
Br17 Bi4 Br15 93.4(16) . . ?
Br17 Bi4 Br18 94(2) . . ?
Br18 Bi4 Br13 97.0(19) . . ?
Br18 Bi4 Br14 96.1(19) . . ?
Br18 Bi4 Br15 171.4(17) . . ?
Br16 Bi4 Br13 96.8(14) . . ?
Br16 Bi4 Br14 168.6(14) . . ?
Br16 Bi4 Br15 91.2(15) . . ?
Br16 Bi4 Br17 89.8(16) . . ?
Br16 Bi4 Br18 93.1(19) . . ?
Bi4 Br13 Bi3 89.1(7) . . ?
Bi4 Br14 Bi3 89.1(7) . . ?
Bi4 Br15 Bi3 89.1(7) . . ?


