# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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_P212121
_database_code_depnum_ccdc_archive 'CCDC 2288194'
loop_
_audit_author_name
_audit_author_address
'Ji-Xing Gao'
;Fuyang Normal University
China
;
_audit_update_record             
;
2023-08-11 deposited with the CCDC.	2023-10-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Bi Cl5, C6 H18 N2'
_chemical_formula_sum            'C6 H18 Bi Cl5 N2'
_chemical_formula_weight         504.45

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'
N N 0.0061 0.0033 '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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   14.9168(9)
_cell_length_b                   13.1553(7)
_cell_length_c                   7.6806(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1507.20(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    4889
_cell_measurement_theta_min      2.7000
_cell_measurement_theta_max      27.9440

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.223
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    12.556
_shelx_estimated_absorpt_T_min   0.339
_shelx_estimated_absorpt_T_max   0.367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.274
_exptl_absorpt_correction_T_max  0.285
_exptl_absorpt_process_details   'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'four-circle diffractometer'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7799
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.731
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_full        25.023
_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 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2657
_reflns_number_gt                2252
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.719
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0435P)²+136.8019P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(3)
_chemical_absolute_configuration rd
_refine_ls_number_reflns         2657
_refine_ls_number_parameters     128
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0853
_refine_ls_wR_factor_ref         0.2035
_refine_ls_wR_factor_gt          0.1978
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

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 0.85389(3) 0.60896(3) 0.01139(7) 0.04435(10) Uani 1 1 d . . . . .
Cl1 Cl 0.9651(2) 0.4527(2) 0.0093(11) 0.0913(16) Uani 1 1 d . . . . .
Cl2 Cl 0.9327(3) 0.7095(3) 0.2538(7) 0.0864(16) Uani 1 1 d . . . . .
Cl3 Cl 0.7483(5) 0.5030(5) 0.2661(8) 0.0789(12) Uani 1 1 d . . . . .
Cl4 Cl 0.7239(2) 0.7541(2) 0.0025(9) 0.0703(12) Uani 1 1 d . . . . .
Cl5 Cl 0.9391(3) 0.7040(3) -0.2333(7) 0.0945(16) Uani 1 1 d . . . . .
N1 N 0.2542(6) 0.2164(9) 0.006(3) 0.127(6) Uani 1 1 d D U . . .
H1A H 0.2725 0.1514 -0.0033 0.191 Uiso 1 1 d R U . . .
H1B H 0.2168 0.2310 -0.0828 0.191 Uiso 1 1 d R U . . .
H1C H 0.2254 0.2252 0.1076 0.191 Uiso 1 1 d R U . . .
N2 N 0.5465(7) 0.6268(6) -0.0658(14) 0.081(5) Uani 1 1 d D U . . .
H2A H 0.6024 0.6432 -0.0315 0.122 Uiso 1 1 d R U . . .
H2B H 0.5098 0.6802 -0.0488 0.122 Uiso 1 1 d R U . . .
H2C H 0.5471 0.6105 -0.1796 0.122 Uiso 1 1 d R U . . .
C1 C 0.3369(5) 0.2654(4) 0.0543(18) 0.151(6) Uani 1 1 d D U . . .
H1D H 0.3767 0.2460 0.1467 0.181 Uiso 1 1 d R U . . .
H1E H 0.3676 0.2521 -0.0532 0.181 Uiso 1 1 d DR U . . .
C2 C 0.3027(4) 0.3788(4) -0.0018(17) 0.110(3) Uani 1 1 d D U . . .
H2 H 0.3081 0.3804 -0.1316 0.132 Uiso 1 1 d DR U . . .
C3 C 0.3680(4) 0.4532(5) 0.0646(12) 0.120(3) Uani 1 1 d D U . . .
H3A H 0.3424 0.4935 0.1562 0.144 Uiso 1 1 d DR U . . .
H3B H 0.4126 0.4105 0.1173 0.144 Uiso 1 1 d R U . . .
C4 C 0.4266(5) 0.5189(9) -0.0307(16) 0.108(3) Uani 1 1 d D U . . .
H4A H 0.4300 0.4889 -0.1444 0.130 Uiso 1 1 d R U . . .
H4B H 0.3931 0.5809 -0.0401 0.130 Uiso 1 1 d R U . . .
C5 C 0.5148(6) 0.5436(7) 0.0396(15) 0.090(5) Uani 1 1 d D U . . .
H5A H 0.5535 0.4861 0.0226 0.108 Uiso 1 1 d R U . . .
H5B H 0.5139 0.5601 0.1613 0.108 Uiso 1 1 d R U . . .
C6 C 0.2222(4) 0.4348(7) 0.0303(16) 0.079(5) Uani 1 1 d D U . . .
H6A H 0.2130 0.4323 0.1565 0.118 Uiso 1 1 d DR U . . .
H6B H 0.1707 0.4038 -0.0286 0.118 Uiso 1 1 d R U . . .
H6C H 0.2283 0.5057 -0.0070 0.118 Uiso 1 1 d DR 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
Bi1 Cl2 2.569(5) . ?
Bi1 Cl5 2.591(5) . ?
Bi1 Cl1 2.641(3) . ?
Bi1 Cl4 2.722(3) . ?
Bi1 Cl3 2.836(6) 2_664 ?
Bi1 Cl3 2.872(6) . ?
Cl3 Bi1 2.836(6) 2_665 ?
N1 C1 1.442(12) . ?
N2 C5 1.441(13) . ?
C1 C2 1.634(8) . ?
C2 C6 1.430(9) . ?
C2 C3 1.472(9) . ?
C3 C4 1.431(12) . ?
C4 C5 1.458(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Bi1 Cl5 93.01(16) . . ?
Cl2 Bi1 Cl1 96.75(17) . . ?
Cl5 Bi1 Cl1 93.60(17) . . ?
Cl2 Bi1 Cl4 89.02(15) . . ?
Cl5 Bi1 Cl4 89.58(15) . . ?
Cl1 Bi1 Cl4 173.25(11) . . ?
Cl2 Bi1 Cl3 174.24(18) . 2_664 ?
Cl5 Bi1 Cl3 91.88(17) . 2_664 ?
Cl1 Bi1 Cl3 85.97(19) . 2_664 ?
Cl4 Bi1 Cl3 87.98(18) . 2_664 ?
Cl2 Bi1 Cl3 90.40(17) . . ?
Cl5 Bi1 Cl3 175.85(18) . . ?
Cl1 Bi1 Cl3 88.33(19) . . ?
Cl4 Bi1 Cl3 88.12(18) . . ?
Cl3 Bi1 Cl3 84.588(12) 2_664 . ?
Bi1 Cl3 Bi1 177.7(3) 2_665 . ?
N1 C1 C2 94.2(7) . . ?
C6 C2 C3 98.8(6) . . ?
C6 C2 C1 133.3(8) . . ?
C3 C2 C1 108.0(6) . . ?
C4 C3 C2 128.9(9) . . ?
C3 C4 C5 119.8(10) . . ?
N2 C5 C4 104.9(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C6 47.0(17) . . . . ?
N1 C1 C2 C3 169.0(11) . . . . ?
C6 C2 C3 C4 -104.7(10) . . . . ?
C1 C2 C3 C4 114.0(10) . . . . ?
C2 C3 C4 C5 -146.2(9) . . . . ?
C3 C4 C5 N2 -167.4(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl3 0.90 2.69 3.310(16) 127.1 3_645
N1 H1A Cl3 0.90 2.89 3.563(16) 133.2 4_455
N1 H1B Cl5 0.90 2.74 3.566(15) 152.4 3_644
N1 H1C Cl2 0.90 2.60 3.345(15) 141.2 3_645
N2 H2A Cl4 0.90 2.34 3.176(10) 154.0 .
N2 H2B Cl2 0.90 2.43 3.099(11) 131.2 4_465
N2 H2B Cl5 0.90 2.85 3.577(11) 138.8 4_465
N2 H2C Cl1 0.90 2.54 3.432(14) 172.9 2_664
C5 H5B Cl1 0.96 2.70 3.620(14) 161.8 2_665

_refine_diff_density_max         5.627
_refine_diff_density_min         -2.131
_refine_diff_density_rms         0.315



####################################################################### 
# 
# 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_Pna21
_database_code_depnum_ccdc_archive 'CCDC 2299482'
loop_
_audit_author_name
_audit_author_address
'Ji-Xing Gao'
;Fuyang Normal University
China
;
_audit_update_record             
;
2023-10-05 deposited with the CCDC.	2023-10-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Bi Cl5, C6 H18 N2'
_chemical_formula_sum            'C6 H18 Bi Cl5 N2'
_chemical_formula_weight         504.45

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'
N N 0.0061 0.0033 '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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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                   14.9838(5)
_cell_length_b                   13.2925(4)
_cell_length_c                   7.7386(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1541.31(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    5307
_cell_measurement_theta_min      3.0250
_cell_measurement_theta_max      30.0920

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.174
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    12.278
_shelx_estimated_absorpt_T_min   0.345
_shelx_estimated_absorpt_T_max   0.373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.269
_exptl_absorpt_correction_T_max  0.293
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'four-circle diffractometer'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7830
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.719
_diffrn_reflns_theta_max         26.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3359
_reflns_number_gt                2747
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0293P)²+10.9776P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3359
_refine_ls_number_parameters     128
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.0931
_refine_ls_wR_factor_gt          0.0909
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.10348(2) 0.10839(2) 0.2335(3) 0.04513(8) Uani 1 1 d . . . . .
Cl1 Cl 0.2137(2) -0.0474(2) 0.2221(11) 0.0865(10) Uani 1 1 d . . . . .
Cl2 Cl 0.1792(3) 0.2056(3) -0.0184(6) 0.0937(15) Uani 1 1 d . . . . .
Cl3 Cl -0.0090(3) 0.0060(5) -0.0315(6) 0.0792(9) Uani 1 1 d . . . . .
Cl4 Cl -0.0275(2) 0.2502(2) 0.2418(10) 0.0845(9) Uani 1 1 d . . . . .
Cl5 Cl 0.1888(3) 0.2027(3) 0.4676(5) 0.0903(12) Uani 1 1 d . . . . .
N1 N 0.4963(10) 0.2871(8) 0.6892(17) 0.105(5) Uani 1 1 d D U . . .
H1A H 0.4835 0.3513 0.7171 0.157 Uiso 1 1 d R U . . .
H1B H 0.5505 0.2710 0.7309 0.157 Uiso 1 1 d R U . . .
H1C H 0.4963 0.2803 0.5735 0.157 Uiso 1 1 d R U . . .
N2 N 0.2034(9) -0.1260(9) 0.6528(16) 0.091(4) Uani 1 1 d D U . . .
H2A H 0.1439 -0.1318 0.6648 0.137 Uiso 1 1 d R U . . .
H2B H 0.2166 -0.1121 0.5418 0.137 Uiso 1 1 d R U . . .
H2C H 0.2297 -0.1841 0.6837 0.137 Uiso 1 1 d R U . . .
C1 C 0.4305(10) 0.2225(9) 0.765(2) 0.095(3) Uani 1 1 d D U . . .
H1D H 0.3729 0.2421 0.7222 0.114 Uiso 1 1 d R U . . .
H1E H 0.4301 0.2322 0.8880 0.114 Uiso 1 1 d R U . . .
C2 C 0.4478(8) 0.1186(8) 0.710(3) 0.097(3) Uani 1 1 d D U . . .
H2D H 0.4686 0.1330 0.5956 0.116 Uiso 1 1 d DR U . . .
C3 C 0.3592(9) 0.0602(10) 0.666(2) 0.106(3) Uani 1 1 d D U . . .
H3A H 0.3753 0.0315 0.5568 0.127 Uiso 1 1 d DR U . . .
H3B H 0.3137 0.1095 0.6446 0.127 Uiso 1 1 d R U . . .
C4 C 0.3284(8) -0.0171(10) 0.771(2) 0.095(3) Uani 1 1 d D U . . .
H4A H 0.3397 0.0005 0.8894 0.114 Uiso 1 1 d R U . . .
H4B H 0.3623 -0.0770 0.7483 0.114 Uiso 1 1 d R U . . .
C5 C 0.2356(8) -0.0482(10) 0.762(2) 0.097(4) Uani 1 1 d D U . . .
H5A H 0.2172 -0.0641 0.8779 0.116 Uiso 1 1 d R U . . .
H5B H 0.2034 0.0112 0.7293 0.116 Uiso 1 1 d R U . . .
C6 C 0.5261(9) 0.0662(9) 0.7747(14) 0.070(4) Uani 1 1 d D . . . .
H6A H 0.5231 -0.0036 0.7434 0.105 Uiso 1 1 d R U . . .
H6B H 0.5738 0.0980 0.7124 0.105 Uiso 1 1 d R U . . .
H6C H 0.5369 0.0719 0.8966 0.105 Uiso 1 1 d 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
Bi1 Cl5 2.548(4) . ?
Bi1 Cl2 2.599(5) . ?
Bi1 Cl1 2.650(3) . ?
Bi1 Cl4 2.722(3) . ?
Bi1 Cl3 2.761(5) 2 ?
Bi1 Cl3 2.983(5) . ?
Cl3 Bi1 2.761(5) 2_554 ?
N1 C1 1.434(16) . ?
N2 C5 1.422(16) . ?
C1 C2 1.468(15) . ?
C2 C6 1.452(15) . ?
C2 C3 1.576(14) . ?
C3 C4 1.388(16) . ?
C4 C5 1.452(15) . ?

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
Cl5 Bi1 Cl2 93.99(12) . . ?
Cl5 Bi1 Cl1 95.48(18) . . ?
Cl2 Bi1 Cl1 95.26(18) . . ?
Cl5 Bi1 Cl4 90.24(16) . . ?
Cl2 Bi1 Cl4 89.31(18) . . ?
Cl1 Bi1 Cl4 172.40(10) . . ?
Cl5 Bi1 Cl3 93.43(16) . 2 ?
Cl2 Bi1 Cl3 172.52(17) . 2 ?
Cl1 Bi1 Cl3 84.89(17) . 2 ?
Cl4 Bi1 Cl3 89.79(17) . 2 ?
Cl5 Bi1 Cl3 175.63(15) . . ?
Cl2 Bi1 Cl3 87.59(16) . . ?
Cl1 Bi1 Cl3 88.43(18) . . ?
Cl4 Bi1 Cl3 85.69(16) . . ?
Cl3 Bi1 Cl3 84.943(18) 2 . ?
Bi1 Cl3 Bi1 173.6(2) 2_554 . ?
N1 C1 C2 108.9(13) . . ?
C6 C2 C1 119.7(13) . . ?
C6 C2 C3 121.3(10) . . ?
C1 C2 C3 112.1(11) . . ?
C4 C3 C2 121.2(13) . . ?
C3 C4 C5 120.0(13) . . ?
N2 C5 C4 124.0(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C6 70(2) . . . . ?
N1 C1 C2 C3 -139.3(15) . . . . ?
C6 C2 C3 C4 40(2) . . . . ?
C1 C2 C3 C4 -110.2(18) . . . . ?
C2 C3 C4 C5 160.5(15) . . . . ?
C3 C4 C5 N2 91.8(19) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5 H5A Cl1 0.96 2.67 3.57(2) 156.3 1_556
C1 H1E Cl4 0.96 2.82 3.759(19) 166.3 3_556
N2 H2C Cl5 0.90 2.93 3.705(13) 145.4 4_545
N2 H2C Cl2 0.90 2.54 3.140(14) 124.5 4_545
N2 H2B Cl1 0.90 2.62 3.496(15) 164.7 .
N2 H2A Cl4 0.90 2.42 3.186(13) 142.5 2
N1 H1C Cl4 0.90 2.62 3.516(15) 171.6 3
N1 H1B Cl5 0.90 2.93 3.358(15) 111.1 3
N1 H1B Cl2 0.90 2.75 3.555(15) 149.0 3_556
N1 H1A Cl3 0.90 2.84 3.379(13) 119.6 4
N1 H1A Cl3 0.90 2.72 3.498(13) 145.4 3_556
N1 H1A Cl3 0.90 2.72 3.498(13) 145.4 3_556
N1 H1A Cl3 0.90 2.84 3.379(13) 119.6 4
N1 H1B Cl2 0.90 2.75 3.555(15) 149.0 3_556
N1 H1B Cl5 0.90 2.93 3.358(15) 111.1 3
N1 H1C Cl4 0.90 2.62 3.516(15) 171.6 3
N2 H2A Cl4 0.90 2.42 3.186(13) 142.5 2
N2 H2B Cl1 0.90 2.62 3.496(15) 164.7 .
N2 H2C Cl2 0.90 2.54 3.140(14) 124.5 4_545
N2 H2C Cl5 0.90 2.93 3.705(13) 145.4 4_545
C1 H1E Cl4 0.96 2.82 3.759(19) 166.3 3_556
C5 H5A Cl1 0.96 2.67 3.57(2) 156.3 1_556

_refine_diff_density_max         1.510
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.139



####################################################################### 
# 
# 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_Pnma
_database_code_depnum_ccdc_archive 'CCDC 2288196'
loop_
_audit_author_name
_audit_author_address
'Ji-Xing Gao'
;Fuyang Normal University
China
;
_audit_update_record             
;
2023-08-11 deposited with the CCDC.	2023-10-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Bi Br5, 2(C3 H9 N)'
_chemical_formula_sum            'C6 H18 Bi Br5 N2'
_chemical_formula_weight         726.70

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'
N N 0.0061 0.0033 '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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   15.2463(11)
_cell_length_b                   7.9575(6)
_cell_length_c                   13.4076(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1626.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    3164
_cell_measurement_theta_min      2.9640
_cell_measurement_theta_max      29.0530

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.968
_exptl_crystal_F_000             1304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    23.095
_shelx_estimated_absorpt_T_min   0.085
_shelx_estimated_absorpt_T_max   0.091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_T_max  0.011
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5784
_diffrn_reflns_av_unetI/netI     0.1938
_diffrn_reflns_av_R_equivalents  0.3666
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.672
_diffrn_reflns_theta_max         25.230
_diffrn_reflns_theta_full        25.230
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1591
_reflns_number_gt                1061
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'PRPKAPPA (Ferguson, 1999)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.7100P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1584
_refine_ls_number_parameters     90
_refine_ls_number_restraints     111
_refine_ls_R_factor_all          0.2780
_refine_ls_R_factor_gt           0.2489
_refine_ls_wR_factor_ref         0.6630
_refine_ls_wR_factor_gt          0.6235
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.081
_refine_ls_shift/su_mean         0.003

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 0.10535(7) 0.7500 0.11713(8) 0.0492(4) Uani 1 2 d S T P . .
Br1 Br 0.0000 1.0000 0.0000 0.1214(16) Uani 1 2 d S . P . .
Br2 Br 0.2189(3) 0.7500 -0.0481(3) 0.0803(13) Uani 1 2 d S T P . .
Br3 Br -0.0356(3) 0.7500 0.2589(3) 0.0815(14) Uani 1 2 d S T P . .
Br4 Br 0.1885(2) 0.9996(4) 0.2153(2) 0.0894(10) Uani 1 1 d . . . . .
C1 C 0.9294(10) 0.2500 0.2881(6) 0.1159(18) Uani 1 2 d DS TU P . .
H1A H 0.8921 0.3491 0.2740 0.139 Uiso 0.5 1 calc R U P . .
H1B H 0.8921 0.1509 0.2740 0.139 Uiso 0.5 1 calc R U P . .
C2 C 0.9389(6) 0.2500 0.3954(7) 0.1162(15) Uani 1 2 d DS TU P . .
H2A H 0.9257 0.3647 0.4076 0.139 Uiso 0.5 1 d R U P . .
C3 C 0.8966(8) 0.1327(14) 0.4626(12) 0.1161(17) Uani 0.5 1 d D U P . .
H3A H 0.9198 0.0361 0.4946 0.139 Uiso 0.5 1 d R U P . .
H3B H 0.8561 0.0923 0.4144 0.139 Uiso 0.5 1 d R U P . .
C4 C 0.8273(6) 0.2500 0.4884(14) 0.1160(18) Uani 1 2 d DS TU P . .
H4A H 0.8003 0.2734 0.4252 0.139 Uiso 0.5 1 d R U P . .
H4B H 0.8547 0.3539 0.5070 0.139 Uiso 0.5 1 d R U P . .
C5 C 0.7438(6) 0.2500 0.5407(14) 0.1160(19) Uani 1 2 d DS TU P . .
H5A H 0.7100 0.3483 0.5251 0.139 Uiso 0.5 1 d R U P . .
H5B H 0.7649 0.2639 0.6076 0.139 Uiso 0.5 1 d R U P . .
C6 C 1.0331(7) 0.2500 0.406(4) 0.116(2) Uani 1 2 d DS TU P . .
H6A H 1.0756 0.2974 0.3626 0.174 Uiso 0.5 1 d R U P . .
H6B H 1.0301 0.3146 0.4654 0.174 Uiso 0.5 1 d R U P . .
H6C H 1.0494 0.1380 0.4219 0.174 Uiso 0.5 1 d R U P . .
N1 N 0.9937(10) 0.2500 0.2084(10) 0.116(3) Uani 1 2 d DS TU P . .
H1C H 1.0222 0.1495 0.2074 0.173 Uiso 0.5 1 calc R U P . .
H1D H 1.0331 0.3341 0.2188 0.173 Uiso 0.5 1 calc R U P . .
H1E H 0.9661 0.2663 0.1490 0.173 Uiso 0.5 1 calc R U P . .
N2 N 0.6680(9) 0.147(2) 0.563(3) 0.116(3) Uani 0.5 1 d D U P . .
H2B H 0.6531 0.1591 0.6279 0.174 Uiso 0.5 1 calc R U P . .
H2C H 0.6809 0.0372 0.5501 0.174 Uiso 0.5 1 calc R U P . .
H2D H 0.6222 0.1795 0.5235 0.174 Uiso 0.5 1 calc R U P . .


_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 Br4 2.699(3) 7_575 ?
Bi1 Br4 2.699(3) . ?
Bi1 Br2 2.812(4) . ?
Bi1 Br3 2.869(4) . ?
Bi1 Br1 3.0006(8) 3_545 ?
Bi1 Br1 3.0006(8) . ?
Br1 Bi1 3.0007(8) 5_575 ?
C1 C2 1.445(11) . ?
C1 N1 1.450(15) . ?
C2 C6 1.443(13) . ?
C2 C3 1.448(13) 7_565 ?
C2 C3 1.448(13) . ?
C3 C4 1.453(13) . ?
C3 C3 1.87(2) 7_565 ?
C4 C3 1.453(13) 7_565 ?
C4 C5 1.453(14) . ?
C5 N2 1.447(14) . ?
C5 N2 1.448(14) 7_565 ?
N2 N2 1.64(4) 7_565 ?

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
Br4 Bi1 Br4 94.75(14) 7_575 . ?
Br4 Bi1 Br2 95.45(9) 7_575 . ?
Br4 Bi1 Br2 95.45(9) . . ?
Br4 Bi1 Br3 91.65(9) 7_575 . ?
Br4 Bi1 Br3 91.66(9) . . ?
Br2 Bi1 Br3 169.49(13) . . ?
Br4 Bi1 Br1 91.08(7) 7_575 3_545 ?
Br4 Bi1 Br1 174.03(8) . 3_545 ?
Br2 Bi1 Br1 85.25(7) . 3_545 ?
Br3 Bi1 Br1 86.89(6) . 3_545 ?
Br4 Bi1 Br1 174.03(8) 7_575 . ?
Br4 Bi1 Br1 91.08(7) . . ?
Br2 Bi1 Br1 85.25(7) . . ?
Br3 Bi1 Br1 86.89(6) . . ?
Br1 Bi1 Br1 83.06(3) 3_545 . ?
Bi1 Br1 Bi1 180.0 . 5_575 ?
C2 C1 N1 131.7(13) . . ?
C6 C2 C1 101(2) . . ?
C6 C2 C3 112.4(17) . 7_565 ?
C1 C2 C3 125.0(9) . 7_565 ?
C6 C2 C3 112.4(17) . . ?
C1 C2 C3 125.0(9) . . ?
C3 C2 C3 80.2(11) 7_565 . ?
C2 C3 C4 93.4(9) . . ?
C2 C3 C3 49.9(6) . 7_565 ?
C4 C3 C3 50.0(5) . 7_565 ?
C3 C4 C3 79.9(11) 7_565 . ?
C3 C4 C5 138.9(7) 7_565 . ?
C3 C4 C5 138.9(7) . . ?
N2 C5 N2 69.1(16) . 7_565 ?
N2 C5 C4 142.9(13) . . ?
N2 C5 C4 142.9(13) 7_565 . ?
C5 N2 N2 55.5(8) . 7_565 ?

_refine_diff_density_max         8.248
_refine_diff_density_min         -10.055
_refine_diff_density_rms         0.994

# start Validation Reply Form

_vrf_RINTA01_Pnma                
;
PROBLEM: The value of Rint is greater than 0.25  Rint given   0.367   
RESPONSE: The overall quality of crystal was effected by the current temperature.
;

_vrf_PLAT020_Pnma                
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.367 Report   
RESPONSE: The overall quality of crystal was effected by the current temperature.
;

_vrf_PLAT082_Pnma                
;
PROBLEM: High R1 Value ..................................       0.25 Report    
RESPONSE: The overall quality of crystal was effected by the current temperature.
;

_vrf_PLAT084_Pnma                
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.66 Report   
RESPONSE: At the current temperature, the crystal is frozen, seriously affecting 
          the quality of crystal data.
;

_vrf_DIFMN02_Pnma                
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00 
         _refine_diff_density_min given = -10.055, Test value = -8.300   
RESPONSE: The overall quality of crystal was effected by the current temperature.
;

_vrf_PLAT098_Pnma                
;
PROBLEM: Large Reported Min.  (Negative) Residual Density     -10.06 eA-3    
RESPONSE: At the current temperature, the crystal is frozen,
          which makes the residual peak value become very larg, 
          seriously affecting the quality of crystal data.
;

# 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_Pna21_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2288195'
loop_
_audit_author_name
_audit_author_address
'Ji-Xing Gao'
;Fuyang Normal University
China
;
_audit_update_record             
;
2023-08-11 deposited with the CCDC.	2023-10-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Bi Cl5, C6 H18 N2'
_chemical_formula_sum            'C6 H18 Bi Cl5 N2'
_chemical_formula_weight         504.45

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'
N N 0.0061 0.0033 '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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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                   14.9944(5)
_cell_length_b                   13.3505(4)
_cell_length_c                   7.7677(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1554.96(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4889
_cell_measurement_theta_min      2.7000
_cell_measurement_theta_max      27.9440

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.155
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    12.170
_shelx_estimated_absorpt_T_min   0.348
_shelx_estimated_absorpt_T_max   0.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.273
_exptl_absorpt_correction_T_max  0.296
_exptl_absorpt_process_details   'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'four-circle diffractometer'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7814
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.717
_diffrn_reflns_theta_max         26.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3395
_reflns_number_gt                2680
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0405P)²+1.6832P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3395
_refine_ls_number_parameters     137
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_ref         0.0864
_refine_ls_wR_factor_gt          0.0834
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.10233(2) 0.10918(2) 0.2345(5) 0.05108(15) Uani 1 1 d . . . . .
Cl1 Cl 0.2129(3) -0.0460(3) 0.2418(15) 0.0958(11) Uani 1 1 d . . . . .
Cl2 Cl 0.1766(5) 0.2059(8) -0.0114(6) 0.088(2) Uani 1 1 d . . . . .
Cl3 Cl 0.0006(6) 0.0017(14) -0.0269(13) 0.1011(13) Uani 1 1 d . . . . .
Cl4 Cl -0.0296(3) 0.2491(2) 0.2397(16) 0.0975(11) Uani 1 1 d . . . . .
Cl5 Cl 0.1877(6) 0.2019(9) 0.4725(9) 0.111(3) Uani 1 1 d . . . . .
N1 N 0.4949(12) 0.2892(11) 0.697(3) 0.121(7) Uani 1 1 d D U . . .
H1A H 0.4838 0.3504 0.7409 0.182 Uiso 1 1 d R U . . .
H1B H 0.5507 0.2704 0.7253 0.182 Uiso 1 1 d R U . . .
H1C H 0.4894 0.2910 0.5819 0.182 Uiso 1 1 d R U . . .
N2 N 0.2066(10) -0.1239(12) 0.650(2) 0.113(5) Uani 1 1 d D U . . .
H2A H 0.1475 -0.1323 0.6648 0.169 Uiso 1 1 d R U . . .
H2B H 0.2172 -0.1036 0.5412 0.169 Uiso 1 1 d R U . . .
H2C H 0.2348 -0.1823 0.6691 0.169 Uiso 1 1 d R U . . .
C1 C 0.4267(11) 0.2174(9) 0.736(5) 0.135(7) Uani 1 1 d D U . . .
H1D H 0.3672 0.2382 0.7081 0.163 Uiso 1 1 d DR U . . .
H1E H 0.4319 0.2164 0.8596 0.163 Uiso 1 1 d R U . . .
C2 C 0.4460(10) 0.1121(10) 0.692(2) 0.091(8) Uani 1 1 d D U . . .
H2D H 0.4667 0.1268 0.5774 0.109 Uiso 1 1 d DR U . . .
C3 C 0.3604(16) 0.066(2) 0.665(8) 0.147(12) Uani 0.5 1 d D U P . .
H3A H 0.3863 0.0137 0.5967 0.177 Uiso 0.5 1 d R U P . .
H3B H 0.3177 0.0995 0.5937 0.177 Uiso 0.5 1 d R U P . .
C3' C 0.381(2) 0.0313(14) 0.669(6) 0.147(12) Uani 0.5 1 d D U P . .
H3'A H 0.3414 0.0785 0.7214 0.177 Uiso 0.5 1 d DR U P . .
H3'B H 0.3675 0.0318 0.5478 0.177 Uiso 0.5 1 d R U P . .
C4' C 0.3241(15) -0.005(4) 0.806(5) 0.094(8) Uani 0.5 1 d D U P . .
H4'A H 0.3526 -0.0145 0.9149 0.113 Uiso 0.5 1 d R U P . .
H4'B H 0.3485 -0.0537 0.7283 0.113 Uiso 0.5 1 d R U P . .
C4 C 0.3322(14) -0.024(3) 0.754(5) 0.094(8) Uani 0.5 1 d D U P . .
H4A H 0.3257 0.0241 0.8453 0.113 Uiso 0.5 1 d R U P . .
H4B H 0.3689 -0.0768 0.7975 0.113 Uiso 0.5 1 d R U P . .
C5 C 0.2377(11) -0.0453(14) 0.761(4) 0.131(8) Uani 1 1 d D U . . .
H5A H 0.2192 -0.0697 0.8713 0.157 Uiso 1 1 d R U . . .
H5B H 0.2009 0.0121 0.7384 0.157 Uiso 1 1 d R U . . .
C6 C 0.523(2) 0.0599(19) 0.781(6) 0.075(8) Uani 0.5 1 d D U P . .
H6A H 0.5350 -0.0064 0.7388 0.113 Uiso 0.5 1 d R U P . .
H6B H 0.5726 0.1029 0.7536 0.113 Uiso 0.5 1 d DR U P . .
H6C H 0.5157 0.0576 0.9039 0.113 Uiso 0.5 1 d R U P . .
C6' C 0.538(2) 0.090(2) 0.792(6) 0.075(8) Uani 0.5 1 d D U P . .
H6'A H 0.5268 0.0255 0.7413 0.113 Uiso 0.5 1 d R U P . .
H6'B H 0.5795 0.1263 0.7231 0.113 Uiso 0.5 1 d DR U P . .
H6'C H 0.5612 0.0812 0.9061 0.113 Uiso 0.5 1 d R U P . .


_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 Cl2 2.560(7) . ?
Bi1 Cl5 2.567(8) . ?
Bi1 Cl1 2.654(3) . ?
Bi1 Cl4 2.721(3) . ?
Bi1 Cl3 2.830(11) 2 ?
Bi1 Cl3 2.917(10) . ?
Cl3 Bi1 2.830(11) 2_554 ?
N1 C1 1.434(12) . ?
N2 C5 1.436(13) . ?
C1 C2 1.478(12) . ?
C2 C3 1.439(13) . ?
C2 C3' 1.463(13) . ?
C2 C6 1.522(11) . ?
C2 C6' 1.607(10) . ?
C3 C3' 0.56(3) . ?
C3 C4 1.442(13) . ?
C3 C4' 1.54(9) . ?
C3' C4 1.23(6) . ?
C3' C4' 1.448(13) . ?
C4' C5 1.446(13) . ?
C4 C5 1.447(13) . ?

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
Cl2 Bi1 Cl5 94.42(14) . . ?
Cl2 Bi1 Cl1 97.9(3) . . ?
Cl5 Bi1 Cl1 92.8(3) . . ?
Cl2 Bi1 Cl4 88.9(3) . . ?
Cl5 Bi1 Cl4 91.2(3) . . ?
Cl1 Bi1 Cl4 171.74(15) . . ?
Cl2 Bi1 Cl3 171.7(3) . 2 ?
Cl5 Bi1 Cl3 93.0(4) . 2 ?
Cl1 Bi1 Cl3 85.3(4) . 2 ?
Cl4 Bi1 Cl3 87.3(4) . 2 ?
Cl2 Bi1 Cl3 87.5(3) . . ?
Cl5 Bi1 Cl3 178.0(3) . . ?
Cl1 Bi1 Cl3 87.6(4) . . ?
Cl4 Bi1 Cl3 88.2(4) . . ?
Cl3 Bi1 Cl3 85.029(15) 2 . ?
Bi1 Cl3 Bi1 176.8(6) 2_554 . ?
N1 C1 C2 116.5(17) . . ?
C3 C2 C3' 22.1(10) . . ?
C3 C2 C1 105.5(17) . . ?
C3' C2 C1 126.9(16) . . ?
C3 C2 C6 123(2) . . ?
C3' C2 C6 103.0(19) . . ?
C1 C2 C6 118.5(16) . . ?
C3 C2 C6' 139(2) . . ?
C3' C2 C6' 119(2) . . ?
C1 C2 C6' 103.2(17) . . ?
C6 C2 C6' 16.7(16) . . ?
C3' C3 C2 81(2) . . ?
C3' C3 C4 57(6) . . ?
C2 C3 C4 123(3) . . ?
C3' C3 C4' 70(9) . . ?
C2 C3 C4' 119(4) . . ?
C4 C3 C4' 18.5(15) . . ?
C3 C3' C4 101(6) . . ?
C3 C3' C4' 89(10) . . ?
C4 C3' C4' 18.9(13) . . ?
C3 C3' C2 76.5(19) . . ?
C4 C3' C2 140(4) . . ?
C4' C3' C2 123(3) . . ?
C5 C4' C3' 118(2) . . ?
C5 C4' C3 112(4) . . ?
C3' C4' C3 21.2(16) . . ?
C3' C4 C3 22.3(13) . . ?
C3' C4 C5 136(4) . . ?
C3 C4 C5 118(3) . . ?
N2 C5 C4' 135(2) . . ?
N2 C5 C4 116(2) . . ?
C4' C5 C4 19.5(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -154(3) . . . . ?
N1 C1 C2 C3' -160(3) . . . . ?
N1 C1 C2 C6 63(4) . . . . ?
N1 C1 C2 C6' 56(3) . . . . ?
C1 C2 C3 C3' -167(10) . . . . ?
C6 C2 C3 C3' -26(12) . . . . ?
C6' C2 C3 C3' -34(13) . . . . ?
C3' C2 C3 C4 41(7) . . . . ?
C1 C2 C3 C4 -126(4) . . . . ?
C6 C2 C3 C4 15(6) . . . . ?
C6' C2 C3 C4 6(8) . . . . ?
C3' C2 C3 C4' 62(10) . . . . ?
C1 C2 C3 C4' -105(3) . . . . ?
C6 C2 C3 C4' 36(5) . . . . ?
C6' C2 C3 C4' 27(6) . . . . ?
C2 C3 C3' C4 140(4) . . . . ?
C4' C3 C3' C4 15(3) . . . . ?
C2 C3 C3' C4' 124.7(19) . . . . ?
C4 C3 C3' C4' -15(3) . . . . ?
C4 C3 C3' C2 -140(4) . . . . ?
C4' C3 C3' C2 -124.7(19) . . . . ?
C1 C2 C3' C3 16(12) . . . . ?
C6 C2 C3' C3 158(10) . . . . ?
C6' C2 C3' C3 155(10) . . . . ?
C3 C2 C3' C4 -90(9) . . . . ?
C1 C2 C3' C4 -74(5) . . . . ?
C6 C2 C3' C4 68(4) . . . . ?
C6' C2 C3' C4 64(5) . . . . ?
C3 C2 C3' C4' -79(12) . . . . ?
C1 C2 C3' C4' -63(4) . . . . ?
C6 C2 C3' C4' 79(4) . . . . ?
C6' C2 C3' C4' 75(5) . . . . ?
C3 C3' C4' C5 77(9) . . . . ?
C4 C3' C4' C5 -52(7) . . . . ?
C2 C3' C4' C5 150(3) . . . . ?
C4 C3' C4' C3 -129(15) . . . . ?
C2 C3' C4' C3 73(7) . . . . ?
C3' C3 C4' C5 -112(7) . . . . ?
C2 C3 C4' C5 -180(3) . . . . ?
C4 C3 C4' C5 -70(5) . . . . ?
C2 C3 C4' C3' -68(5) . . . . ?
C4 C3 C4' C3' 42(11) . . . . ?
C4' C3' C4 C3 52(17) . . . . ?
C2 C3' C4 C3 82(8) . . . . ?
C3 C3' C4 C5 41(10) . . . . ?
C4' C3' C4 C5 93(9) . . . . ?
C2 C3' C4 C5 122(4) . . . . ?
C2 C3 C4 C3' -50(6) . . . . ?
C4' C3 C4 C3' -131(14) . . . . ?
C3' C3 C4 C5 -149(8) . . . . ?
C2 C3 C4 C5 161(3) . . . . ?
C4' C3 C4 C5 80(7) . . . . ?
C3' C4' C5 N2 56(7) . . . . ?
C3 C4' C5 N2 79(5) . . . . ?
C3' C4' C5 C4 41(8) . . . . ?
C3 C4' C5 C4 63(11) . . . . ?
C3' C4 C5 N2 89(4) . . . . ?
C3 C4 C5 N2 105(4) . . . . ?
C3' C4 C5 C4' -103(11) . . . . ?
C3 C4 C5 C4' -87(13) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5 H5A Cl1 0.96 2.90 3.76(3) 149.4 1_556
N2 H2C Cl2 0.90 2.44 3.13(2) 133.7 4_545
N2 H2B Cl1 0.90 2.45 3.34(2) 168.2 .
N2 H2A Cl4 0.90 2.43 3.213(16) 145.8 2
N1 H1C Cl4 0.90 2.73 3.61(2) 167.1 3
N1 H1B Cl5 0.90 2.87 3.38(2) 117.7 3
N1 H1B Cl2 0.90 2.80 3.54(2) 140.5 3_556
N1 H1A Cl3 0.90 2.91 3.33(2) 110.2 4
N1 H1A Cl3 0.90 2.69 3.52(2) 154.5 3_556

_refine_diff_density_max         0.995
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.119



####################################################################### 
# 
# 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_Pnma_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2288199'
loop_
_audit_author_name
_audit_author_address
'Ji-Xing Gao'
;Fuyang Normal University
China
;
_audit_update_record             
;
2023-08-11 deposited with the CCDC.	2023-10-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Bi I5, 2(C3 H9 N)'
_chemical_formula_sum            'C6 H18 Bi I5 N2'
_chemical_formula_weight         961.70

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   15.9510(8)
_cell_length_b                   8.5792(4)
_cell_length_c                   13.9712(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1911.91(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5502
_cell_measurement_theta_min      2.5420
_cell_measurement_theta_max      29.8970

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.341
_exptl_crystal_F_000             1664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    17.275
_shelx_estimated_absorpt_T_min   0.122
_shelx_estimated_absorpt_T_max   0.130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.032
_exptl_absorpt_correction_T_max  0.037
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7491
_diffrn_reflns_av_unetI/netI     0.1065
_diffrn_reflns_av_R_equivalents  0.2395
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.554
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1860
_reflns_number_gt                1511
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'PRPKAPPA (Ferguson, 1999)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0037(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1851
_refine_ls_number_parameters     91
_refine_ls_number_restraints     124
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.1240
_refine_ls_wR_factor_ref         0.3327
_refine_ls_wR_factor_gt          0.3227
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_restrained_S_all      1.303
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.002

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 0.10210(3) 0.7500 0.12905(4) 0.05123(16) Uani 1 2 d S TU P . .
I1 I 0.0000 1.0000 0.0000 0.1348(4) Uani 0.5 2 d S U P . .
I1' I 0.0000 1.0000 0.0000 0.1348(4) Uani 0.5 2 d S U P . .
I2 I 0.23063(9) 0.7500 -0.03137(10) 0.0881(3) Uani 1 2 d S TU P . .
I3 I -0.05126(9) 0.7500 0.26452(10) 0.0831(4) Uani 1 2 d S TU P . .
I4 I 0.18184(6) 1.00458(9) 0.23437(7) 0.0855(3) Uani 1 1 d . U . . .
C1 C 0.9093(7) 0.2500 0.2914(6) 0.1498(9) Uani 1 2 d DS TU P . .
H1A H 0.8741 0.1585 0.2847 0.180 Uiso 0.5 1 calc R U P . .
H1B H 0.8741 0.3415 0.2847 0.180 Uiso 0.5 1 calc R U P . .
C2 C 0.9478(6) 0.2500 0.3851(6) 0.1494(9) Uani 1 2 d DS TU P . .
H2D H 0.9268 0.3516 0.4033 0.179 Uiso 0.5 1 d R U P . .
C3 C 0.8848(7) 0.1477(14) 0.4261(11) 0.1490(9) Uani 0.5 1 d D U P . .
H3A H 0.9154 0.0825 0.4707 0.179 Uiso 0.5 1 d R U P . .
H3B H 0.8541 0.0827 0.3814 0.179 Uiso 0.5 1 d R U P . .
C4 C 0.8315(6) 0.2500 0.4816(11) 0.1486(9) Uani 1 2 d DS TU P . .
H4A H 0.8429 0.3495 0.4515 0.178 Uiso 0.5 1 d R U P . .
H4B H 0.8549 0.2500 0.5458 0.178 Uiso 1 2 d R U P . .
C5 C 0.7460(6) 0.2500 0.5151(10) 0.1485(9) Uani 1 2 d DS TU P . .
H5A H 0.7227 0.2500 0.4508 0.178 Uiso 1 2 d R U P . .
H5B H 0.7340 0.3531 0.5398 0.178 Uiso 0.5 1 d R U P . .
C6 C 1.0188(8) 0.2500 0.4494(12) 0.238(8) Uani 1 2 d DS TU P . .
H6A H 1.0302 0.3547 0.4698 0.357 Uiso 0.5 1 calc R U P . .
H6B H 1.0670 0.2088 0.4169 0.357 Uiso 0.5 1 calc R U P . .
H6C H 1.0064 0.1865 0.5041 0.357 Uiso 0.5 1 calc R U P . .
N1 N 0.9717(8) 0.2500 0.2181(9) 0.1506(13) Uani 1 2 d DS TU P . .
H1C H 0.9656 0.3345 0.1818 0.226 Uiso 0.5 1 calc R U P . .
H1D H 0.9659 0.1651 0.1821 0.226 Uiso 0.5 1 calc R U P . .
H1E H 1.0223 0.2505 0.2447 0.226 Uiso 1 2 calc R U P . .
N2 N 0.6929(10) 0.159(2) 0.5751(12) 0.1478(13) Uani 0.5 1 d D U P . .
H2A H 0.6390 0.1912 0.5695 0.222 Uiso 0.5 1 d R U P . .
H2B H 0.6975 0.0601 0.5524 0.222 Uiso 0.5 1 d R U P . .
H2C H 0.7084 0.1613 0.6379 0.222 Uiso 0.5 1 d R U P . .


_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 I4 2.9245(10) . ?
Bi1 I4 2.9246(10) 7_575 ?
Bi1 I2 3.0375(15) . ?
Bi1 I3 3.0929(14) . ?
Bi1 I1' 3.2408(4) 3_545 ?
Bi1 I1 3.2408(4) 3_545 ?
Bi1 I1' 3.2408(4) . ?
Bi1 I1 3.2408(4) . ?
I1 Bi1 3.2408(4) 5_575 ?
I1' Bi1 3.2408(4) 5_575 ?
C1 N1 1.427(13) . ?
C1 C2 1.446(12) . ?
C2 C6 1.445(14) . ?
C2 C3 1.452(12) 7_565 ?
C2 C3 1.452(12) . ?
C3 C4 1.447(13) . ?
C3 C3 1.76(2) 7_565 ?
C4 C5 1.442(12) . ?
C4 C3 1.447(13) 7_565 ?
C5 N2 1.426(14) 7_565 ?
C5 N2 1.426(14) . ?
N2 N2 1.56(3) 7_565 ?

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
I4 Bi1 I4 96.63(4) . 7_575 ?
I4 Bi1 I2 94.46(3) . . ?
I4 Bi1 I2 94.46(3) 7_575 . ?
I4 Bi1 I3 92.07(3) . . ?
I4 Bi1 I3 92.07(3) 7_575 . ?
I2 Bi1 I3 170.18(4) . . ?
I4 Bi1 I1' 173.07(2) . 3_545 ?
I4 Bi1 I1' 90.241(19) 7_575 3_545 ?
I2 Bi1 I1' 85.91(2) . 3_545 ?
I3 Bi1 I1' 86.73(2) . 3_545 ?
I4 Bi1 I1 173.07(2) . 3_545 ?
I4 Bi1 I1 90.241(19) 7_575 3_545 ?
I2 Bi1 I1 85.91(2) . 3_545 ?
I3 Bi1 I1 86.73(2) . 3_545 ?
I1' Bi1 I1 0.0 3_545 3_545 ?
I4 Bi1 I1' 90.241(19) . . ?
I4 Bi1 I1' 173.07(2) 7_575 . ?
I2 Bi1 I1' 85.91(2) . . ?
I3 Bi1 I1' 86.73(2) . . ?
I1' Bi1 I1' 82.875(13) 3_545 . ?
I1 Bi1 I1' 82.875(13) 3_545 . ?
I4 Bi1 I1 90.241(19) . . ?
I4 Bi1 I1 173.07(2) 7_575 . ?
I2 Bi1 I1 85.91(2) . . ?
I3 Bi1 I1 86.73(2) . . ?
I1' Bi1 I1 82.875(13) 3_545 . ?
I1 Bi1 I1 82.875(13) 3_545 . ?
I1' Bi1 I1 0.0 . . ?
Bi1 I1 Bi1 180.0 5_575 . ?
Bi1 I1' Bi1 180.0 5_575 . ?
N1 C1 C2 110.7(10) . . ?
C1 C2 C6 153.6(11) . . ?
C1 C2 C3 93.6(8) . 7_565 ?
C6 C2 C3 107.3(9) . 7_565 ?
C1 C2 C3 93.6(8) . . ?
C6 C2 C3 107.3(9) . . ?
C3 C2 C3 74.4(10) 7_565 . ?
C4 C3 C2 104.6(9) . . ?
C4 C3 C3 52.7(5) . 7_565 ?
C2 C3 C3 52.8(5) . 7_565 ?
C5 C4 C3 136.8(7) . . ?
C5 C4 C3 136.8(7) . 7_565 ?
C3 C4 C3 74.7(11) . 7_565 ?
N2 C5 N2 66.5(15) 7_565 . ?
N2 C5 C4 138.9(10) 7_565 . ?
N2 C5 C4 138.9(10) . . ?
C5 N2 N2 56.7(8) . 7_565 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C6 0.000(2) . . . . ?
N1 C1 C2 C3 142.7(5) . . . 7_565 ?
N1 C1 C2 C3 -142.7(5) . . . . ?
C1 C2 C3 C4 -103.2(10) . . . . ?
C6 C2 C3 C4 93.2(11) . . . . ?
C3 C2 C3 C4 -10.5(14) 7_565 . . . ?
C1 C2 C3 C3 -92.7(6) . . . 7_565 ?
C6 C2 C3 C3 103.7(8) . . . 7_565 ?
C2 C3 C4 C5 154.8(15) . . . . ?
C3 C3 C4 C5 144(2) 7_565 . . . ?
C2 C3 C4 C3 10.5(14) . . . 7_565 ?
C3 C4 C5 N2 174.1(17) . . . 7_565 ?
C3 C4 C5 N2 -61(3) 7_565 . . 7_565 ?
C3 C4 C5 N2 61(3) . . . . ?
C3 C4 C5 N2 -174.1(17) 7_565 . . . ?
C4 C5 N2 N2 139(2) . . . 7_565 ?

_refine_diff_density_max         4.344
_refine_diff_density_min         -3.873
_refine_diff_density_rms         0.598

# start Validation Reply Form

_vrf_RINTA01_Pnma                
;
PROBLEM: The value of Rint is greater than 0.18  Rint given   0.240   
RESPONSE: Both the anions and cations are highly disordered 
          at the current temperature.
;

_vrf_PLAT020_Pnma                
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.240 Report   
RESPONSE: Both the anions and cations are highly disordered 
          at the current temperature.
;

_vrf_PLAT242_Pnma                
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Bi1 Check    
RESPONSE: The overall quality of crystal was effected by the current temperature.
          Besides, the false alarms may occurred for the BiI6 groups, 
          which like an octahedron.

;

# 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_Pnma_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2288198'
loop_
_audit_author_name
_audit_author_address
'Ji-Xing Gao'
;Fuyang Normal University
China
;
_audit_update_record             
;
2023-08-11 deposited with the CCDC.	2023-10-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Bi I5, 2(C3 H9 N)'
_chemical_formula_sum            'C6 H18 Bi I5 N2'
_chemical_formula_weight         961.70

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   15.8297(6)
_cell_length_b                   8.5091(3)
_cell_length_c                   13.7812(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1856.28(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    6649
_cell_measurement_theta_min      2.5620
_cell_measurement_theta_max      30.2230

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.441
_exptl_crystal_F_000             1664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    17.792
_shelx_estimated_absorpt_T_min   0.118
_shelx_estimated_absorpt_T_max   0.125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.028
_exptl_absorpt_correction_T_max  0.033
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7841
_diffrn_reflns_av_unetI/netI     0.0871
_diffrn_reflns_av_R_equivalents  0.1883
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.573
_diffrn_reflns_theta_max         25.247
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1804
_reflns_number_gt                1683
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'PRPKAPPA (Ferguson, 1999)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.6150P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0015(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1795
_refine_ls_number_parameters     91
_refine_ls_number_restraints     138
_refine_ls_R_factor_all          0.1621
_refine_ls_R_factor_gt           0.1591
_refine_ls_wR_factor_ref         0.5569
_refine_ls_wR_factor_gt          0.5483
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.008

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 0.10238(6) 0.7500 0.12965(6) 0.0299(3) Uani 1 2 d S TU P . .
I1 I 0.0000 1.0000 0.0000 0.1421(14) Uani 0.5 2 d S U P . .
I1' I 0.0000 1.0000 0.0000 0.1421(14) Uani 0.5 2 d S U P . .
I2 I 0.23089(15) 0.7500 -0.03314(16) 0.0543(5) Uani 1 2 d S TU P . .
I3 I -0.05196(14) 0.7500 0.26752(15) 0.0527(6) Uani 1 2 d S TU P . .
I4 I 0.18432(12) 1.0045(2) 0.23609(14) 0.0753(5) Uani 1 1 d . U . . .
C1 C 0.9240(17) 0.2500 0.2967(7) 0.083(2) Uani 1 2 d DS TU P . .
H1A H 0.8855 0.1583 0.2952 0.099 Uiso 0.5 1 calc R U P . .
H1B H 0.8855 0.3417 0.2952 0.099 Uiso 0.5 1 calc R U P . .
C2 C 0.9451(7) 0.2500 0.3993(8) 0.082(2) Uani 1 2 d DS TU P . .
H2D H 0.9240 0.3516 0.4175 0.099 Uiso 0.5 1 d R U P . .
C3 C 0.8814(9) 0.1549(18) 0.4478(12) 0.081(2) Uani 0.5 1 d D U P . .
H3A H 0.9120 0.0897 0.4925 0.097 Uiso 0.5 1 d R U P . .
H3B H 0.8507 0.0899 0.4031 0.097 Uiso 0.5 1 d R U P . .
C4 C 0.8302(7) 0.2500 0.5122(14) 0.079(2) Uani 1 2 d DS TU P . .
H4A H 0.8415 0.3495 0.4820 0.095 Uiso 0.5 1 d R U P . .
H4B H 0.8535 0.2500 0.5763 0.095 Uiso 1 2 d R U P . .
C5 C 0.7386(7) 0.2500 0.5075(16) 0.078(2) Uani 1 2 d DS TU P . .
H5A H 0.7152 0.2500 0.4433 0.094 Uiso 1 2 d R U P . .
H5B H 0.7266 0.3531 0.5322 0.094 Uiso 0.5 1 d R U P . .
C6 C 1.0266(9) 0.2500 0.447(2) 0.174(10) Uani 1 2 d DS TU P . .
H6A H 1.0193 0.2735 0.5159 0.261 Uiso 0.5 1 calc R U P . .
H6B H 1.0628 0.3301 0.4170 0.261 Uiso 0.5 1 calc R U P . .
H6C H 1.0530 0.1465 0.4394 0.261 Uiso 0.5 1 calc R U P . .
N1 N 0.9510(17) 0.2500 0.1964(9) 0.083(3) Uani 1 2 d DS TU P . .
H1C H 0.9882 0.1700 0.1865 0.125 Uiso 0.5 1 calc R U P . .
H1D H 0.9765 0.3431 0.1824 0.125 Uiso 0.5 1 calc R U P . .
H1E H 0.9053 0.2369 0.1571 0.125 Uiso 0.5 1 calc R U P . .
N2 N 0.6827(12) 0.154(3) 0.5649(16) 0.076(3) Uani 0.5 1 d D U P . .
H2A H 0.6288 0.1859 0.5594 0.115 Uiso 0.5 1 d R U P . .
H2B H 0.6873 0.0547 0.5422 0.115 Uiso 0.5 1 d R U P . .
H2C H 0.6982 0.1559 0.6278 0.115 Uiso 0.5 1 d R U P . .


_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 I4 2.9197(18) . ?
Bi1 I4 2.9197(18) 7_575 ?
Bi1 I2 3.028(2) . ?
Bi1 I3 3.095(2) . ?
Bi1 I1' 3.2162(6) 3_545 ?
Bi1 I1 3.2162(6) 3_545 ?
Bi1 I1' 3.2162(6) . ?
Bi1 I1 3.2162(6) . ?
I1 Bi1 3.2162(6) 5_575 ?
I1' Bi1 3.2162(6) 5_575 ?
C1 N1 1.448(15) . ?
C1 C2 1.453(13) . ?
C2 C6 1.447(15) . ?
C2 C3 1.454(14) 7_565 ?
C2 C3 1.454(14) . ?
C3 C4 1.449(15) . ?
C3 C3 1.62(3) 7_565 ?
C4 C3 1.449(15) 7_565 ?
C4 C5 1.451(13) . ?
C5 N2 1.443(16) 7_565 ?
C5 N2 1.443(16) . ?
N2 N2 1.64(4) 7_565 ?

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
I4 Bi1 I4 95.76(8) . 7_575 ?
I4 Bi1 I2 94.23(5) . . ?
I4 Bi1 I2 94.23(5) 7_575 . ?
I4 Bi1 I3 92.42(5) . . ?
I4 Bi1 I3 92.42(5) 7_575 . ?
I2 Bi1 I3 170.08(7) . . ?
I4 Bi1 I1' 173.51(5) . 3_545 ?
I4 Bi1 I1' 90.71(4) 7_575 3_545 ?
I2 Bi1 I1' 85.81(4) . 3_545 ?
I3 Bi1 I1' 86.75(4) . 3_545 ?
I4 Bi1 I1 173.51(5) . 3_545 ?
I4 Bi1 I1 90.71(4) 7_575 3_545 ?
I2 Bi1 I1 85.81(4) . 3_545 ?
I3 Bi1 I1 86.75(4) . 3_545 ?
I1' Bi1 I1 0.0 3_545 3_545 ?
I4 Bi1 I1' 90.71(4) . . ?
I4 Bi1 I1' 173.51(5) 7_575 . ?
I2 Bi1 I1' 85.81(4) . . ?
I3 Bi1 I1' 86.75(4) . . ?
I1' Bi1 I1' 82.82(2) 3_545 . ?
I1 Bi1 I1' 82.82(2) 3_545 . ?
I4 Bi1 I1 90.71(4) . . ?
I4 Bi1 I1 173.51(5) 7_575 . ?
I2 Bi1 I1 85.81(4) . . ?
I3 Bi1 I1 86.75(4) . . ?
I1' Bi1 I1 82.82(2) 3_545 . ?
I1 Bi1 I1 82.82(2) 3_545 . ?
I1' Bi1 I1 0.0 . . ?
Bi1 I1 Bi1 180.0 . 5_575 ?
Bi1 I1' Bi1 180.0 . 5_575 ?
N1 C1 C2 150(2) . . ?
C6 C2 C1 130.1(17) . . ?
C6 C2 C3 114.2(12) . 7_565 ?
C1 C2 C3 106.7(12) . 7_565 ?
C6 C2 C3 114.2(12) . . ?
C1 C2 C3 106.7(12) . . ?
C3 C2 C3 67.6(13) 7_565 . ?
C4 C3 C2 111.0(12) . . ?
C4 C3 C3 56.1(7) . 7_565 ?
C2 C3 C3 56.2(6) . 7_565 ?
C3 C4 C3 67.9(14) . 7_565 ?
C3 C4 C5 122.2(13) . . ?
C3 C4 C5 122.2(13) 7_565 . ?
N2 C5 N2 69(2) 7_565 . ?
N2 C5 C4 126.0(15) 7_565 . ?
N2 C5 C4 126.0(15) . . ?
C5 N2 N2 55.3(10) . 7_565 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C6 0.000(4) . . . . ?
N1 C1 C2 C3 144.5(7) . . . 7_565 ?
N1 C1 C2 C3 -144.5(7) . . . . ?
C6 C2 C3 C4 95.1(15) . . . . ?
C1 C2 C3 C4 -114.0(13) . . . . ?
C3 C2 C3 C4 -12.4(16) 7_565 . . . ?
C6 C2 C3 C3 107.6(11) . . . 7_565 ?
C1 C2 C3 C3 -101.6(9) . . . 7_565 ?
C2 C3 C4 C3 12.4(16) . . . 7_565 ?
C2 C3 C4 C5 127.5(13) . . . . ?
C3 C3 C4 C5 115.0(16) 7_565 . . . ?
C3 C4 C5 N2 -176.6(17) . . . 7_565 ?
C3 C4 C5 N2 -94(2) 7_565 . . 7_565 ?
C3 C4 C5 N2 94(2) . . . . ?
C3 C4 C5 N2 176.5(17) 7_565 . . . ?
C4 C5 N2 N2 120(2) . . . 7_565 ?

_refine_diff_density_max         17.198
_refine_diff_density_min         -12.035
_refine_diff_density_rms         0.959

# start Validation Reply Form

_vrf_PLAT084_Pnma                
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.56 Report
RESPONSE: At the current temperature, the crystal is frozen, seriously affecting 
          the quality of crystal data.
;

_vrf_PLAT097_Pnma                
;
PROBLEM: Large Reported Max.  (Positive) Residual Density      17.20 eA-3
RESPONSE: At the current temperature, the crystal is frozen,
          which makes the residual peak value become very larg, 
          seriously affecting the quality of crystal data.
;

_vrf_DIFMN02_Pnma                
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00 
         _refine_diff_density_min given = -12.035, Test value = -8.300
RESPONSE: The overall quality of crystal was effected by the current temperature.
;

_vrf_RINTA01_Pnma                
;
PROBLEM: The value of Rint is greater than 0.18, Rint given   0.188
RESPONSE: At the current temperature, the crystal is frozen, seriously affecting 
          the quality of crystal data.
;

_vrf_PLAT020_Pnma                
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.188 Report
RESPONSE:At the current temperature, the crystal is frozen, seriously affecting 
          the quality of crystal data.
;

_vrf_PLAT082_Pnma                
;
PROBLEM: High R1 Value ..................................       0.16 Report
RESPONSE:At the current temperature, the crystal is frozen, seriously affecting 
          the quality of crystal data.
;

_vrf_PLAT098_Pnma                
;
PROBLEM: Large Reported Min.  (Negative) Residual Density     -12.03 eA-3
RESPONSE: At the current temperature, the crystal is frozen,
          which makes the residual peak value become very larg, 
          seriously affecting the quality of crystal data.
;

_vrf_PLAT242_Pnma                
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Bi1 Check
RESPONSE: The overall quality of crystal was effected by the current temperature.
          Besides, the false alarms may occurred for the BiI6 groups, 
          which like an octahedron.

;

# 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_Pnma_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2288197'
loop_
_audit_author_name
_audit_author_address
'Ji-Xing Gao'
;Fuyang Normal University
China
;
_audit_update_record             
;
2023-08-11 deposited with the CCDC.	2023-10-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Bi Br5, 2(C3 H9 N)'
_chemical_formula_sum            'C6 H18 Bi Br5 N2'
_chemical_formula_weight         726.70

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'
N N 0.0061 0.0033 '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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   15.3618(6)
_cell_length_b                   8.0509(3)
_cell_length_c                   13.5870(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1680.39(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5897
_cell_measurement_theta_min      2.6590
_cell_measurement_theta_max      29.1900

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.873
_exptl_crystal_F_000             1304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    22.357
_shelx_estimated_absorpt_T_min   0.089
_shelx_estimated_absorpt_T_max   0.094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.011
_exptl_absorpt_correction_T_max  0.013
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10733
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_av_R_equivalents  0.1235
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.652
_diffrn_reflns_theta_max         27.243
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2017
_reflns_number_gt                1626
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'PRPKAPPA (Ferguson, 1999)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0571P)²+17.1195P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00311(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2021
_refine_ls_number_parameters     90
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1390
_refine_ls_wR_factor_gt          0.1309
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.002

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 0.10384(2) 0.7500 0.11719(2) 0.04431(8) Uani 1 2 d S T P . .
Br1 Br 0.0000 1.0000 0.0000 0.1015(4) Uani 1 2 d S . P . .
Br2 Br 0.21891(9) 0.7500 -0.04365(9) 0.0891(4) Uani 1 2 d S T P . .
Br3 Br -0.03717(8) 0.7500 0.25591(8) 0.0841(4) Uani 1 2 d S T P . .
Br4 Br 0.18422(6) 1.00055(10) 0.21460(6) 0.0821(2) Uani 1 1 d . . . . .
C1 C 0.9256(8) 0.2500 0.2846(6) 0.112(6) Uani 1 2 d DS T P . .
H1E H 0.8893 0.1531 0.2737 0.135 Uiso 0.5 1 calc R U P . .
H1D H 0.8893 0.3469 0.2737 0.135 Uiso 0.5 1 calc R U P . .
C2 C 0.9512(6) 0.2500 0.3853(6) 0.120(5) Uani 1 2 d DS TU P . .
H2A H 0.9380 0.3647 0.3976 0.144 Uiso 0.5 1 d R U P . .
C3 C 0.8758(8) 0.184(3) 0.4384(13) 0.166(8) Uani 0.5 1 d D U P . .
H3A H 0.8990 0.0870 0.4704 0.199 Uiso 0.5 1 d R U P . .
H3B H 0.8353 0.1431 0.3902 0.199 Uiso 0.5 1 d R U P . .
C4 C 0.8317(6) 0.2500 0.5018(12) 0.127(5) Uani 1 2 d DS TU P . .
H4A H 0.8442 0.3656 0.4916 0.153 Uiso 0.5 1 d R U P . .
H4B H 0.8603 0.2218 0.5624 0.153 Uiso 0.5 1 d R U P . .
C5 C 0.7450(6) 0.2500 0.5370(9) 0.140(6) Uani 1 2 d DS TU P . .
H5A H 0.7159 0.2241 0.4764 0.168 Uiso 0.5 1 d R U P . .
H5B H 0.7325 0.3650 0.5492 0.168 Uiso 0.5 1 d R U P . .
C6 C 1.0319(7) 0.2500 0.4334(11) 0.159(8) Uani 1 2 d DS TU P . .
H6A H 1.0744 0.2974 0.3900 0.238 Uiso 0.5 1 d R U P . .
H6B H 1.0289 0.3146 0.4928 0.238 Uiso 0.5 1 d R U P . .
H6C H 1.0482 0.1380 0.4492 0.238 Uiso 0.5 1 d R U P . .
N1 N 0.9911(8) 0.2500 0.2127(8) 0.172(8) Uani 1 2 d DS T P . .
H1A H 1.0247 0.1609 0.2205 0.257 Uiso 0.5 1 calc R U P . .
H1B H 1.0232 0.3414 0.2188 0.257 Uiso 0.5 1 calc R U P . .
H1C H 0.9669 0.2477 0.1532 0.257 Uiso 1 2 calc R U P . .
N2 N 0.6960(9) 0.1667(19) 0.6040(10) 0.143(7) Uani 0.5 1 d D U P . .
H2B H 0.6399 0.1979 0.5992 0.215 Uiso 0.5 1 d R U P . .
H2C H 0.7002 0.0564 0.5943 0.215 Uiso 0.5 1 d R U P . .
H2D H 0.7162 0.1920 0.6644 0.215 Uiso 0.5 1 d R U P . .


_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 Br4 2.7102(8) . ?
Bi1 Br4 2.7102(8) 7_575 ?
Bi1 Br2 2.8108(12) . ?
Bi1 Br3 2.8714(12) . ?
Bi1 Br1 3.0217(2) 3_545 ?
Bi1 Br1 3.0217(2) . ?
Br1 Bi1 3.0217(2) 5_575 ?
C1 N1 1.402(13) . ?
C1 C2 1.424(11) . ?
C2 C6 1.402(12) . ?
C2 C3 1.464(14) 7_565 ?
C2 C3 1.464(14) . ?
C3 C3 1.07(5) 7_565 ?
C3 C4 1.22(2) . ?
C4 C3 1.22(2) 7_565 ?
C4 C5 1.416(12) . ?
C5 N2 1.358(13) 7_565 ?
C5 N2 1.358(13) . ?
N2 N2 1.34(3) 7_565 ?

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
Br4 Bi1 Br4 96.19(4) . 7_575 ?
Br4 Bi1 Br2 95.34(3) . . ?
Br4 Bi1 Br2 95.35(3) 7_575 . ?
Br4 Bi1 Br3 91.33(3) . . ?
Br4 Bi1 Br3 91.32(3) 7_575 . ?
Br2 Bi1 Br3 170.00(4) . . ?
Br4 Bi1 Br1 173.51(2) . 3_545 ?
Br4 Bi1 Br1 90.120(18) 7_575 3_545 ?
Br2 Bi1 Br1 85.55(2) . 3_545 ?
Br3 Bi1 Br1 87.00(2) . 3_545 ?
Br4 Bi1 Br1 90.120(18) . . ?
Br4 Bi1 Br1 173.51(2) 7_575 . ?
Br2 Bi1 Br1 85.55(2) . . ?
Br3 Bi1 Br1 87.00(2) . . ?
Br1 Bi1 Br1 83.532(8) 3_545 . ?
Bi1 Br1 Bi1 180.000(10) . 5_575 ?
N1 C1 C2 118.1(10) . . ?
C6 C2 C1 133.8(10) . . ?
C6 C2 C3 118.0(10) . 7_565 ?
C1 C2 C3 104.8(10) . 7_565 ?
C6 C2 C3 118.0(10) . . ?
C1 C2 C3 104.8(10) . . ?
C3 C2 C3 42.8(18) 7_565 . ?
C3 C3 C4 64.0(10) 7_565 . ?
C3 C3 C2 68.6(9) 7_565 . ?
C4 C3 C2 128.8(17) . . ?
C3 C4 C3 52(2) . 7_565 ?
C3 C4 C5 139.6(12) . . ?
C3 C4 C5 139.6(12) 7_565 . ?
N2 C5 N2 59.2(14) 7_565 . ?
N2 C5 C4 138.4(10) 7_565 . ?
N2 C5 C4 138.4(10) . . ?
N2 N2 C5 60.4(7) 7_565 . ?

_refine_diff_density_max         2.252
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.251



