# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_BM41_a
_database_code_depnum_ccdc_archive 'CCDC 1875700'
_audit_update_record             
;
2018-10-27 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
#complex (C3H7NC5H5)[SbBr6]
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 Br6 N Sb'
_chemical_formula_weight         723.40

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'
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'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   7.3687(2)
_cell_length_b                   16.4706(4)
_cell_length_c                   13.8620(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.054(3)
_cell_angle_gamma                90
_cell_volume                     1669.65(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    3855
_cell_measurement_theta_min      3.7300
_cell_measurement_theta_max      28.4820

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.878
_exptl_crystal_F_000             1312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    15.989
_shelx_estimated_absorpt_T_min   0.103
_shelx_estimated_absorpt_T_max   0.250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.46468
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            8273
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.312
_diffrn_reflns_theta_max         29.051
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3729
_reflns_number_gt                3239
_reflns_threshold_expression     >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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.0185P)²+0.1107P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3729
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0595
_refine_ls_wR_factor_gt          0.0572
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_restrained_S_all      1.173
_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
C1 C 0.0463(7) 0.2543(4) 0.7117(4) 0.0370(15) Uani 1 1 d . . . . .
H1A H -0.065776 0.284808 0.718082 0.056 Uiso 1 1 calc R U . . .
H1B H 0.146808 0.275963 0.757263 0.056 Uiso 1 1 calc R U . . .
H1C H 0.027330 0.196899 0.726441 0.056 Uiso 1 1 calc R U . . .
C2 C 0.0933(6) 0.2621(3) 0.6087(3) 0.0200(11) Uani 1 1 d . . . . .
H2A H 0.124376 0.319271 0.595853 0.024 Uiso 1 1 calc R U . . .
H2B H 0.201287 0.228123 0.600818 0.024 Uiso 1 1 calc R U . . .
C3 C -0.0669(6) 0.2355(3) 0.5366(3) 0.0182(10) Uani 1 1 d . . . . .
H3A H -0.093457 0.177615 0.548043 0.022 Uiso 1 1 calc R U . . .
H3B H -0.176233 0.267441 0.547746 0.022 Uiso 1 1 calc R U . . .
C4 C -0.0482(6) 0.3207(3) 0.3943(3) 0.0183(10) Uani 1 1 d . . . . .
H4 H -0.086060 0.364997 0.430902 0.022 Uiso 1 1 calc R U . . .
C5 C -0.0106(6) 0.3331(3) 0.3016(4) 0.0209(11) Uani 1 1 d . . . . .
H5 H -0.020926 0.385936 0.273993 0.025 Uiso 1 1 calc R U . . .
C6 C 0.0427(6) 0.2684(3) 0.2479(4) 0.0226(11) Uani 1 1 d . . . . .
H6 H 0.066708 0.275991 0.182696 0.027 Uiso 1 1 calc R U . . .
C7 C 0.0605(6) 0.1925(3) 0.2908(4) 0.0227(11) Uani 1 1 d . . . . .
H7 H 0.098973 0.147464 0.255692 0.027 Uiso 1 1 calc R U . . .
C8 C 0.0223(6) 0.1829(3) 0.3842(4) 0.0198(11) Uani 1 1 d . . . . .
H8 H 0.034300 0.130863 0.413802 0.024 Uiso 1 1 calc R U . . .
N1 N -0.0320(5) 0.2460(2) 0.4345(3) 0.0143(8) Uani 1 1 d . . . . .
Br1 Br 0.24080(6) 0.02495(3) 0.60285(3) 0.01988(12) Uani 1 1 d . . . . .
Br2 Br 0.73744(6) 0.02881(3) 0.64559(3) 0.01652(11) Uani 1 1 d . . . . .
Br3 Br 0.49637(6) 0.14942(3) 0.45400(4) 0.02029(12) Uani 1 1 d . . . . .
Br4 Br 0.80968(6) 0.46638(3) 0.59523(3) 0.01827(11) Uani 1 1 d . . . . .
Br5 Br 0.44978(6) 0.34954(3) 0.46373(4) 0.02049(12) Uani 1 1 d . . . . .
Br6 Br 0.65385(6) 0.51330(3) 0.34582(3) 0.01917(11) Uani 1 1 d . . . . .
Sb1 Sb 0.500000 0.000000 0.500000 0.00915(9) Uani 1 2 d S . P . .
Sb2 Sb 0.500000 0.500000 0.500000 0.01011(10) Uani 1 2 d S . 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
C1 C2 1.516(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.515(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N1 1.480(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N1 1.349(5) . ?
C4 C5 1.362(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.383(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.368(6) . ?
C7 H7 0.9500 . ?
C8 N1 1.340(6) . ?
C8 H8 0.9500 . ?
Br1 Sb1 2.5531(4) . ?
Br2 Sb1 2.5479(4) . ?
Br3 Sb1 2.5416(4) . ?
Br4 Sb2 2.5527(4) . ?
Br5 Sb2 2.5467(4) . ?
Br6 Sb2 2.5488(5) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 110.3(4) . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N1 C3 C2 112.6(4) . . ?
N1 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
N1 C3 H3B 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
N1 C4 C5 120.5(4) . . ?
N1 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 119.7(5) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C7 C6 C5 118.8(5) . . ?
C7 C6 H6 120.6 . . ?
C5 C6 H6 120.6 . . ?
C8 C7 C6 119.5(4) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
N1 C8 C7 120.8(4) . . ?
N1 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C8 N1 C4 120.6(4) . . ?
C8 N1 C3 120.3(4) . . ?
C4 N1 C3 119.0(4) . . ?
Br3 Sb1 Br3 180.0 3_656 . ?
Br3 Sb1 Br2 90.197(15) 3_656 3_656 ?
Br3 Sb1 Br2 89.803(15) . 3_656 ?
Br3 Sb1 Br2 89.803(15) 3_656 . ?
Br3 Sb1 Br2 90.197(15) . . ?
Br2 Sb1 Br2 180.000(14) 3_656 . ?
Br3 Sb1 Br1 89.926(16) 3_656 3_656 ?
Br3 Sb1 Br1 90.074(16) . 3_656 ?
Br2 Sb1 Br1 90.905(15) 3_656 3_656 ?
Br2 Sb1 Br1 89.095(15) . 3_656 ?
Br3 Sb1 Br1 90.074(16) 3_656 . ?
Br3 Sb1 Br1 89.927(16) . . ?
Br2 Sb1 Br1 89.096(15) 3_656 . ?
Br2 Sb1 Br1 90.904(15) . . ?
Br1 Sb1 Br1 180.0 3_656 . ?
Br5 Sb2 Br5 180.0 . 3_666 ?
Br5 Sb2 Br6 90.750(15) . 3_666 ?
Br5 Sb2 Br6 89.251(15) 3_666 3_666 ?
Br5 Sb2 Br6 89.249(15) . . ?
Br5 Sb2 Br6 90.750(15) 3_666 . ?
Br6 Sb2 Br6 179.999(17) 3_666 . ?
Br5 Sb2 Br4 89.427(15) . . ?
Br5 Sb2 Br4 90.574(15) 3_666 . ?
Br6 Sb2 Br4 90.525(15) 3_666 . ?
Br6 Sb2 Br4 89.475(15) . . ?
Br5 Sb2 Br4 90.571(15) . 3_666 ?
Br5 Sb2 Br4 89.428(15) 3_666 3_666 ?
Br6 Sb2 Br4 89.476(15) 3_666 3_666 ?
Br6 Sb2 Br4 90.523(15) . 3_666 ?
Br4 Sb2 Br4 180.0 . 3_666 ?

_refine_diff_density_max         0.763
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.172

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
####################################################################### 
# 
# 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_8_a
_database_code_depnum_ccdc_archive 'CCDC 1875707'
_audit_update_record             
;
2018-10-27 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
#complex (C2H5NC5H4CH3)2[SbBr6]Br3
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H24 Br9 N2 Sb'
_chemical_formula_weight         1085.31

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'
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'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   8.4645(4)
_cell_length_b                   13.0802(6)
_cell_length_c                   13.1574(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.702(5)
_cell_angle_gamma                90
_cell_volume                     1402.39(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    2334
_cell_measurement_theta_min      3.9940
_cell_measurement_theta_max      28.0790

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.570
_exptl_crystal_F_000             1000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    13.813
_shelx_estimated_absorpt_T_min   0.104
_shelx_estimated_absorpt_T_max   0.231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.51598
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            6198
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.506
_diffrn_reflns_theta_max         28.876
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3059
_reflns_number_gt                2572
_reflns_threshold_expression     >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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.0164P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3059
_refine_ls_number_parameters     130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0545
_refine_ls_wR_factor_gt          0.0516
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_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
C1 C 0.4331(6) 0.2896(4) 0.7913(3) 0.0302(12) Uani 1 1 d . . . . .
H1A H 0.345609 0.247788 0.805758 0.045 Uiso 1 1 calc R U . . .
H1B H 0.407367 0.362129 0.796261 0.045 Uiso 1 1 calc R U . . .
H1C H 0.537436 0.273726 0.843014 0.045 Uiso 1 1 calc R U . . .
C2 C 0.3709(5) 0.1846(3) 0.6309(3) 0.0238(11) Uani 1 1 d . . . . .
H2 H 0.311159 0.140127 0.663933 0.029 Uiso 1 1 calc R U . . .
C3 C 0.3787(5) 0.1645(3) 0.5317(3) 0.0225(10) Uani 1 1 d . . . . .
H3 H 0.326183 0.105252 0.496400 0.027 Uiso 1 1 calc R U . . .
C4 C 0.4618(5) 0.2287(3) 0.4807(3) 0.0203(10) Uani 1 1 d . . . . .
C5 C 0.5419(5) 0.3127(3) 0.5378(3) 0.0252(11) Uani 1 1 d . . . . .
H5 H 0.603544 0.357761 0.506724 0.030 Uiso 1 1 calc R U . . .
C6 C 0.5316(5) 0.3303(3) 0.6386(3) 0.0221(10) Uani 1 1 d . . . . .
H6 H 0.585298 0.387945 0.676627 0.027 Uiso 1 1 calc R U . . .
C7 C 0.4706(6) 0.2081(4) 0.3700(3) 0.0327(12) Uani 1 1 d . . . . .
H7A H 0.357907 0.205105 0.322355 0.039 Uiso 1 1 calc R U . . .
H7B H 0.528814 0.265179 0.346324 0.039 Uiso 1 1 calc R U . . .
C8 C 0.5576(6) 0.1098(4) 0.3620(3) 0.0419(14) Uani 1 1 d . . . . .
H8A H 0.659765 0.106422 0.418974 0.063 Uiso 1 1 calc R U . . .
H8B H 0.582855 0.106605 0.293668 0.063 Uiso 1 1 calc R U . . .
H8C H 0.487052 0.052013 0.368246 0.063 Uiso 1 1 calc R U . . .
N1 N 0.4468(4) 0.2670(3) 0.6835(3) 0.0197(8) Uani 1 1 d . . . . .
Br1 Br 0.17684(5) 0.44764(3) 0.37754(3) 0.02098(11) Uani 1 1 d . . . . .
Br2 Br 0.25963(5) 0.53114(3) 0.64948(3) 0.01848(11) Uani 1 1 d . . . . .
Br3 Br -0.00904(5) 0.31522(3) 0.56019(3) 0.02049(11) Uani 1 1 d . . . . .
Br4 Br 0.62722(6) 0.56036(4) 0.85502(3) 0.02850(13) Uani 1 1 d . . . . .
Br5 Br 0.500000 0.500000 1.000000 0.02227(15) Uani 1 2 d S . P . .
Sb1 Sb 0.000000 0.500000 0.500000 0.01420(10) Uani 1 2 d S . 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
C1 N1 1.483(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.346(5) . ?
C2 C3 1.351(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.380(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.399(6) . ?
C4 C7 1.503(5) . ?
C5 C6 1.371(6) . ?
C5 H5 0.9500 . ?
C6 N1 1.335(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.500(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Br1 Sb1 2.5712(4) . ?
Br2 Sb1 2.5542(4) . ?
Br3 Sb1 2.5511(4) . ?
Br4 Br5 2.5561(5) . ?

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
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 120.8(4) . . ?
N1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C2 C3 C4 121.1(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C3 C4 C5 117.0(4) . . ?
C3 C4 C7 121.8(4) . . ?
C5 C4 C7 121.2(4) . . ?
C6 C5 C4 120.2(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
N1 C6 C5 120.4(4) . . ?
N1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C8 C7 C4 112.0(4) . . ?
C8 C7 H7A 109.2 . . ?
C4 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
C4 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 N1 C2 120.5(4) . . ?
C6 N1 C1 119.4(4) . . ?
C2 N1 C1 120.1(4) . . ?
Br4 Br5 Br4 180.0 . 3_667 ?
Br3 Sb1 Br3 180.0 . 3_566 ?
Br3 Sb1 Br2 89.779(14) . 3_566 ?
Br3 Sb1 Br2 90.221(14) 3_566 3_566 ?
Br3 Sb1 Br2 90.221(14) . . ?
Br3 Sb1 Br2 89.779(14) 3_566 . ?
Br2 Sb1 Br2 180.000(15) 3_566 . ?
Br3 Sb1 Br1 89.218(14) . 3_566 ?
Br3 Sb1 Br1 90.783(14) 3_566 3_566 ?
Br2 Sb1 Br1 89.972(14) 3_566 3_566 ?
Br2 Sb1 Br1 90.028(14) . 3_566 ?
Br3 Sb1 Br1 90.783(14) . . ?
Br3 Sb1 Br1 89.216(14) 3_566 . ?
Br2 Sb1 Br1 90.028(14) 3_566 . ?
Br2 Sb1 Br1 89.972(14) . . ?
Br1 Sb1 Br1 180.0 3_566 . ?

_refine_diff_density_max         0.655
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.152

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
####################################################################### 
# 
# 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_BM65_a
_database_code_depnum_ccdc_archive 'CCDC 1875701'
_audit_update_record             
;
2018-10-27 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_BM65_a              
;
PROBLEM: Check Calcd Positive Resid. Density on       Sb1       3.30 eA-3
RESPONSE: Residual density without any chemical sense
;
# Added during the CSD deposition process: Saturday 27 October 2018 03:22 PM
# end Validation Reply Form

#complex (C4H9NC5H5)[SbBr6]
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H14 Br6 N Sb'
_chemical_formula_weight         737.42

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'
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'
Sb Sb -0.5866 1.5461 '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'

_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                   7.4277(5)
_cell_length_b                   14.1293(8)
_cell_length_c                   16.7699(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1759.97(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    1656
_cell_measurement_theta_min      3.6510
_cell_measurement_theta_max      28.3920

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.783
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    15.171
_shelx_estimated_absorpt_T_min   0.085
_shelx_estimated_absorpt_T_max   0.209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.13321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            5901
_diffrn_reflns_av_unetI/netI     0.0868
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.328
_diffrn_reflns_theta_max         28.947
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3628
_reflns_number_gt                3067
_reflns_threshold_expression     >2σ(I)
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_max     0.860
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (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)+(0.0956P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_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   0.47(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3628
_refine_ls_number_parameters     155
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0674
_refine_ls_wR_factor_ref         0.1685
_refine_ls_wR_factor_gt          0.1544
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.046
_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
C1 C 0.765(4) 0.7614(14) 0.4526(15) 0.036(6) Uani 1 1 d . . . . .
H1A H 0.877451 0.748657 0.423888 0.053 Uiso 1 1 calc R U . . .
H1B H 0.746383 0.829960 0.456201 0.053 Uiso 1 1 calc R U . . .
H1C H 0.664184 0.732558 0.423852 0.053 Uiso 1 1 calc R U . . .
C2 C 0.776(3) 0.7203(16) 0.5350(13) 0.028(5) Uani 1 1 d . . . . .
H2A H 0.660841 0.731672 0.562913 0.033 Uiso 1 1 calc R U . . .
H2B H 0.872028 0.753517 0.565041 0.033 Uiso 1 1 calc R U . . .
C3 C 0.816(3) 0.6140(18) 0.5356(12) 0.034(6) Uani 1 1 d . . . . .
H3A H 0.918946 0.600883 0.499737 0.040 Uiso 1 1 calc R U . . .
H3B H 0.850978 0.594547 0.590158 0.040 Uiso 1 1 calc R U . . .
C4 C 0.659(3) 0.5575(15) 0.5097(12) 0.023(5) Uani 1 1 d . . . . .
H4A H 0.621715 0.578571 0.455947 0.027 Uiso 1 1 calc R U . . .
H4B H 0.557963 0.568766 0.546743 0.027 Uiso 1 1 calc R U . . .
C5 C 0.733(3) 0.4086(15) 0.4380(12) 0.022(4) Uani 1 1 d . U . . .
H5 H 0.722403 0.442276 0.389248 0.027 Uiso 1 1 calc R U . . .
C6 C 0.779(3) 0.3176(15) 0.4357(11) 0.030(5) Uani 1 1 d . . . . .
H6 H 0.805566 0.288751 0.385925 0.036 Uiso 1 1 calc R U . . .
C7 C 0.789(3) 0.2649(16) 0.5043(13) 0.027(5) Uani 1 1 d . . . . .
H7 H 0.820679 0.199718 0.502501 0.033 Uiso 1 1 calc R U . . .
C8 C 0.752(3) 0.3097(14) 0.5770(11) 0.025(5) Uani 1 1 d . . . . .
H8 H 0.759018 0.275539 0.625680 0.030 Uiso 1 1 calc R U . . .
C9 C 0.705(3) 0.4062(15) 0.5769(12) 0.023(4) Uani 1 1 d . U . . .
H9 H 0.676224 0.437114 0.625586 0.027 Uiso 1 1 calc R U . . .
N1 N 0.700(2) 0.4551(12) 0.5074(9) 0.019(4) Uani 1 1 d . . . . .
Br1 Br 0.5616(3) -0.14059(14) 0.25205(11) 0.0209(5) Uani 1 1 d . . . . .
Br2 Br 0.7136(3) 0.03868(15) 0.39243(10) 0.0220(5) Uani 1 1 d . . . . .
Br3 Br 0.4536(3) 0.10462(16) 0.22034(11) 0.0230(5) Uani 1 1 d . . . . .
Br4 Br 0.9285(3) 0.16278(15) 0.23292(11) 0.0238(5) Uani 1 1 d . . . . .
Br5 Br 0.7746(3) -0.01204(15) 0.09165(10) 0.0239(5) Uani 1 1 d . . . . .
Br6 Br 1.0319(3) -0.08381(15) 0.26442(11) 0.0227(5) Uani 1 1 d . . . . .
Sb1 Sb 0.74381(16) 0.01150(8) 0.24231(6) 0.0125(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.50(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.53(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.48(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N1 1.48(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.33(3) . ?
C5 N1 1.36(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.37(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.40(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.41(3) . ?
C8 H8 0.9500 . ?
C9 N1 1.36(2) . ?
C9 H9 0.9500 . ?
Br1 Sb1 2.545(2) . ?
Br2 Sb1 2.5565(19) . ?
Br3 Sb1 2.552(2) . ?
Br4 Sb1 2.545(2) . ?
Br5 Sb1 2.5587(19) . ?
Br6 Sb1 2.555(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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 C2 C3 113.4(17) . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
C3 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C4 C3 C2 112(2) . . ?
C4 C3 H3A 109.2 . . ?
C2 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 N1 112.2(18) . . ?
C3 C4 H4A 109.2 . . ?
N1 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
N1 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C6 C5 N1 122.6(18) . . ?
C6 C5 H5 118.7 . . ?
N1 C5 H5 118.7 . . ?
C5 C6 C7 121.0(19) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C6 C7 C8 118.2(19) . . ?
C6 C7 H7 120.9 . . ?
C8 C7 H7 120.9 . . ?
C7 C8 C9 119.1(18) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
N1 C9 C8 120.1(18) . . ?
N1 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 N1 C5 119.0(17) . . ?
C9 N1 C4 118.8(17) . . ?
C5 N1 C4 122.2(17) . . ?
Br4 Sb1 Br1 179.49(9) . . ?
Br4 Sb1 Br3 90.77(8) . . ?
Br1 Sb1 Br3 89.74(8) . . ?
Br4 Sb1 Br6 90.01(8) . . ?
Br1 Sb1 Br6 89.48(7) . . ?
Br3 Sb1 Br6 179.22(9) . . ?
Br4 Sb1 Br2 88.97(7) . . ?
Br1 Sb1 Br2 90.97(7) . . ?
Br3 Sb1 Br2 89.46(7) . . ?
Br6 Sb1 Br2 90.56(7) . . ?
Br4 Sb1 Br5 89.99(7) . . ?
Br1 Sb1 Br5 90.07(7) . . ?
Br3 Sb1 Br5 90.00(7) . . ?
Br6 Sb1 Br5 89.99(7) . . ?
Br2 Sb1 Br5 178.83(8) . . ?

_refine_diff_density_max         3.444
_refine_diff_density_min         -2.841
_refine_diff_density_rms         0.411

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
####################################################################### 
# 
# 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_3_a
_database_code_depnum_ccdc_archive 'CCDC 1875702'
_audit_update_record             
;
2018-10-27 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
#complex (C2H5NC5H3(CH3)2)[SbBr6]
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H14 Br6 N Sb'
_chemical_formula_weight         737.42

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'
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'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   9.9470(3)
_cell_length_b                   11.5017(3)
_cell_length_c                   16.4632(5)
_cell_angle_alpha                90
_cell_angle_beta                 107.201(3)
_cell_angle_gamma                90
_cell_volume                     1799.27(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    6488
_cell_measurement_theta_min      3.8160
_cell_measurement_theta_max      28.6790

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.722
_exptl_crystal_F_000             1344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    14.840
_shelx_estimated_absorpt_T_min   0.269
_shelx_estimated_absorpt_T_max   0.524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.27133
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            13341
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.325
_diffrn_reflns_theta_max         28.921
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4208
_reflns_number_gt                3610
_reflns_threshold_expression     >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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.0198P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4208
_refine_ls_number_parameters     157
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0220
_refine_ls_wR_factor_ref         0.0446
_refine_ls_wR_factor_gt          0.0425
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
C1 C 0.3664(3) 0.2820(2) 0.2279(2) 0.0259(7) Uani 1 1 d . . . . .
H1A H 0.316282 0.280627 0.166891 0.039 Uiso 1 1 calc R U . . .
H1B H 0.398766 0.203342 0.246953 0.039 Uiso 1 1 calc R U . . .
H1C H 0.447671 0.334146 0.238329 0.039 Uiso 1 1 calc R U . . .
C2 C 0.2681(3) 0.3251(2) 0.2765(2) 0.0217(7) Uani 1 1 d . . . . .
H2A H 0.185251 0.273131 0.264959 0.026 Uiso 1 1 calc R U . . .
H2B H 0.317368 0.322263 0.338280 0.026 Uiso 1 1 calc R U . . .
C3 C 0.0145(3) 0.3645(2) 0.1433(2) 0.0264(7) Uani 1 1 d . . . . .
H3A H 0.072595 0.314113 0.119253 0.040 Uiso 1 1 calc R U . . .
H3B H -0.066081 0.392948 0.097525 0.040 Uiso 1 1 calc R U . . .
H3C H -0.019235 0.320198 0.184220 0.040 Uiso 1 1 calc R U . . .
C4 C 0.1006(3) 0.4655(2) 0.18731(19) 0.0195(6) Uani 1 1 d . . . . .
C5 C 0.0599(3) 0.5782(2) 0.1628(2) 0.0252(7) Uani 1 1 d . . . . .
H5 H -0.024056 0.592045 0.117992 0.030 Uiso 1 1 calc R U . . .
C6 C 0.1405(3) 0.6704(2) 0.2031(2) 0.0270(7) Uani 1 1 d . . . . .
H6 H 0.113579 0.747811 0.185584 0.032 Uiso 1 1 calc R U . . .
C7 C 0.2600(4) 0.6495(2) 0.2686(2) 0.0300(8) Uani 1 1 d . . . . .
H7 H 0.314864 0.713081 0.297165 0.036 Uiso 1 1 calc R U . . .
C8 C 0.3020(3) 0.5372(2) 0.2937(2) 0.0237(7) Uani 1 1 d . . . . .
C9 C 0.4316(4) 0.5124(2) 0.3650(2) 0.0364(9) Uani 1 1 d . . . . .
H9A H 0.405436 0.477780 0.412555 0.055 Uiso 1 1 calc R U . . .
H9B H 0.483049 0.585010 0.383641 0.055 Uiso 1 1 calc R U . . .
H9C H 0.491627 0.458136 0.345577 0.055 Uiso 1 1 calc R U . . .
N1 N 0.2198(2) 0.44753(18) 0.25163(15) 0.0169(5) Uani 1 1 d . . . . .
Br1 Br 0.49538(3) 0.27947(2) -0.00384(2) 0.02414(8) Uani 1 1 d . . . . .
Br2 Br 0.28037(3) 0.50266(2) 0.04883(2) 0.02350(8) Uani 1 1 d . . . . .
Br3 Br 0.65367(3) 0.49241(2) 0.15400(2) 0.02287(8) Uani 1 1 d . . . . .
Br4 Br 0.91695(3) 0.52661(2) 0.33854(2) 0.02439(8) Uani 1 1 d . . . . .
Br5 Br 1.15909(3) 0.33366(2) 0.48291(2) 0.02449(8) Uani 1 1 d . . . . .
Br6 Br 1.19899(3) 0.64242(2) 0.51074(2) 0.02575(8) Uani 1 1 d . . . . .
Sb1 Sb 0.500000 0.500000 0.000000 0.01183(6) Uani 1 2 d S . P . .
Sb2 Sb 1.000000 0.500000 0.500000 0.01300(6) Uani 1 2 d S . 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
C1 C2 1.519(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.506(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.497(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 N1 1.352(4) . ?
C4 C5 1.382(4) . ?
C5 C6 1.376(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.369(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.383(4) . ?
C7 H7 0.9500 . ?
C8 N1 1.370(4) . ?
C8 C9 1.492(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
Br1 Sb1 2.5374(3) . ?
Br2 Sb1 2.5413(3) . ?
Br3 Sb1 2.5455(3) . ?
Br4 Sb2 2.5580(3) . ?
Br5 Sb2 2.5509(3) . ?
Br6 Sb2 2.5348(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 111.4(2) . . ?
N1 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 C5 119.0(3) . . ?
N1 C4 C3 120.3(2) . . ?
C5 C4 C3 120.7(3) . . ?
C6 C5 C4 120.2(3) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C7 C6 C5 119.4(3) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 121.0(3) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
N1 C8 C7 118.0(3) . . ?
N1 C8 C9 120.1(3) . . ?
C7 C8 C9 121.9(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 N1 C8 122.4(2) . . ?
C4 N1 C2 119.5(2) . . ?
C8 N1 C2 118.1(3) . . ?
Br1 Sb1 Br1 180.0 3_665 . ?
Br1 Sb1 Br2 89.487(8) 3_665 . ?
Br1 Sb1 Br2 90.513(8) . . ?
Br1 Sb1 Br2 90.513(8) 3_665 3_665 ?
Br1 Sb1 Br2 89.487(8) . 3_665 ?
Br2 Sb1 Br2 180.0 . 3_665 ?
Br1 Sb1 Br3 90.478(9) 3_665 . ?
Br1 Sb1 Br3 89.522(9) . . ?
Br2 Sb1 Br3 90.261(10) . . ?
Br2 Sb1 Br3 89.740(10) 3_665 . ?
Br1 Sb1 Br3 89.523(9) 3_665 3_665 ?
Br1 Sb1 Br3 90.477(9) . 3_665 ?
Br2 Sb1 Br3 89.740(10) . 3_665 ?
Br2 Sb1 Br3 90.260(10) 3_665 3_665 ?
Br3 Sb1 Br3 180.0 . 3_665 ?
Br6 Sb2 Br6 180.0 3_766 . ?
Br6 Sb2 Br5 90.271(10) 3_766 . ?
Br6 Sb2 Br5 89.730(10) . . ?
Br6 Sb2 Br5 89.728(10) 3_766 3_766 ?
Br6 Sb2 Br5 90.271(10) . 3_766 ?
Br5 Sb2 Br5 180.0 . 3_766 ?
Br6 Sb2 Br4 90.040(11) 3_766 3_766 ?
Br6 Sb2 Br4 89.960(10) . 3_766 ?
Br5 Sb2 Br4 90.268(10) . 3_766 ?
Br5 Sb2 Br4 89.731(10) 3_766 3_766 ?
Br6 Sb2 Br4 89.961(11) 3_766 . ?
Br6 Sb2 Br4 90.039(10) . . ?
Br5 Sb2 Br4 89.732(10) . . ?
Br5 Sb2 Br4 90.269(10) 3_766 . ?
Br4 Sb2 Br4 180.0 3_766 . ?

_refine_diff_density_max         0.684
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.120

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
####################################################################### 
# 
# 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_5_a
_database_code_depnum_ccdc_archive 'CCDC 1875704'
_audit_update_record             
;
2018-10-27 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
#complex (NC7H10)2[SbBr6]Br3
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H20 Br9 N2 Sb'
_chemical_formula_weight         1057.26

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'
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'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   7.2611(8)
_cell_length_b                   9.0862(10)
_cell_length_c                   11.1895(9)
_cell_angle_alpha                67.617(9)
_cell_angle_beta                 87.457(8)
_cell_angle_gamma                72.163(10)
_cell_volume                     647.61(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    1367
_cell_measurement_theta_min      4.3760
_cell_measurement_theta_max      28.2350

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.711
_exptl_crystal_F_000             484
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    14.952
_shelx_estimated_absorpt_T_min   0.050
_shelx_estimated_absorpt_T_max   0.381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.12768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            4812
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.391
_diffrn_reflns_theta_max         28.890
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2792
_reflns_number_gt                2244
_reflns_threshold_expression     >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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.0781P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2792
_refine_ls_number_parameters     121
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1371
_refine_ls_wR_factor_gt          0.1248
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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
C1 C 0.7807(15) 0.4836(12) 0.9253(8) 0.037(2) Uani 1 1 d . . . . .
H1A H 0.685156 0.432864 0.973827 0.055 Uiso 1 1 calc R U . . .
H1B H 0.748094 0.599188 0.919456 0.055 Uiso 1 1 calc R U . . .
H1C H 0.910279 0.418941 0.970092 0.055 Uiso 1 1 calc R U . . .
C2 C 0.8725(12) 0.3474(10) 0.7717(8) 0.0250(18) Uani 1 1 d . . . . .
H2 H 0.944928 0.248794 0.841357 0.030 Uiso 1 1 calc R U . . .
C3 C 0.8655(14) 0.3487(12) 0.6477(9) 0.035(2) Uani 1 1 d . . . . .
H3 H 0.931818 0.251207 0.631478 0.042 Uiso 1 1 calc R U . . .
C4 C 0.7606(13) 0.4941(11) 0.5485(8) 0.031(2) Uani 1 1 d . . . . .
H4 H 0.754650 0.496629 0.463014 0.037 Uiso 1 1 calc R U . . .
C5 C 0.6651(12) 0.6342(10) 0.5713(8) 0.0255(18) Uani 1 1 d . . . . .
C6 C 0.6730(11) 0.6270(10) 0.6959(8) 0.0219(17) Uani 1 1 d . . . . .
H6 H 0.604852 0.722339 0.714390 0.026 Uiso 1 1 calc R U . . .
C7 C 0.5500(14) 0.7949(11) 0.4655(8) 0.035(2) Uani 1 1 d . . . . .
H7A H 0.444833 0.857386 0.502402 0.052 Uiso 1 1 calc R U . . .
H7B H 0.494930 0.769617 0.400044 0.052 Uiso 1 1 calc R U . . .
H7C H 0.635131 0.862539 0.425176 0.052 Uiso 1 1 calc R U . . .
N1 N 0.7786(10) 0.4832(8) 0.7928(6) 0.0216(14) Uani 1 1 d . . . . .
Br1 Br 0.78355(12) -0.06060(10) 0.86493(7) 0.0263(2) Uani 1 1 d . . . . .
Br2 Br 0.38224(12) 0.30809(10) 0.84460(7) 0.0225(2) Uani 1 1 d . . . . .
Br3 Br 0.29664(12) -0.07288(10) 0.86412(7) 0.0258(2) Uani 1 1 d . . . . .
Br4 Br 0.12911(13) 0.71874(10) 0.68894(8) 0.0291(2) Uani 1 1 d . . . . .
Br5 Br 0.000000 1.000000 0.500000 0.0243(3) Uani 1 2 d S . P . .
Sb1 Sb 0.500000 0.000000 1.000000 0.0172(2) Uani 1 2 d S . 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
C1 N1 1.485(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.317(11) . ?
C2 C3 1.386(12) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.364(12) . ?
C4 H4 0.9500 . ?
C5 C6 1.373(11) . ?
C5 C7 1.501(12) . ?
C6 N1 1.361(10) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
Br1 Sb1 2.5475(8) . ?
Br2 Sb1 2.5592(8) . ?
Br3 Sb1 2.5486(7) . ?
Br4 Br5 2.5442(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
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 119.9(8) . . ?
N1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 118.7(9) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C5 C4 C3 120.9(8) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 118.6(8) . . ?
C4 C5 C7 122.3(8) . . ?
C6 C5 C7 119.0(8) . . ?
N1 C6 C5 119.9(8) . . ?
N1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 N1 C6 122.0(7) . . ?
C2 N1 C1 120.8(7) . . ?
C6 N1 C1 117.2(7) . . ?
Br4 Br5 Br4 180.0 . 2_576 ?
Br1 Sb1 Br1 180.00(3) . 2_657 ?
Br1 Sb1 Br3 89.00(3) . . ?
Br1 Sb1 Br3 91.00(3) 2_657 . ?
Br1 Sb1 Br3 91.01(3) . 2_657 ?
Br1 Sb1 Br3 88.99(3) 2_657 2_657 ?
Br3 Sb1 Br3 180.0 . 2_657 ?
Br1 Sb1 Br2 89.01(3) . 2_657 ?
Br1 Sb1 Br2 90.99(3) 2_657 2_657 ?
Br3 Sb1 Br2 89.55(3) . 2_657 ?
Br3 Sb1 Br2 90.45(3) 2_657 2_657 ?
Br1 Sb1 Br2 90.99(3) . . ?
Br1 Sb1 Br2 89.01(3) 2_657 . ?
Br3 Sb1 Br2 90.45(3) . . ?
Br3 Sb1 Br2 89.55(3) 2_657 . ?
Br2 Sb1 Br2 180.00(4) 2_657 . ?

_refine_diff_density_max         1.865
_refine_diff_density_min         -2.545
_refine_diff_density_rms         0.296

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
####################################################################### 
# 
# 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_9_a
_database_code_depnum_ccdc_archive 'CCDC 1875708'
_audit_update_record             
;
2018-10-27 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
#complex (NC5H5-CH2-C5H4Br)2[SbBr6]Br3
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H22 Br11 N2 Sb'
_chemical_formula_weight         1339.19

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'
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'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   8.6483(4)
_cell_length_b                   15.1885(9)
_cell_length_c                   13.3520(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.887(4)
_cell_angle_gamma                90
_cell_volume                     1732.79(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    2725
_cell_measurement_theta_min      3.7370
_cell_measurement_theta_max      28.4910

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.567
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    13.498
_shelx_estimated_absorpt_T_min   0.173
_shelx_estimated_absorpt_T_max   0.345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.54625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            8438
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.318
_diffrn_reflns_theta_max         28.899
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.835
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3805
_reflns_number_gt                3055
_reflns_threshold_expression     >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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.0235P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3805
_refine_ls_number_parameters     175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0597
_refine_ls_wR_factor_gt          0.0551
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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
C1 C 0.7282(4) 0.4018(3) 0.7746(3) 0.0253(10) Uani 1 1 d . . . . .
H1 H 0.813328 0.427434 0.818367 0.030 Uiso 1 1 calc R U . . .
N1 N 0.5849(3) 0.4374(2) 0.7661(2) 0.0170(7) Uani 1 1 d . . . . .
C2 C 0.7506(5) 0.3276(3) 0.7194(3) 0.0342(11) Uani 1 1 d . . . . .
H2 H 0.851664 0.301744 0.725290 0.041 Uiso 1 1 calc R U . . .
C3 C 0.6275(6) 0.2908(3) 0.6559(3) 0.0342(11) Uani 1 1 d . . . . .
H3 H 0.642860 0.239530 0.617999 0.041 Uiso 1 1 calc R U . . .
C4 C 0.4822(5) 0.3288(3) 0.6477(3) 0.0283(10) Uani 1 1 d . . . . .
H4 H 0.396140 0.304574 0.603437 0.034 Uiso 1 1 calc R U . . .
C5 C 0.4631(4) 0.4017(3) 0.7038(3) 0.0203(9) Uani 1 1 d . . . . .
H5 H 0.362429 0.427854 0.699194 0.024 Uiso 1 1 calc R U . . .
C6 C 0.7409(5) 0.6382(3) 0.7757(3) 0.0258(9) Uani 1 1 d . . . . .
H6 H 0.820735 0.615572 0.826019 0.031 Uiso 1 1 calc R U . . .
C7 C 0.7720(5) 0.7092(3) 0.7170(3) 0.0267(9) Uani 1 1 d . . . . .
H7 H 0.873368 0.734859 0.725727 0.032 Uiso 1 1 calc R U . . .
C8 C 0.6538(5) 0.7424(2) 0.6455(3) 0.0224(9) Uani 1 1 d . . . . .
C9 C 0.5061(5) 0.7066(3) 0.6309(3) 0.0221(9) Uani 1 1 d . . . . .
H9 H 0.425808 0.730442 0.581778 0.026 Uiso 1 1 calc R U . . .
C10 C 0.4771(4) 0.6349(3) 0.6893(3) 0.0208(9) Uani 1 1 d . . . . .
H10 H 0.375703 0.609207 0.679812 0.025 Uiso 1 1 calc R U . . .
C11 C 0.5608(5) 0.5199(3) 0.8215(3) 0.0249(9) Uani 1 1 d . . . . .
H11A H 0.631227 0.520147 0.887452 0.030 Uiso 1 1 calc R U . . .
H11B H 0.451610 0.522151 0.835184 0.030 Uiso 1 1 calc R U . . .
C12 C 0.5932(4) 0.5999(2) 0.7614(3) 0.0194(9) Uani 1 1 d . . . . .
Br1 Br 0.07509(4) 0.51062(3) 0.69290(3) 0.02872(12) Uani 1 1 d . . . . .
Br2 Br 0.28739(4) 0.49452(3) 0.47721(3) 0.02272(11) Uani 1 1 d . . . . .
Br3 Br 0.00507(5) 0.66755(3) 0.48873(3) 0.03334(12) Uani 1 1 d . . . . .
Br4 Br 1.000000 0.000000 0.500000 0.01919(13) Uani 1 2 d S . P . .
Br5 Br 0.79061(5) 0.10015(3) 0.54963(3) 0.03343(12) Uani 1 1 d . . . . .
Br6 Br 0.69724(6) 0.84254(3) 0.56892(3) 0.03767(13) Uani 1 1 d . . . . .
Sb1 Sb 0.000000 0.500000 0.500000 0.01742(9) Uani 1 2 d S . 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
C1 N1 1.341(5) . ?
C1 C2 1.376(6) . ?
C1 H1 0.9500 . ?
N1 C5 1.351(5) . ?
N1 C11 1.487(5) . ?
C2 C3 1.373(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.371(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.362(5) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.385(5) . ?
C6 C12 1.389(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.382(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.374(5) . ?
C8 Br6 1.902(4) . ?
C9 C10 1.386(5) . ?
C9 H9 0.9500 . ?
C10 C12 1.385(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.506(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
Br1 Sb1 2.5622(4) . ?
Br2 Sb1 2.5516(4) . ?
Br3 Sb1 2.5501(5) . ?
Br4 Br5 2.5304(4) 3_756 ?
Br4 Br5 2.5304(4) . ?

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
N1 C1 C2 119.3(4) . . ?
N1 C1 H1 120.3 . . ?
C2 C1 H1 120.3 . . ?
C1 N1 C5 120.9(3) . . ?
C1 N1 C11 119.8(3) . . ?
C5 N1 C11 119.3(3) . . ?
C3 C2 C1 120.2(4) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C4 C3 C2 119.5(4) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C5 C4 C3 119.0(4) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
N1 C5 C4 121.0(4) . . ?
N1 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C7 C6 C12 120.2(4) . . ?
C7 C6 H6 119.9 . . ?
C12 C6 H6 119.9 . . ?
C8 C7 C6 119.2(4) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C7 121.7(4) . . ?
C9 C8 Br6 119.8(3) . . ?
C7 C8 Br6 118.5(3) . . ?
C8 C9 C10 118.5(4) . . ?
C8 C9 H9 120.8 . . ?
C10 C9 H9 120.8 . . ?
C12 C10 C9 121.2(3) . . ?
C12 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
N1 C11 C12 111.3(3) . . ?
N1 C11 H11A 109.4 . . ?
C12 C11 H11A 109.4 . . ?
N1 C11 H11B 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C10 C12 C6 119.2(4) . . ?
C10 C12 C11 120.3(3) . . ?
C6 C12 C11 120.4(4) . . ?
Br5 Br4 Br5 180.0 3_756 . ?
Br3 Sb1 Br3 180.000(19) 3_566 . ?
Br3 Sb1 Br2 89.975(13) 3_566 3_566 ?
Br3 Sb1 Br2 90.025(13) . 3_566 ?
Br3 Sb1 Br2 90.026(13) 3_566 . ?
Br3 Sb1 Br2 89.975(13) . . ?
Br2 Sb1 Br2 180.0 3_566 . ?
Br3 Sb1 Br1 89.572(14) 3_566 3_566 ?
Br3 Sb1 Br1 90.428(14) . 3_566 ?
Br2 Sb1 Br1 91.241(12) 3_566 3_566 ?
Br2 Sb1 Br1 88.760(12) . 3_566 ?
Br3 Sb1 Br1 90.429(14) 3_566 . ?
Br3 Sb1 Br1 89.571(14) . . ?
Br2 Sb1 Br1 88.759(12) 3_566 . ?
Br2 Sb1 Br1 91.241(12) . . ?
Br1 Sb1 Br1 179.999(16) 3_566 . ?

_refine_diff_density_max         0.714
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.133

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
####################################################################### 
# 
# 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_11_a
_database_code_depnum_ccdc_archive 'CCDC 1875710'
_audit_update_record             
;
2018-10-27 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_11_a                
;
PROBLEM: Check Calcd Resid. Dens.  0.79A   From Br2            -3.55 eA-3
RESPONSE: Residual density without any chemical sense
;
_vrf_PLAT973_11_a                
;
PROBLEM: Check Calcd Positive Resid. Density on       Sb1       3.81 eA-3
RESPONSE: Residual density without any chemical sense
;
# Added during the CSD deposition process: Saturday 27 October 2018 03:22 PM
# end Validation Reply Form

#complex (NC5H5Br)2[SbBr6]Br3
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H10 Br11 N2 Sb'
_chemical_formula_weight         1158.96

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'
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'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   7.3255(4)
_cell_length_b                   20.6666(10)
_cell_length_c                   16.5665(7)
_cell_angle_alpha                90
_cell_angle_beta                 95.627(4)
_cell_angle_gamma                90
_cell_volume                     2496.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    3229
_cell_measurement_theta_min      3.8290
_cell_measurement_theta_max      28.6360

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.084
_exptl_crystal_F_000             2080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    18.715
_shelx_estimated_absorpt_T_min   0.050
_shelx_estimated_absorpt_T_max   0.166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.04016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            10924
_diffrn_reflns_av_unetI/netI     0.1171
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.420
_diffrn_reflns_theta_max         28.863
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.827
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5408
_reflns_number_gt                3737
_reflns_threshold_expression     >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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.1469P)²+10.1836P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5408
_refine_ls_number_parameters     220
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.0906
_refine_ls_wR_factor_ref         0.2655
_refine_ls_wR_factor_gt          0.2310
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.085
_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
C1 C -0.108(2) 0.4727(10) 0.3546(10) 0.033(4) Uani 1 1 d . . . . .
H1 H -0.145483 0.482751 0.406489 0.040 Uiso 1 1 calc R U . . .
C2 C -0.091(3) 0.5197(9) 0.3007(11) 0.037(5) Uani 1 1 d . . . . .
H2 H -0.115017 0.563430 0.313878 0.045 Uiso 1 1 calc R U . . .
C3 C -0.037(2) 0.5037(8) 0.2249(9) 0.022(3) Uani 1 1 d . U . . .
C4 C -0.001(2) 0.4432(8) 0.2072(10) 0.027(4) Uani 1 1 d . . . . .
H4 H 0.036196 0.432406 0.155622 0.032 Uiso 1 1 calc R U . . .
C5 C -0.019(2) 0.3954(10) 0.2647(11) 0.037(5) Uani 1 1 d . . . . .
H5 H 0.007485 0.351475 0.253837 0.044 Uiso 1 1 calc R U . . .
C6 C 0.482(2) 0.1460(7) 0.3626(9) 0.022(3) Uani 1 1 d . . . . .
H6 H 0.465829 0.119326 0.408098 0.027 Uiso 1 1 calc R U . . .
C7 C 0.462(2) 0.2126(8) 0.3672(9) 0.026(4) Uani 1 1 d . . . . .
H7 H 0.431755 0.232004 0.416142 0.032 Uiso 1 1 calc R U . . .
C8 C 0.4860(19) 0.2503(8) 0.3015(8) 0.016(3) Uani 1 1 d . U . . .
C9 C 0.528(3) 0.2208(9) 0.2290(10) 0.032(4) Uani 1 1 d . . . . .
H9 H 0.541831 0.246026 0.182084 0.039 Uiso 1 1 calc R U . . .
C10 C 0.548(2) 0.1565(12) 0.2276(10) 0.044(6) Uani 1 1 d . . . . .
H10 H 0.580392 0.136140 0.179570 0.053 Uiso 1 1 calc R U . . .
N1 N 0.5239(18) 0.1201(7) 0.2930(7) 0.026(3) Uani 1 1 d . . . . .
H1A H 0.536027 0.077840 0.289832 0.031 Uiso 1 1 calc R U . . .
N2 N -0.074(2) 0.4133(8) 0.3360(8) 0.035(4) Uani 1 1 d . . . . .
H2A H -0.087792 0.383011 0.372272 0.042 Uiso 1 1 calc R U . . .
Br1 Br -0.2432(2) 0.18031(9) 0.56280(9) 0.0272(4) Uani 1 1 d . . . . .
Br2 Br 0.0296(2) 0.28859(9) 0.69662(8) 0.0245(4) Uani 1 1 d . . . . .
Br3 Br -0.2415(2) 0.35328(9) 0.52126(9) 0.0291(4) Uani 1 1 d . . . . .
Br4 Br 0.2457(2) 0.35027(9) 0.52534(9) 0.0293(4) Uani 1 1 d . . . . .
Br5 Br -0.0287(2) 0.24455(8) 0.39055(8) 0.0243(4) Uani 1 1 d . . . . .
Br6 Br 0.2439(2) 0.17668(9) 0.56578(9) 0.0266(4) Uani 1 1 d . . . . .
Br7 Br 0.500000 0.500000 0.500000 0.0196(5) Uani 1 2 d S . P . .
Br8 Br 0.4052(2) 0.49528(8) 0.34833(9) 0.0279(4) Uani 1 1 d . . . . .
Br9 Br 0.500000 0.500000 0.000000 0.0239(5) Uani 1 2 d S . P . .
Br10 Br 0.4864(2) 0.46610(9) 0.14718(8) 0.0289(4) Uani 1 1 d . . . . .
Br11 Br 0.4637(2) 0.33911(8) 0.30673(9) 0.0295(4) Uani 1 1 d . . . . .
Br12 Br -0.0143(3) 0.56888(10) 0.14696(11) 0.0409(5) Uani 1 1 d . . . . .
Sb1 Sb 0.00255(13) 0.26480(5) 0.54446(5) 0.0180(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.30(2) . ?
C1 C2 1.33(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.39(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.32(2) . ?
C3 Br12 1.885(16) . ?
C4 C5 1.39(2) . ?
C4 H4 0.9500 . ?
C5 N2 1.34(2) . ?
C5 H5 0.9500 . ?
C6 N1 1.33(2) . ?
C6 C7 1.39(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.36(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.41(2) . ?
C8 Br11 1.846(16) . ?
C9 C10 1.34(3) . ?
C9 H9 0.9500 . ?
C10 N1 1.35(2) . ?
C10 H10 0.9500 . ?
N1 H1A 0.8800 . ?
N2 H2A 0.8800 . ?
Br1 Sb1 2.5472(19) . ?
Br2 Sb1 2.5567(15) . ?
Br3 Sb1 2.5599(19) . ?
Br4 Sb1 2.550(2) . ?
Br5 Sb1 2.5719(15) . ?
Br6 Sb1 2.5386(19) . ?
Br7 Br8 2.5422(14) . ?
Br7 Br8 2.5423(14) 3_666 ?
Br9 Br10 2.5482(15) 3_665 ?
Br9 Br10 2.5482(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
N2 C1 C2 119.8(16) . . ?
N2 C1 H1 120.1 . . ?
C2 C1 H1 120.1 . . ?
C1 C2 C3 119.0(17) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 120.4(16) . . ?
C4 C3 Br12 119.5(12) . . ?
C2 C3 Br12 120.1(13) . . ?
C3 C4 C5 119.3(17) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N2 C5 C4 117.9(18) . . ?
N2 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?
N1 C6 C7 118.7(14) . . ?
N1 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
C8 C7 C6 120.0(15) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 119.3(16) . . ?
C7 C8 Br11 120.7(12) . . ?
C9 C8 Br11 119.9(12) . . ?
C10 C9 C8 118.6(15) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C9 C10 N1 121.2(17) . . ?
C9 C10 H10 119.4 . . ?
N1 C10 H10 119.4 . . ?
C6 N1 C10 122.2(17) . . ?
C6 N1 H1A 118.9 . . ?
C10 N1 H1A 118.9 . . ?
C1 N2 C5 123.6(16) . . ?
C1 N2 H2A 118.2 . . ?
C5 N2 H2A 118.2 . . ?
Br8 Br7 Br8 180.00(8) . 3_666 ?
Br10 Br9 Br10 180.00(8) 3_665 . ?
Br6 Sb1 Br1 88.99(7) . . ?
Br6 Sb1 Br4 91.64(7) . . ?
Br1 Sb1 Br4 179.34(7) . . ?
Br6 Sb1 Br2 90.87(6) . . ?
Br1 Sb1 Br2 90.10(6) . . ?
Br4 Sb1 Br2 90.10(6) . . ?
Br6 Sb1 Br3 179.34(6) . . ?
Br1 Sb1 Br3 90.93(7) . . ?
Br4 Sb1 Br3 88.43(7) . . ?
Br2 Sb1 Br3 89.78(6) . . ?
Br6 Sb1 Br5 90.82(6) . . ?
Br1 Sb1 Br5 90.65(6) . . ?
Br4 Sb1 Br5 89.13(6) . . ?
Br2 Sb1 Br5 178.16(7) . . ?
Br3 Sb1 Br5 88.53(6) . . ?

_refine_diff_density_max         3.153
_refine_diff_density_min         -3.525
_refine_diff_density_rms         0.558

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2

####################################################################### 
# 
# 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_6_a
_database_code_depnum_ccdc_archive 'CCDC 1875705'
_audit_update_record             
;
2018-10-27 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
#complex (C2H5NC5H4CH3)2[SbBr6]Br3
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H24 Br9 N2 Sb'
_chemical_formula_weight         1085.31

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'
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'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   7.2472(3)
_cell_length_b                   9.4088(5)
_cell_length_c                   11.5541(5)
_cell_angle_alpha                69.263(4)
_cell_angle_beta                 81.162(4)
_cell_angle_gamma                71.303(4)
_cell_volume                     697.20(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    2446
_cell_measurement_theta_min      3.7590
_cell_measurement_theta_max      28.2570

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.585
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    13.892
_shelx_estimated_absorpt_T_min   0.189
_shelx_estimated_absorpt_T_max   0.403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.40844
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            5318
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.447
_diffrn_reflns_theta_max         28.896
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3012
_reflns_number_gt                2526
_reflns_threshold_expression     >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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.0179P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3012
_refine_ls_number_parameters     130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0662
_refine_ls_wR_factor_gt          0.0615
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.991
_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
C1 C 0.2988(7) 0.0583(6) 0.4268(5) 0.0217(12) Uani 1 1 d . . . . .
H1A H 0.377173 -0.012585 0.381086 0.033 Uiso 1 1 calc R U . . .
H1B H 0.267134 -0.004955 0.510847 0.033 Uiso 1 1 calc R U . . .
H1C H 0.372845 0.126984 0.430946 0.033 Uiso 1 1 calc R U . . .
C2 C 0.1142(7) 0.1584(6) 0.3617(5) 0.0233(12) Uani 1 1 d . . . . .
H2A H 0.046964 0.089373 0.348251 0.028 Uiso 1 1 calc R U . . .
H2B H 0.026250 0.218523 0.413720 0.028 Uiso 1 1 calc R U . . .
C3 C 0.1282(7) 0.4227(6) 0.2269(5) 0.0248(13) Uani 1 1 d . . . . .
H3 H 0.073069 0.460780 0.294212 0.030 Uiso 1 1 calc R U . . .
C4 C 0.1758(7) 0.5248(7) 0.1176(5) 0.0273(13) Uani 1 1 d . . . . .
H4 H 0.153150 0.633517 0.107949 0.033 Uiso 1 1 calc R U . . .
C5 C 0.2571(7) 0.4675(6) 0.0219(5) 0.0260(13) Uani 1 1 d . . . . .
H5 H 0.292152 0.537413 -0.054453 0.031 Uiso 1 1 calc R U . . .
C6 C 0.3834(8) 0.2423(7) -0.0680(5) 0.0336(14) Uani 1 1 d . . . . .
H6A H 0.525503 0.210736 -0.063904 0.050 Uiso 1 1 calc R U . . .
H6B H 0.344584 0.323134 -0.148250 0.050 Uiso 1 1 calc R U . . .
H6C H 0.341244 0.149541 -0.058573 0.050 Uiso 1 1 calc R U . . .
C7 C 0.2892(7) 0.3093(6) 0.0345(5) 0.0218(12) Uani 1 1 d . . . . .
C8 C 0.2349(7) 0.2141(6) 0.1470(5) 0.0207(12) Uani 1 1 d . . . . .
H8 H 0.252390 0.105603 0.158558 0.025 Uiso 1 1 calc R U . . .
N1 N 0.1578(5) 0.2703(5) 0.2410(4) 0.0178(9) Uani 1 1 d . . . . .
Br1 Br 0.60442(6) 0.36484(6) 0.33415(5) 0.01702(12) Uani 1 1 d . . . . .
Br2 Br 0.23760(6) 0.71907(6) 0.35849(5) 0.01910(13) Uani 1 1 d . . . . .
Br3 Br 0.25554(6) 0.34269(6) 0.59259(5) 0.01962(13) Uani 1 1 d . . . . .
Br4 Br 0.78374(8) 0.08638(7) 0.17312(6) 0.03072(15) Uani 1 1 d . . . . .
Br5 Br 1.000000 0.000000 0.000000 0.02189(17) Uani 1 2 d S . P . .
Sb1 Sb 0.500000 0.500000 0.500000 0.01321(12) Uani 1 2 d S . 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
C1 C2 1.497(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.480(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N1 1.334(6) . ?
C3 C4 1.362(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.371(7) . ?
C4 H4 0.9500 . ?
C5 C7 1.388(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.507(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.375(7) . ?
C8 N1 1.341(6) . ?
C8 H8 0.9500 . ?
Br1 Sb1 2.5544(5) . ?
Br2 Sb1 2.5678(5) . ?
Br3 Sb1 2.5400(5) . ?
Br4 Br5 2.5473(6) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 110.2(4) . . ?
N1 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N1 C3 C4 121.1(5) . . ?
N1 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C3 C4 C5 118.7(5) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
C4 C5 C7 121.2(5) . . ?
C4 C5 H5 119.4 . . ?
C7 C5 H5 119.4 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C5 116.7(5) . . ?
C8 C7 C6 121.0(5) . . ?
C5 C7 C6 122.3(5) . . ?
N1 C8 C7 121.8(5) . . ?
N1 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C3 N1 C8 120.5(5) . . ?
C3 N1 C2 120.8(5) . . ?
C8 N1 C2 118.7(4) . . ?
Br4 Br5 Br4 180.0 2_755 . ?
Br3 Sb1 Br3 180.0 2_666 . ?
Br3 Sb1 Br1 90.206(16) 2_666 . ?
Br3 Sb1 Br1 89.793(16) . . ?
Br3 Sb1 Br1 89.794(16) 2_666 2_666 ?
Br3 Sb1 Br1 90.207(16) . 2_666 ?
Br1 Sb1 Br1 180.0 . 2_666 ?
Br3 Sb1 Br2 90.623(16) 2_666 . ?
Br3 Sb1 Br2 89.377(16) . . ?
Br1 Sb1 Br2 89.516(16) . . ?
Br1 Sb1 Br2 90.484(16) 2_666 . ?
Br3 Sb1 Br2 89.378(16) 2_666 2_666 ?
Br3 Sb1 Br2 90.623(16) . 2_666 ?
Br1 Sb1 Br2 90.484(16) . 2_666 ?
Br1 Sb1 Br2 89.516(16) 2_666 2_666 ?
Br2 Sb1 Br2 180.0 . 2_666 ?

_refine_diff_density_max         0.797
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.177

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
####################################################################### 
# 
# 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_7_a
_database_code_depnum_ccdc_archive 'CCDC 1875706'
_audit_update_record             
;
2018-10-27 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
#complex (CH3C5H4NCH2C6H5)2SbBr6Br3
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H28 Br9 N2 Sb'
_chemical_formula_weight         1209.44

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'
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'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   8.9834(4)
_cell_length_b                   10.2599(5)
_cell_length_c                   10.3601(5)
_cell_angle_alpha                94.223(4)
_cell_angle_beta                 102.737(4)
_cell_angle_gamma                111.846(4)
_cell_volume                     851.62(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    2711
_cell_measurement_theta_min      3.9320
_cell_measurement_theta_max      28.6360

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.358
_exptl_crystal_F_000             564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    11.387
_shelx_estimated_absorpt_T_min   0.209
_shelx_estimated_absorpt_T_max   0.396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.55206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            6184
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.491
_diffrn_reflns_theta_max         28.847
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.818
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.818
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.818
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             3645
_reflns_number_gt                2988
_reflns_threshold_expression     >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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.0139P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3645
_refine_ls_number_parameters     175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0590
_refine_ls_wR_factor_gt          0.0539
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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
C1 C 0.8632(6) 0.9375(5) 0.2231(4) 0.0245(11) Uani 1 1 d . . . . .
H1A H 0.905579 0.863777 0.209372 0.037 Uiso 1 1 calc R U . . .
H1B H 0.956756 1.029091 0.262410 0.037 Uiso 1 1 calc R U . . .
H1C H 0.798907 0.945446 0.136582 0.037 Uiso 1 1 calc R U . . .
C2 C 0.7543(6) 0.8984(5) 0.3154(4) 0.0178(10) Uani 1 1 d . . . . .
C3 C 0.7889(6) 0.9835(5) 0.4370(4) 0.0242(11) Uani 1 1 d . . . . .
H3 H 0.885761 1.069883 0.463400 0.029 Uiso 1 1 calc R U . . .
C4 C 0.6856(6) 0.9455(5) 0.5209(4) 0.0255(12) Uani 1 1 d . . . . .
H4 H 0.711798 1.004594 0.604652 0.031 Uiso 1 1 calc R U . . .
C5 C 0.5460(6) 0.8226(5) 0.4827(4) 0.0263(12) Uani 1 1 d . . . . .
H5 H 0.473497 0.794869 0.539177 0.032 Uiso 1 1 calc R U . . .
C6 C 0.5114(6) 0.7390(5) 0.3606(4) 0.0235(11) Uani 1 1 d . . . . .
H6 H 0.413433 0.653584 0.332871 0.028 Uiso 1 1 calc R U . . .
C7 C 0.5700(6) 0.6818(5) 0.1477(4) 0.0242(11) Uani 1 1 d . . . . .
H7A H 0.540976 0.732322 0.074673 0.029 Uiso 1 1 calc R U . . .
H7B H 0.669673 0.665959 0.138636 0.029 Uiso 1 1 calc R U . . .
C8 C 0.4288(6) 0.5400(5) 0.1297(4) 0.0195(10) Uani 1 1 d . . . . .
C9 C 0.2683(6) 0.5191(5) 0.0612(4) 0.0224(11) Uani 1 1 d . . . . .
H9 H 0.247187 0.594921 0.025147 0.027 Uiso 1 1 calc R U . . .
C10 C 0.1388(6) 0.3872(5) 0.0455(4) 0.0308(12) Uani 1 1 d . . . . .
H10 H 0.028531 0.372930 -0.000290 0.037 Uiso 1 1 calc R U . . .
C11 C 0.1704(7) 0.2768(5) 0.0964(4) 0.0343(13) Uani 1 1 d . . . . .
H11 H 0.081258 0.186583 0.085003 0.041 Uiso 1 1 calc R U . . .
C12 C 0.3297(7) 0.2955(5) 0.1637(4) 0.0322(13) Uani 1 1 d . . . . .
H12 H 0.350742 0.218960 0.198282 0.039 Uiso 1 1 calc R U . . .
C13 C 0.4580(6) 0.4277(5) 0.1800(4) 0.0266(12) Uani 1 1 d . . . . .
H13 H 0.568006 0.441756 0.226389 0.032 Uiso 1 1 calc R U . . .
N1 N 0.6129(4) 0.7757(4) 0.2806(3) 0.0176(8) Uani 1 1 d . . . . .
Br1 Br 0.76927(6) 0.58006(5) 0.52630(4) 0.02531(12) Uani 1 1 d . . . . .
Br2 Br 0.79674(6) 0.29915(5) 0.30778(4) 0.02367(12) Uani 1 1 d . . . . .
Br3 Br 0.93311(6) 0.33547(5) 0.67153(4) 0.02458(12) Uani 1 1 d . . . . .
Br4 Br 0.71600(7) 0.09711(5) 0.87101(4) 0.03011(13) Uani 1 1 d . . . . .
Br5 Br 0.500000 0.000000 1.000000 0.02029(15) Uani 1 2 d S . P . .
Sb1 Sb 1.000000 0.500000 0.500000 0.01627(11) Uani 1 2 d S . 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
C1 C2 1.486(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.367(5) . ?
C2 C3 1.382(6) . ?
C3 C4 1.380(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.360(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.378(5) . ?
C5 H5 0.9500 . ?
C6 N1 1.336(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.497(6) . ?
C7 N1 1.506(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C13 1.386(6) . ?
C8 C9 1.387(6) . ?
C9 C10 1.387(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(6) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
Br1 Sb1 2.5551(5) . ?
Br2 Sb1 2.5570(4) . ?
Br3 Sb1 2.5546(4) . ?
Br4 Br5 2.5385(5) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 117.5(4) . . ?
N1 C2 C1 120.2(4) . . ?
C3 C2 C1 122.3(4) . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 119.5(4) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 118.9(5) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
N1 C6 C5 121.3(4) . . ?
N1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C8 C7 N1 114.2(3) . . ?
C8 C7 H7A 108.7 . . ?
N1 C7 H7A 108.7 . . ?
C8 C7 H7B 108.7 . . ?
N1 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C13 C8 C9 119.4(4) . . ?
C13 C8 C7 120.1(4) . . ?
C9 C8 C7 120.5(4) . . ?
C10 C9 C8 119.8(4) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C11 C10 C9 119.9(5) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 121.0(5) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C13 118.8(5) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C12 C13 C8 121.1(5) . . ?
C12 C13 H13 119.5 . . ?
C8 C13 H13 119.5 . . ?
C6 N1 C2 121.5(4) . . ?
C6 N1 C7 119.6(4) . . ?
C2 N1 C7 118.9(4) . . ?
Br4 Br5 Br4 180.0 . 2_657 ?
Br3 Sb1 Br3 179.999(11) 2_766 . ?
Br3 Sb1 Br1 89.993(16) 2_766 . ?
Br3 Sb1 Br1 90.008(16) . . ?
Br3 Sb1 Br1 90.007(16) 2_766 2_766 ?
Br3 Sb1 Br1 89.993(16) . 2_766 ?
Br1 Sb1 Br1 180.0 . 2_766 ?
Br3 Sb1 Br2 89.149(15) 2_766 . ?
Br3 Sb1 Br2 90.851(15) . . ?
Br1 Sb1 Br2 91.055(15) . . ?
Br1 Sb1 Br2 88.945(15) 2_766 . ?
Br3 Sb1 Br2 90.850(15) 2_766 2_766 ?
Br3 Sb1 Br2 89.150(15) . 2_766 ?
Br1 Sb1 Br2 88.945(15) . 2_766 ?
Br1 Sb1 Br2 91.055(16) 2_766 2_766 ?
Br2 Sb1 Br2 180.00(2) . 2_766 ?

_refine_diff_density_max         0.658
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.145

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
####################################################################### 
# 
# 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_4_a
_database_code_depnum_ccdc_archive 'CCDC 1875703'
_audit_update_record             
;
2018-10-27 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
#complex (NC5H5I)2[SbBr6]Br3 
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H10 Br9 I2 N2 Sb'
_chemical_formula_weight         1252.94

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'
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'
Sb Sb -0.5866 1.5461 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   8.1800(5)
_cell_length_b                   12.9394(8)
_cell_length_c                   12.5865(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.412(7)
_cell_angle_gamma                90
_cell_volume                     1284.30(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    1623
_cell_measurement_theta_min      4.6260
_cell_measurement_theta_max      28.8370

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.240
_exptl_crystal_F_000             1112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_exptl_absorpt_coefficient_mu    17.479
_shelx_estimated_absorpt_T_min   0.042
_shelx_estimated_absorpt_T_max   0.054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.36090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            5485
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.358
_diffrn_reflns_theta_max         29.015
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2811
_reflns_number_gt                2293
_reflns_threshold_expression     >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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.0280P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2811
_refine_ls_number_parameters     112
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.0829
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
C1 C 0.3801(10) 0.6546(6) 0.6281(6) 0.0217(18) Uani 1 1 d . . . . .
H1 H 0.322298 0.600755 0.654466 0.026 Uiso 1 1 calc R U . . .
C2 C 0.4473(10) 0.7361(6) 0.6956(6) 0.0186(17) Uani 1 1 d . . . . .
H2 H 0.436271 0.739787 0.768773 0.022 Uiso 1 1 calc R U . . .
C3 C 0.5331(10) 0.8142(5) 0.6536(6) 0.0201(17) Uani 1 1 d . . . . .
H3 H 0.582417 0.871003 0.698603 0.024 Uiso 1 1 calc R U . . .
C4 C 0.5446(10) 0.8070(5) 0.5459(6) 0.0177(17) Uani 1 1 d . . . . .
H4 H 0.599813 0.860002 0.516272 0.021 Uiso 1 1 calc R U . . .
C5 C 0.4762(9) 0.7235(5) 0.4819(5) 0.0147(16) Uani 1 1 d . . . . .
N1 N 0.3965(8) 0.6512(4) 0.5245(5) 0.0162(13) Uani 1 1 d . . . . .
H1A H 0.352220 0.598348 0.482695 0.019 Uiso 1 1 calc R U . . .
Br1 Br 0.18687(9) 0.96126(5) 0.37184(6) 0.01474(17) Uani 1 1 d . . . . .
Br2 Br -0.01144(10) 0.80603(5) 0.53922(6) 0.01620(18) Uani 1 1 d . . . . .
Br3 Br 0.26485(10) 1.01886(5) 0.66050(6) 0.01566(17) Uani 1 1 d . . . . .
Br4 Br 0.18761(10) 0.45612(5) 0.37413(6) 0.01880(18) Uani 1 1 d . . . . .
Br5 Br 0.000000 0.500000 0.500000 0.0155(2) Uani 1 2 d S . P . .
Sb1 Sb 0.000000 1.000000 0.500000 0.00935(16) Uani 1 2 d S . P . .
I1 I 0.49689(7) 0.70199(4) 0.32289(4) 0.02256(15) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.347(8) . ?
C1 C2 1.374(10) . ?
C1 H1 0.9500 . ?
C2 C3 1.410(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.387(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.376(10) . ?
C4 H4 0.9500 . ?
C5 N1 1.331(8) . ?
C5 I1 2.071(6) . ?
N1 H1A 0.8800 . ?
Br1 Sb1 2.5496(6) . ?
Br2 Sb1 2.5644(6) . ?
Br3 Sb1 2.5511(8) . ?
Br4 Br5 2.5455(7) . ?

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
N1 C1 C2 119.8(6) . . ?
N1 C1 H1 120.1 . . ?
C2 C1 H1 120.1 . . ?
C1 C2 C3 118.4(6) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 119.2(7) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C5 C4 C3 120.2(7) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
N1 C5 C4 118.8(6) . . ?
N1 C5 I1 118.0(5) . . ?
C4 C5 I1 123.1(5) . . ?
C5 N1 C1 123.5(6) . . ?
C5 N1 H1A 118.2 . . ?
C1 N1 H1A 118.2 . . ?
Br4 Br5 Br4 180.0 . 3_566 ?
Br1 Sb1 Br1 180.0 . 3_576 ?
Br1 Sb1 Br3 90.34(2) . 3_576 ?
Br1 Sb1 Br3 89.66(2) 3_576 3_576 ?
Br1 Sb1 Br3 89.66(2) . . ?
Br1 Sb1 Br3 90.34(2) 3_576 . ?
Br3 Sb1 Br3 180.0 3_576 . ?
Br1 Sb1 Br2 89.31(2) . . ?
Br1 Sb1 Br2 90.68(2) 3_576 . ?
Br3 Sb1 Br2 89.55(2) 3_576 . ?
Br3 Sb1 Br2 90.45(2) . . ?
Br1 Sb1 Br2 90.69(2) . 3_576 ?
Br1 Sb1 Br2 89.31(2) 3_576 3_576 ?
Br3 Sb1 Br2 90.45(2) 3_576 3_576 ?
Br3 Sb1 Br2 89.55(2) . 3_576 ?
Br2 Sb1 Br2 180.0 . 3_576 ?

_refine_diff_density_max         1.283
_refine_diff_density_min         -1.580
_refine_diff_density_rms         0.280

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
####################################################################### 
# 
# 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_10_a
_database_code_depnum_ccdc_archive 'CCDC 1875709'
_audit_update_record             
;
2018-10-27 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT434_10_a                
;
PROBLEM: Short Inter HL..HL Contact Br6      ..Br7              2.94 Ang.
RESPONSE: Br...Br non valence interaction
;
# Added during the CSD deposition process: Saturday 27 October 2018 03:22 PM
# end Validation Reply Form

#complex (NC6H7Br)2[SbBr6]Br3
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H14 Br11 N2 Sb'
_chemical_formula_weight         1187.01

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'
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'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_H-M_alt        'I m'
_space_group_name_Hall           'I -2y'

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

_cell_length_a                   8.4041(9)
_cell_length_b                   13.3407(16)
_cell_length_c                   12.2371(11)
_cell_angle_alpha                90
_cell_angle_beta                 95.731(9)
_cell_angle_gamma                90
_cell_volume                     1365.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    1706
_cell_measurement_theta_min      4.3120
_cell_measurement_theta_max      28.4800

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.888
_exptl_crystal_F_000             1072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    17.113
_shelx_estimated_absorpt_T_min   0.079
_shelx_estimated_absorpt_T_max   0.131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.30294
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            3259
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.154
_diffrn_reflns_theta_max         28.677
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             2096
_reflns_number_gt                2025
_reflns_threshold_expression     >2σ(I)
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_max     0.831
_reflns_Friedel_fraction_full    0.990

_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (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)+(0.1041P)²+14.9071P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_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   0.54(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2096
_refine_ls_number_parameters     91
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0555
_refine_ls_wR_factor_ref         0.1539
_refine_ls_wR_factor_gt          0.1514
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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
Br1 Br 0.3425(3) 0.500000 0.3740(2) 0.0243(6) Uani 1 2 d S T P . .
Br2 Br 0.1476(3) 0.500000 0.62417(18) 0.0233(6) Uani 1 2 d S T P . .
Br3 Br -0.2378(3) 0.500000 0.4638(2) 0.0248(6) Uani 1 2 d S T P . .
Br4 Br -0.0411(3) 0.500000 0.21687(18) 0.0239(6) Uani 1 2 d S T P . .
Br5 Br 0.0524(2) 0.69242(13) 0.42080(17) 0.0242(4) Uani 1 1 d . . . . .
Br6 Br 0.6080(3) 1.000000 0.4283(2) 0.0199(5) Uani 1 2 d S T P . .
Br7 Br 0.9558(3) 1.000000 0.4151(2) 0.0237(6) Uani 1 2 d S T P . .
Br8 Br 1.2387(3) 1.000000 0.4363(2) 0.0257(6) Uani 1 2 d S T P . .
Sb1 Sb 0.05275(19) 0.500000 0.42076(13) 0.0132(3) Uani 1 2 d S T P . .
Br9 Br 0.4398(3) 0.73399(19) 0.55221(19) 0.0337(5) Uiso 0.92 1 d . . P A 1
C1A C 0.648(2) 0.7426(16) 0.6206(14) 0.023(4) Uiso 0.92 1 d . . P A 1
C2A C 0.709(2) 0.6683(18) 0.6906(17) 0.028(4) Uiso 0.92 1 d . . P A 1
H2A H 0.647363 0.611451 0.706461 0.034 Uiso 0.92 1 calc R U P A 1
C3A C 0.871(2) 0.6809(17) 0.7385(16) 0.025(4) Uiso 0.92 1 d . . P A 1
H3A H 0.916810 0.631599 0.787956 0.030 Uiso 0.92 1 calc R U P A 1
C4A C 0.961(2) 0.7644(16) 0.7139(15) 0.024(4) Uiso 0.92 1 d . . P A 1
N1 N 0.737(2) 0.8203(16) 0.6006(15) 0.032(4) Uiso 0.92 1 d . . P A 1
H1 H 0.696139 0.867162 0.555625 0.038 Uiso 0.92 1 calc R U P A 1
C8 C 0.888(3) 0.8312(17) 0.6453(17) 0.030(4) Uiso 0.92 1 d . . P A 1
H8 H 0.945024 0.889269 0.627485 0.037 Uiso 0.92 1 calc R U P A 1
C5 C 1.1661(18) 0.7631(14) 0.7853(13) 0.049(4) Uiso 0.92 1 d . . P A 1
H5A H 1.226030 0.820720 0.761410 0.073 Uiso 0.92 1 calc R U P A 1
H5B H 1.220162 0.700964 0.767464 0.073 Uiso 0.92 1 calc R U P A 1
H5C H 1.160462 0.766795 0.864798 0.073 Uiso 0.92 1 calc R U P A 1
C6 C 0.4398(3) 0.73399(19) 0.55221(19) 0.0337(5) Uiso 0.08 1 d . . P B 2
H6A H 0.378510 0.792735 0.571672 0.050 Uiso 0.08 1 calc R U P B 2
H6B H 0.388739 0.673010 0.576591 0.050 Uiso 0.08 1 calc R U P B 2
H6C H 0.442779 0.731723 0.472399 0.050 Uiso 0.08 1 calc R U P B 2
C1B C 0.648(2) 0.7426(16) 0.6206(14) 0.023(4) Uiso 0.08 1 d . . P B 2
C2B C 0.709(2) 0.6683(18) 0.6906(17) 0.028(4) Uiso 0.08 1 d . . P B 2
H2B H 0.647363 0.611451 0.706461 0.034 Uiso 0.08 1 calc R U P B 2
C3B C 0.871(2) 0.6809(17) 0.7385(16) 0.025(4) Uiso 0.08 1 d . . P B 2
H3B H 0.916810 0.631599 0.787956 0.030 Uiso 0.08 1 calc R U P B 2
C4B C 0.961(2) 0.7644(16) 0.7139(15) 0.024(4) Uiso 0.08 1 d . . P B 2
Br10 Br 1.1661(18) 0.7631(14) 0.7853(13) 0.049(4) Uiso 0.08 1 d . . P B 2
N2 N 0.888(3) 0.8312(17) 0.6453(17) 0.030(4) Uiso 0.08 1 d . . P B 2
H2 H 0.940795 0.884986 0.628801 0.037 Uiso 0.08 1 calc R U P B 2
C7 C 0.737(2) 0.8203(16) 0.6006(15) 0.032(4) Uiso 0.08 1 d . . P B 2
H7 H 0.692861 0.870886 0.552051 0.038 Uiso 0.08 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Sb1 2.556(3) . ?
Br2 Sb1 2.537(3) . ?
Br3 Sb1 2.549(3) . ?
Br4 Sb1 2.540(3) . ?
Br5 Sb1 2.5670(17) . ?
Br7 Br8 2.365(4) . ?
Br9 C1A 1.864(19) . ?
C1A N1 1.32(3) . ?
C1A C2A 1.38(3) . ?
C2A C3A 1.43(3) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.40(3) . ?
C3A H3A 0.9500 . ?
C4A C8 1.33(3) . ?
C4A C5 1.85(2) . ?
N1 C8 1.33(3) . ?
N1 H1 0.8800 . ?
C8 H8 0.9500 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C1B 1.864(19) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C1B C7 1.32(3) . ?
C1B C2B 1.38(3) . ?
C2B C3B 1.43(3) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.40(3) . ?
C3B H3B 0.9500 . ?
C4B N2 1.33(3) . ?
C4B Br10 1.85(2) . ?
N2 C7 1.33(3) . ?
N2 H2 0.8800 . ?
C7 H7 0.9500 . ?

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
Br2 Sb1 Br4 179.78(11) . . ?
Br2 Sb1 Br3 90.62(9) . . ?
Br4 Sb1 Br3 89.60(10) . . ?
Br2 Sb1 Br1 90.38(10) . . ?
Br4 Sb1 Br1 89.40(10) . . ?
Br3 Sb1 Br1 179.00(12) . . ?
Br2 Sb1 Br5 90.00(6) . . ?
Br4 Sb1 Br5 90.00(6) . . ?
Br3 Sb1 Br5 89.93(6) . . ?
Br1 Sb1 Br5 90.07(6) . . ?
Br2 Sb1 Br5 90.00(6) . 2_565 ?
Br4 Sb1 Br5 90.00(6) . 2_565 ?
Br3 Sb1 Br5 89.93(6) . 2_565 ?
Br1 Sb1 Br5 90.07(6) . 2_565 ?
Br5 Sb1 Br5 179.85(12) . 2_565 ?
N1 C1A C2A 119.7(18) . . ?
N1 C1A Br9 119.5(15) . . ?
C2A C1A Br9 120.8(15) . . ?
C1A C2A C3A 117(2) . . ?
C1A C2A H2A 121.6 . . ?
C3A C2A H2A 121.6 . . ?
C4A C3A C2A 121.3(19) . . ?
C4A C3A H3A 119.4 . . ?
C2A C3A H3A 119.4 . . ?
C8 C4A C3A 116.0(19) . . ?
C8 C4A C5 130.9(18) . . ?
C3A C4A C5 113.1(16) . . ?
C1A N1 C8 123(2) . . ?
C1A N1 H1 118.5 . . ?
C8 N1 H1 118.5 . . ?
C4A C8 N1 123(2) . . ?
C4A C8 H8 118.4 . . ?
N1 C8 H8 118.4 . . ?
C4A C5 H5A 109.5 . . ?
C4A C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4A C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C1B C6 H6A 109.5 . . ?
C1B C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C1B C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 C1B C2B 119.7(18) . . ?
C7 C1B C6 119.5(15) . . ?
C2B C1B C6 120.8(15) . . ?
C1B C2B C3B 117(2) . . ?
C1B C2B H2B 121.6 . . ?
C3B C2B H2B 121.6 . . ?
C4B C3B C2B 121.3(19) . . ?
C4B C3B H3B 119.4 . . ?
C2B C3B H3B 119.4 . . ?
N2 C4B C3B 116.0(19) . . ?
N2 C4B Br10 130.9(18) . . ?
C3B C4B Br10 113.1(16) . . ?
C4B N2 C7 123(2) . . ?
C4B N2 H2 118.4 . . ?
C7 N2 H2 118.4 . . ?
C1B C7 N2 123(2) . . ?
C1B C7 H7 118.5 . . ?
N2 C7 H7 118.5 . . ?

_refine_diff_density_max         2.703
_refine_diff_density_min         -2.862
_refine_diff_density_rms         0.478

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
