# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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. 
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data_SbBrDIBA250K
_database_code_depnum_ccdc_archive 'CCDC 1475468'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;

_chemical_name_systematic        
;
Bis(diisobutylammonium) octabromodiantimonate(III)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H20 N, Br4 Sb'
_chemical_formula_sum            'C8 H20 Br4 N Sb'
_chemical_formula_weight         571.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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                   5.964(2)
_cell_length_b                   20.098(8)
_cell_length_c                   14.385(8)
_cell_angle_alpha                90
_cell_angle_beta                 99.25(5)
_cell_angle_gamma                90
_cell_volume                     1701.8(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    3373
_cell_measurement_theta_min      3.0346
_cell_measurement_theta_max      28.6414

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.231
_exptl_crystal_F_000             1064
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    10.987
_shelx_estimated_absorpt_T_min   0.073
_shelx_estimated_absorpt_T_max   0.242
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.35463
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28c (release 15-05-2013 CrysAlis171 .NET)
(compiled May 15 2013,09:16:53)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3359
_diffrn_reflns_number            7558
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.043
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measured_fraction_theta_full 0.918
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 0.918
_reflns_number_total             2824
_reflns_number_gt                1934
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0810P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2824
_refine_ls_number_parameters     232
_refine_ls_number_restraints     175
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.1210
_refine_ls_wR_factor_gt          0.1133
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_restrained_S_all      0.895
_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
Sb Sb 0.51344(8) 0.58099(2) 0.11704(4) 0.0440(2) Uani 1 1 d . . . . .
Br1 Br 0.08699(15) 0.56836(5) 0.09586(9) 0.0813(4) Uani 1 1 d . . . . .
Br2 Br 0.53588(13) 0.42618(4) 0.10574(6) 0.0533(3) Uani 1 1 d . . . . .
Br3 Br 0.4949(2) 0.70853(4) 0.11592(8) 0.0946(4) Uani 1 1 d . . . . .
Br4 Br 0.5757(2) 0.57398(5) 0.29617(7) 0.0830(4) Uani 1 1 d . . . . .
N N 0.0645(11) 0.3731(3) 0.1869(5) 0.0651(19) Uani 1 1 d D . . . .
H11 H -0.0269 0.3898 0.1293 0.078 Uiso 0.6409 1 d . U P A 1
H12 H 0.2221 0.3680 0.1748 0.078 Uiso 0.6409 1 d . U P A 1
H13 H 0.1178 0.4087 0.1615 0.078 Uiso 0.3591 1 d . U P A 2
H14 H -0.0783 0.3797 0.1955 0.078 Uiso 0.3591 1 d . U P A 2
C11 C 0.057(3) 0.4212(7) 0.2709(9) 0.073(4) Uani 0.641(9) 1 d D . P A 1
H1A H 0.1223 0.4638 0.2557 0.087 Uiso 0.641(9) 1 calc R U P A 1
H1B H -0.1026 0.4293 0.2759 0.087 Uiso 0.641(9) 1 calc R U P A 1
C21 C 0.176(4) 0.3996(11) 0.3643(16) 0.094(4) Uani 0.641(9) 1 d . U P A 1
H21 H 0.1122 0.3562 0.3796 0.113 Uiso 0.641(9) 1 calc R U P A 1
C31 C 0.144(3) 0.4483(9) 0.4402(13) 0.104(4) Uani 0.641(9) 1 d . U P A 1
H3A H 0.1682 0.4932 0.4189 0.156 Uiso 0.641(9) 1 calc R U P A 1
H3B H 0.2517 0.4388 0.4965 0.156 Uiso 0.641(9) 1 calc R U P A 1
H3C H -0.0096 0.4445 0.4541 0.156 Uiso 0.641(9) 1 calc R U P A 1
C41 C 0.438(3) 0.3911(10) 0.3667(14) 0.097(4) Uani 0.641(9) 1 d . U P A 1
H4A H 0.4879 0.4209 0.3211 0.145 Uiso 0.641(9) 1 calc R U P A 1
H4B H 0.4703 0.3455 0.3513 0.145 Uiso 0.641(9) 1 calc R U P A 1
H4C H 0.5171 0.4017 0.4292 0.145 Uiso 0.641(9) 1 calc R U P A 1
C12 C 0.217(4) 0.3557(11) 0.2810(11) 0.062(7) Uani 0.359(9) 1 d D U P A 2
H12A H 0.1449 0.3223 0.3162 0.075 Uiso 0.359(9) 1 calc R U P A 2
H12B H 0.3656 0.3392 0.2707 0.075 Uiso 0.359(9) 1 calc R U P A 2
C22 C 0.236(5) 0.4163(13) 0.327(2) 0.064(8) Uani 0.359(9) 1 d . U P A 2
H22 H 0.3197 0.4471 0.2914 0.076 Uiso 0.359(9) 1 calc R U P A 2
C32 C 0.386(6) 0.4043(17) 0.427(3) 0.097(5) Uani 0.359(9) 1 d . U P A 2
H32A H 0.4624 0.4453 0.4488 0.146 Uiso 0.359(9) 1 calc R U P A 2
H32B H 0.4977 0.3701 0.4216 0.146 Uiso 0.359(9) 1 calc R U P A 2
H32C H 0.2890 0.3901 0.4713 0.146 Uiso 0.359(9) 1 calc R U P A 2
C42 C 0.016(6) 0.4505(18) 0.342(3) 0.104(5) Uani 0.359(9) 1 d . U P A 2
H42A H 0.0455 0.4795 0.3967 0.157 Uiso 0.359(9) 1 calc R U P A 2
H42B H -0.0953 0.4171 0.3524 0.157 Uiso 0.359(9) 1 calc R U P A 2
H42C H -0.0432 0.4766 0.2869 0.157 Uiso 0.359(9) 1 calc R U P A 2
C51 C -0.022(3) 0.3031(5) 0.2074(11) 0.074(5) Uani 0.641(9) 1 d D . P A 1
H51A H 0.0933 0.2787 0.2504 0.089 Uiso 0.641(9) 1 calc R U P A 1
H51B H -0.1608 0.3061 0.2356 0.089 Uiso 0.641(9) 1 calc R U P A 1
C61 C -0.067(4) 0.2707(11) 0.1165(15) 0.091(6) Uani 0.641(9) 1 d . U P A 1
H61 H -0.1837 0.2966 0.0747 0.109 Uiso 0.641(9) 1 calc R U P A 1
C52 C 0.068(7) 0.3137(14) 0.119(2) 0.121(13) Uani 0.359(9) 1 d D U P A 2
H52A H -0.0295 0.3262 0.0597 0.145 Uiso 0.359(9) 1 calc R U P A 2
H52B H 0.2233 0.3111 0.1043 0.145 Uiso 0.359(9) 1 calc R U P A 2
C62 C 0.001(5) 0.2429(13) 0.141(2) 0.057(7) Uani 0.359(9) 1 d . U P A 2
H62 H 0.1074 0.2260 0.1964 0.069 Uiso 0.359(9) 1 calc R U P A 2
C71 C -0.167(5) 0.2040(14) 0.136(2) 0.090(5) Uani 0.49(2) 1 d . U P A 1
H71A H -0.3133 0.2107 0.1567 0.135 Uiso 0.49(2) 1 calc R U P A 1
H71B H -0.0654 0.1814 0.1858 0.135 Uiso 0.49(2) 1 calc R U P A 1
H71C H -0.1876 0.1771 0.0798 0.135 Uiso 0.49(2) 1 calc R U P A 1
C81 C 0.135(5) 0.2612(14) 0.068(2) 0.089(5) Uani 0.49(2) 1 d . U P A 1
H81A H 0.0843 0.2500 0.0026 0.133 Uiso 0.49(2) 1 calc R U P A 1
H81B H 0.2285 0.2255 0.0987 0.133 Uiso 0.49(2) 1 calc R U P A 1
H81C H 0.2225 0.3020 0.0722 0.133 Uiso 0.49(2) 1 calc R U P A 1
C72 C -0.240(7) 0.250(2) 0.168(3) 0.088(6) Uani 0.269(10) 1 d . U P A 2
H72A H -0.2413 0.2878 0.2106 0.132 Uiso 0.269(10) 1 calc R U P A 2
H72B H -0.2789 0.2100 0.1991 0.132 Uiso 0.269(10) 1 calc R U P A 2
H72C H -0.3494 0.2578 0.1117 0.132 Uiso 0.269(10) 1 calc R U P A 2
C82 C 0.000(7) 0.198(2) 0.062(3) 0.089(5) Uani 0.269(10) 1 d . U P A 2
H82A H 0.1504 0.1968 0.0445 0.133 Uiso 0.269(10) 1 calc R U P A 2
H82B H -0.1092 0.2133 0.0094 0.133 Uiso 0.269(10) 1 calc R U P A 2
H82C H -0.0410 0.1535 0.0801 0.133 Uiso 0.269(10) 1 calc R U P A 2
C73 C 0.227(10) 0.250(2) 0.102(4) 0.086(6) Uani 0.25(2) 1 d . U P A 3
H73A H 0.3500 0.2617 0.0680 0.129 Uiso 0.25(2) 1 calc R U P A 3
H73B H 0.0832 0.2538 0.0595 0.129 Uiso 0.25(2) 1 calc R U P A 3
H73C H 0.2470 0.2048 0.1246 0.129 Uiso 0.25(2) 1 calc R U P A 3
C83 C -0.109(10) 0.183(3) 0.110(4) 0.088(6) Uani 0.25(2) 1 d . U P A 3
H83A H -0.2375 0.1529 0.1057 0.132 Uiso 0.25(2) 1 calc R U P A 3
H83B H 0.0309 0.1570 0.1185 0.132 Uiso 0.25(2) 1 calc R U P A 3
H83C H -0.1195 0.2083 0.0519 0.132 Uiso 0.25(2) 1 calc R U P A 3


_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
Sb Br1 2.5253(13) . ?
Sb Br4 2.5476(18) . ?
Sb Br3 2.5656(14) . ?
Sb Br2 3.1196(16) . ?
Sb Br2 3.174(2) 3_665 ?
Sb Br1 3.4918(16) 1_655 ?
N C51 1.543(9) . ?
N C12 1.544(10) . ?
N C52 1.549(10) . ?
N C11 1.554(9) . ?
N H11 0.9757 . ?
N H12 0.9884 . ?
N H13 0.8861 . ?
N H14 0.8899 . ?
C11 C21 1.48(2) . ?
C11 H1A 0.9800 . ?
C11 H1B 0.9800 . ?
C21 C31 1.50(3) . ?
C21 C41 1.57(3) . ?
C21 H21 0.9900 . ?
C31 H3A 0.9700 . ?
C31 H3B 0.9700 . ?
C31 H3C 0.9700 . ?
C41 H4A 0.9700 . ?
C41 H4B 0.9700 . ?
C41 H4C 0.9700 . ?
C12 C22 1.38(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C22 C42 1.53(4) . ?
C22 C32 1.58(4) . ?
C22 H22 0.9900 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 H42C 0.9700 . ?
C51 C61 1.45(2) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C61 C81 1.50(3) . ?
C61 C71 1.51(3) . ?
C61 C83 1.78(6) . ?
C61 C73 1.85(6) . ?
C61 H61 0.9900 . ?
C52 C62 1.53(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C62 C82 1.45(5) . ?
C62 C72 1.55(5) . ?
C62 H62 0.9900 . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C71 H71C 0.9700 . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C81 H81C 0.9700 . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
C72 H72C 0.9700 . ?
C82 H82A 0.9700 . ?
C82 H82B 0.9700 . ?
C82 H82C 0.9700 . ?
C73 H73A 0.9700 . ?
C73 H73B 0.9700 . ?
C73 H73C 0.9700 . ?
C83 H83A 0.9700 . ?
C83 H83B 0.9700 . ?
C83 H83C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Sb Br4 95.55(7) . . ?
Br1 Sb Br3 93.33(4) . . ?
Br4 Sb Br3 93.48(4) . . ?
Br1 Sb Br2 86.80(3) . . ?
Br4 Sb Br2 89.83(3) . . ?
Br3 Sb Br2 176.66(4) . . ?
Br1 Sb Br2 86.88(6) . 3_665 ?
Br4 Sb Br2 173.49(3) . 3_665 ?
Br3 Sb Br2 92.41(3) . 3_665 ?
Br2 Sb Br2 84.26(2) . 3_665 ?
Br1 Sb Br1 164.56(5) . 1_655 ?
Br4 Sb Br1 95.67(6) . 1_655 ?
Br3 Sb Br1 96.55(4) . 1_655 ?
Br2 Sb Br1 82.65(3) . 1_655 ?
Br2 Sb Br1 80.89(6) 3_665 1_655 ?
C12 N C52 108.4(17) . . ?
C51 N C11 111.5(10) . . ?
C51 N H11 108.5 . . ?
C11 N H11 111.3 . . ?
C51 N H12 107.3 . . ?
C11 N H12 110.4 . . ?
H11 N H12 107.6 . . ?
C12 N H13 110.2 . . ?
C52 N H13 108.6 . . ?
C12 N H14 110.7 . . ?
C52 N H14 108.4 . . ?
H13 N H14 110.5 . . ?
C21 C11 N 117.0(12) . . ?
C21 C11 H1A 108.0 . . ?
N C11 H1A 108.0 . . ?
C21 C11 H1B 108.0 . . ?
N C11 H1B 108.0 . . ?
H1A C11 H1B 107.3 . . ?
C11 C21 C31 111.7(15) . . ?
C11 C21 C41 112.4(19) . . ?
C31 C21 C41 107.4(16) . . ?
C11 C21 H21 108.4 . . ?
C31 C21 H21 108.4 . . ?
C41 C21 H21 108.4 . . ?
C21 C31 H3A 109.5 . . ?
C21 C31 H3B 109.5 . . ?
H3A C31 H3B 109.5 . . ?
C21 C31 H3C 109.5 . . ?
H3A C31 H3C 109.5 . . ?
H3B C31 H3C 109.5 . . ?
C21 C41 H4A 109.5 . . ?
C21 C41 H4B 109.5 . . ?
H4A C41 H4B 109.5 . . ?
C21 C41 H4C 109.5 . . ?
H4A C41 H4C 109.5 . . ?
H4B C41 H4C 109.5 . . ?
C22 C12 N 102.3(17) . . ?
C22 C12 H12A 111.3 . . ?
N C12 H12A 111.3 . . ?
C22 C12 H12B 111.3 . . ?
N C12 H12B 111.3 . . ?
H12A C12 H12B 109.2 . . ?
C12 C22 C42 117(3) . . ?
C12 C22 C32 107(2) . . ?
C42 C22 C32 108(3) . . ?
C12 C22 H22 108.0 . . ?
C42 C22 H22 108.0 . . ?
C32 C22 H22 108.0 . . ?
C22 C32 H32A 109.5 . . ?
C22 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C22 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C22 C42 H42A 109.5 . . ?
C22 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C22 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C61 C51 N 104.9(13) . . ?
C61 C51 H51A 110.8 . . ?
N C51 H51A 110.8 . . ?
C61 C51 H51B 110.8 . . ?
N C51 H51B 110.8 . . ?
H51A C51 H51B 108.8 . . ?
C51 C61 C81 115.4(19) . . ?
C51 C61 C71 104.5(18) . . ?
C81 C61 C71 110(2) . . ?
C83 C61 C73 84(3) . . ?
C51 C61 H61 108.8 . . ?
C81 C61 H61 108.8 . . ?
C71 C61 H61 108.8 . . ?
C62 C52 N 123(3) . . ?
C62 C52 H52A 106.5 . . ?
N C52 H52A 106.5 . . ?
C62 C52 H52B 106.5 . . ?
N C52 H52B 106.5 . . ?
H52A C52 H52B 106.5 . . ?
C82 C62 C52 112(3) . . ?
C82 C62 C72 112(3) . . ?
C52 C62 C72 104(3) . . ?
C82 C62 H62 109.5 . . ?
C52 C62 H62 109.5 . . ?
C72 C62 H62 109.5 . . ?
C61 C71 H71A 109.5 . . ?
C61 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C61 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C61 C81 H81A 109.5 . . ?
C61 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C61 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C62 C72 H72A 109.5 . . ?
C62 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C62 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C62 C82 H82A 109.5 . . ?
C62 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C62 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C51_a N C11_a C21_a 54.5(19) . . . . ?
C12 N C11 C21 -8.8(18) . . . . ?
C52 N C11 C21 37(8) . . . . ?
N C11 C21 C31 -176.4(15) . . . . ?
N C11 C21 C41 63(2) . . . . ?
C51 N C12 C22 -143(2) . . . . ?
C52 N C12 C22 168(2) . . . . ?
C11 N C12 C22 -20.7(18) . . . . ?
N C12 C22 C42 57(3) . . . . ?
N C12 C22 C32 179(2) . . . . ?
C12 N C51 C61 -141.6(17) . . . . ?
C52 N C51 C61 -20(2) . . . . ?
C11 N C51 C61 164.0(13) . . . . ?
N C51 C61 C81 62(2) . . . . ?
N C51 C61 C71 -176.2(16) . . . . ?
N C51 C61 C83 166(3) . . . . ?
N C51 C61 C73 77(2) . . . . ?
C51 N C52 C62 -5(2) . . . . ?
C12 N C52 C62 57(4) . . . . ?
C11 N C52 C62 15(11) . . . . ?
N C52 C62 C82 175(3) . . . . ?
N C52 C62 C72 54(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N H14 Br2 0.89 2.62 3.355(7) 140.2 1_455
N H12 Br2 0.99 2.54 3.386(7) 143.4 .

_refine_diff_density_max         0.894
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.191

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method water
####################################################################### 
# 
# 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_SbBrDIBA100K
_database_code_depnum_ccdc_archive 'CCDC 1475469'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
Bis(diisobutylammonium) octabromodiantimonate(III)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H20 N, Br4 Sb'
_chemical_formula_sum            'C8 H20 Br4 N Sb'
_chemical_formula_weight         571.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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                   6.046(2)
_cell_length_b                   18.186(3)
_cell_length_c                   14.839(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.32(2)
_cell_angle_gamma                90
_cell_volume                     1621.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11923
_cell_measurement_theta_min      2.9750
_cell_measurement_theta_max      36.8817

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.341
_exptl_crystal_F_000             1064
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    11.530
_shelx_estimated_absorpt_T_min   0.069
_shelx_estimated_absorpt_T_max   0.231
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.077
_exptl_absorpt_correction_T_max  0.274
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28c (release 15-05-2013 CrysAlis171 .NET)
(compiled May 15 2013,09:16:53)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3359
_diffrn_reflns_number            21768
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.981
_diffrn_reflns_theta_max         36.972
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.779
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.779
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6414
_reflns_number_gt                4633
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0387P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6414
_refine_ls_number_parameters     131
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0752
_refine_ls_wR_factor_gt          0.0724
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.002
_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
Sb Sb 0.48461(3) 0.59610(2) 0.11203(2) 0.01299(5) Uani 1 1 d . . . . .
Br1 Br 0.08094(5) 0.55957(2) 0.10983(2) 0.01968(7) Uani 1 1 d . . . . .
Br2 Br 0.58887(5) 0.43330(2) 0.10982(2) 0.01498(7) Uani 1 1 d . . . . .
Br3 Br 0.38888(6) 0.73622(2) 0.11832(2) 0.02096(7) Uani 1 1 d . . . . .
Br4 Br 0.56745(5) 0.59120(2) 0.28344(2) 0.01981(7) Uani 1 1 d . . . . .
N N 0.1273(4) 0.37722(13) 0.20212(18) 0.0162(5) Uani 1 1 d . . . . .
H1 H 0.0015 0.4047 0.1906 0.019 Uiso 1 1 calc R U . . .
H2 H 0.2127 0.3853 0.1563 0.019 Uiso 1 1 calc R U . . .
C1 C 0.0632(5) 0.29781(16) 0.2013(2) 0.0179(6) Uani 1 1 d . . . . .
H1A H -0.0584 0.2907 0.2401 0.021 Uiso 1 1 calc R U . . .
H1B H 0.1923 0.2682 0.2272 0.021 Uiso 1 1 calc R U . . .
C2 C -0.0131(5) 0.27075(16) 0.1057(2) 0.0173(6) Uani 1 1 d . . . . .
H2A H -0.1283 0.3055 0.0772 0.021 Uiso 1 1 calc R U . . .
C3 C 0.1773(6) 0.26822(19) 0.0474(2) 0.0265(7) Uani 1 1 d . . . . .
H3A H 0.2483 0.3167 0.0474 0.040 Uiso 1 1 calc R U . . .
H3B H 0.1200 0.2548 -0.0147 0.040 Uiso 1 1 calc R U . . .
H3C H 0.2866 0.2316 0.0719 0.040 Uiso 1 1 calc R U . . .
C4 C -0.1207(6) 0.19519(18) 0.1127(3) 0.0266(7) Uani 1 1 d . . . . .
H4A H -0.1773 0.1779 0.0520 0.040 Uiso 1 1 calc R U . . .
H4B H -0.2440 0.1989 0.1502 0.040 Uiso 1 1 calc R U . . .
H4C H -0.0098 0.1603 0.1405 0.040 Uiso 1 1 calc R U . . .
C5 C 0.2529(5) 0.40357(16) 0.2897(2) 0.0177(6) Uani 1 1 d . . . . .
H5A H 0.3957 0.3766 0.2996 0.021 Uiso 1 1 calc R U . . .
H5B H 0.2882 0.4563 0.2833 0.021 Uiso 1 1 calc R U . . .
C6 C 0.1321(5) 0.39424(16) 0.3720(2) 0.0166(6) Uani 1 1 d . . . . .
H6A H 0.1012 0.3407 0.3796 0.020 Uiso 1 1 calc R U . . .
C7 C 0.2845(6) 0.42028(19) 0.4548(2) 0.0242(7) Uani 1 1 d . . . . .
H7A H 0.4211 0.3908 0.4610 0.036 Uiso 1 1 calc R U . . .
H7B H 0.2081 0.4146 0.5093 0.036 Uiso 1 1 calc R U . . .
H7C H 0.3221 0.4722 0.4472 0.036 Uiso 1 1 calc R U . . .
C8 C -0.0874(6) 0.4353(2) 0.3641(3) 0.0321(9) Uani 1 1 d . . . . .
H8A H -0.0610 0.4875 0.3531 0.048 Uiso 1 1 calc R U . . .
H8B H -0.1562 0.4297 0.4205 0.048 Uiso 1 1 calc R U . . .
H8C H -0.1868 0.4151 0.3135 0.048 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb Br1 2.5261(9) . ?
Sb Br4 2.5393(7) . ?
Sb Br3 2.6170(5) . ?
Sb Br2 3.0280(6) . ?
Sb Br2 3.3163(8) 3_665 ?
Sb Br1 3.6698(12) 1_655 ?
N C1 1.495(4) . ?
N C5 1.509(4) . ?
N H1 0.9100 . ?
N H2 0.9100 . ?
C1 C2 1.524(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.515(5) . ?
C2 C4 1.529(4) . ?
C2 H2A 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.500(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C8 1.515(5) . ?
C6 C7 1.528(4) . ?
C6 H6A 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Sb Br4 95.02(2) . . ?
Br1 Sb Br3 92.254(16) . . ?
Br4 Sb Br3 91.057(12) . . ?
Br1 Sb Br2 86.831(14) . . ?
Br4 Sb Br2 87.603(11) . . ?
Br3 Sb Br2 178.305(13) . . ?
Br1 Sb Br2 85.48(2) . 3_665 ?
Br4 Sb Br2 168.169(11) . 3_665 ?
Br3 Sb Br2 100.741(12) . 3_665 ?
Br2 Sb Br2 80.616(11) . 3_665 ?
Br1 Sb Br1 154.295(16) . 1_655 ?
Br4 Sb Br1 85.23(2) . 1_655 ?
Br3 Sb Br1 113.449(11) . 1_655 ?
Br2 Sb Br1 67.482(8) . 1_655 ?
Br2 Sb Br1 89.22(2) 3_665 1_655 ?
C1 N C5 114.8(2) . . ?
C1 N H1 108.6 . . ?
C5 N H1 108.6 . . ?
C1 N H2 108.6 . . ?
C5 N H2 108.6 . . ?
H1 N H2 107.6 . . ?
N C1 C2 111.8(2) . . ?
N C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
C3 C2 C1 111.7(3) . . ?
C3 C2 C4 111.5(3) . . ?
C1 C2 C4 108.3(3) . . ?
C3 C2 H2A 108.4 . . ?
C1 C2 H2A 108.4 . . ?
C4 C2 H2A 108.4 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 N 114.9(3) . . ?
C6 C5 H5A 108.5 . . ?
N C5 H5A 108.5 . . ?
C6 C5 H5B 108.5 . . ?
N C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
C5 C6 C8 112.4(3) . . ?
C5 C6 C7 108.4(3) . . ?
C8 C6 C7 110.8(3) . . ?
C5 C6 H6A 108.4 . . ?
C8 C6 H6A 108.4 . . ?
C7 C6 H6A 108.4 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N C1 C2 -166.7(3) . . . . ?
N C1 C2 C3 68.5(3) . . . . ?
N C1 C2 C4 -168.2(3) . . . . ?
C1 N C5 C6 -58.7(3) . . . . ?
N C5 C6 C8 -59.6(3) . . . . ?
N C5 C6 C7 177.6(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N H1 Br2 0.91 2.70 3.540(3) 154.5 1_455
N H2 Br2 0.91 2.60 3.398(3) 146.9 .
N H1 Br2 0.91 2.70 3.540(3) 154.5 1_455
N H2 Br2 0.91 2.60 3.398(3) 146.9 .
N H1 Br2 0.91 2.70 3.540(3) 154.5 1_455

_refine_diff_density_max         1.359
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.242

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method water
####################################################################### 
# 
# 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_SbClDIBA250K
_database_code_depnum_ccdc_archive 'CCDC 1475470'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
Bis(diisobutylammonium) octachlorodiantimonate(III)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H20 N, Cl4 Sb'
_chemical_formula_sum            'C8 H20 Cl4 N Sb'
_chemical_formula_weight         393.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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                   5.790(2)
_cell_length_b                   19.485(3)
_cell_length_c                   14.275(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.28(3)
_cell_angle_gamma                90
_cell_volume                     1579.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    18539
_cell_measurement_theta_min      0.64895
_cell_measurement_theta_max      1.00000

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    2.395
_shelx_estimated_absorpt_T_min   0.633
_shelx_estimated_absorpt_T_max   0.813
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3359
_diffrn_reflns_number            6588
_diffrn_reflns_av_unetI/netI     0.0895
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.458
_diffrn_reflns_theta_max         26.438
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3221
_reflns_number_gt                1781
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0238P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3221
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0645
_refine_ls_wR_factor_gt          0.0589
_refine_ls_goodness_of_fit_ref   0.822
_refine_ls_restrained_S_all      0.822
_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
N1 N 0.0545(6) 0.37286(19) 0.1819(3) 0.0401(10) Uani 1 1 d . . . . .
H11 H -0.0487 0.3905 0.1313 0.048 Uiso 1 1 calc R U . . .
H12 H 0.1986 0.3713 0.1656 0.048 Uiso 1 1 calc R U . . .
C1 C -0.0187(8) 0.3018(3) 0.1989(4) 0.0564(15) Uani 1 1 d . . . . .
H1A H -0.1620 0.3036 0.2270 0.068 Uiso 1 1 calc R U . . .
H1B H 0.1072 0.2796 0.2461 0.068 Uiso 1 1 calc R U . . .
C2 C -0.0679(9) 0.2589(3) 0.1113(4) 0.0672(17) Uani 1 1 d . . . . .
H2A H -0.1947 0.2822 0.0645 0.081 Uiso 1 1 calc R U . . .
C3 C 0.1389(12) 0.2498(4) 0.0646(5) 0.141(3) Uani 1 1 d . . . . .
H3A H 0.0938 0.2211 0.0075 0.212 Uiso 1 1 calc R U . . .
H3B H 0.1918 0.2947 0.0462 0.212 Uiso 1 1 calc R U . . .
H3C H 0.2670 0.2275 0.1093 0.212 Uiso 1 1 calc R U . . .
C4 C -0.1617(10) 0.1890(3) 0.1346(5) 0.100(2) Uani 1 1 d . . . . .
H4A H -0.1940 0.1608 0.0766 0.150 Uiso 1 1 calc R U . . .
H4B H -0.0440 0.1660 0.1831 0.150 Uiso 1 1 calc R U . . .
H4C H -0.3073 0.1952 0.1589 0.150 Uiso 1 1 calc R U . . .
C5 C 0.0675(8) 0.4216(3) 0.2666(3) 0.0552(14) Uani 1 1 d . . . . .
H5A H 0.1344 0.4659 0.2507 0.066 Uiso 1 1 calc R U . . .
H5B H -0.0943 0.4306 0.2766 0.066 Uiso 1 1 calc R U . . .
C6 C 0.2110(8) 0.3954(3) 0.3569(3) 0.0588(15) Uani 1 1 d . . . . .
H6A H 0.1388 0.3514 0.3728 0.071 Uiso 1 1 calc R U . . .
C7 C 0.1891(10) 0.4480(4) 0.4357(4) 0.101(2) Uani 1 1 d . . . . .
H7A H 0.2821 0.4325 0.4969 0.151 Uiso 1 1 calc R U . . .
H7B H 0.2477 0.4927 0.4193 0.151 Uiso 1 1 calc R U . . .
H7C H 0.0235 0.4523 0.4410 0.151 Uiso 1 1 calc R U . . .
C8 C 0.4647(9) 0.3816(3) 0.3552(4) 0.0769(18) Uani 1 1 d . . . . .
H8A H 0.5442 0.3645 0.4178 0.115 Uiso 1 1 calc R U . . .
H8B H 0.4754 0.3471 0.3063 0.115 Uiso 1 1 calc R U . . .
H8C H 0.5404 0.4242 0.3404 0.115 Uiso 1 1 calc R U . . .
Sb Sb 0.54367(5) 0.57645(2) 0.11463(2) 0.03420(11) Uani 1 1 d . . . . .
Cl1 Cl 0.12715(18) 0.56930(7) 0.08500(10) 0.0592(4) Uani 1 1 d . . . . .
Cl2 Cl 0.51996(17) 0.42065(7) 0.10002(7) 0.0435(3) Uani 1 1 d . . . . .
Cl3 Cl 0.5342(2) 0.69913(7) 0.12241(10) 0.0687(4) Uani 1 1 d . . . . .
Cl4 Cl 0.5845(2) 0.56564(7) 0.28438(8) 0.0638(4) 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
N1 C1 1.482(6) . ?
N1 C5 1.527(6) . ?
N1 H11 0.9100 . ?
N1 H12 0.9100 . ?
C1 C2 1.484(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.491(7) . ?
C2 C4 1.528(7) . ?
C2 H2A 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.481(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C8 1.498(6) . ?
C6 C7 1.547(7) . ?
C6 H6A 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Sb Cl1 2.3697(13) . ?
Sb Cl3 2.3941(13) . ?
Sb Cl4 2.3975(13) . ?
Sb Cl2 3.0143(13) 3_665 ?
Sb Cl2 3.0442(14) . ?
Sb Cl1 3.4886(16) 1_655 ?

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
C1 N1 C5 115.0(4) . . ?
C1 N1 H11 108.5 . . ?
C5 N1 H11 108.5 . . ?
C1 N1 H12 108.5 . . ?
C5 N1 H12 108.5 . . ?
H11 N1 H12 107.5 . . ?
N1 C1 C2 113.7(4) . . ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C1 C2 C3 114.0(5) . . ?
C1 C2 C4 109.7(5) . . ?
C3 C2 C4 110.0(6) . . ?
C1 C2 H2A 107.7 . . ?
C3 C2 H2A 107.7 . . ?
C4 C2 H2A 107.7 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 N1 114.0(4) . . ?
C6 C5 H5A 108.8 . . ?
N1 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
N1 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 C8 115.7(4) . . ?
C5 C6 C7 107.0(5) . . ?
C8 C6 C7 110.5(4) . . ?
C5 C6 H6A 107.8 . . ?
C8 C6 H6A 107.8 . . ?
C7 C6 H6A 107.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Cl1 Sb Cl3 92.02(5) . . ?
Cl1 Sb Cl4 94.07(6) . . ?
Cl3 Sb Cl4 92.26(5) . . ?
Cl1 Sb Cl2 84.37(5) . 3_665 ?
Cl3 Sb Cl2 91.67(4) . 3_665 ?
Cl4 Sb Cl2 175.82(4) . 3_665 ?
Cl1 Sb Cl2 84.17(4) . . ?
Cl3 Sb Cl2 176.15(4) . . ?
Cl4 Sb Cl2 88.62(4) . . ?
Cl2 Sb Cl2 87.37(3) 3_665 . ?
Cl1 Sb Cl1 162.15(6) . 1_655 ?
Cl3 Sb Cl1 94.42(4) . 1_655 ?
Cl4 Sb Cl1 102.27(5) . 1_655 ?
Cl2 Sb Cl1 78.83(4) 3_665 1_655 ?
Cl2 Sb Cl1 89.06(3) . 1_655 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 170.4(4) . . . . ?
N1 C1 C2 C3 61.1(7) . . . . ?
N1 C1 C2 C4 -175.2(4) . . . . ?
C1 N1 C5 C6 52.3(5) . . . . ?
N1 C5 C6 C8 60.7(6) . . . . ?
N1 C5 C6 C7 -175.7(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H11 Cl2 0.91 2.52 3.224(4) 134.7 1_455
N1 H12 Cl2 0.91 2.44 3.276(4) 153.2 .

_refine_diff_density_max         0.415
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.119

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method water
####################################################################### 
# 
# 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_SbClDIBA100K
_database_code_depnum_ccdc_archive 'CCDC 1475471'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
Bis(diisobutylammonium) octachlorodiantimonate(III)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H20 N, Cl4 Sb'
_chemical_formula_sum            'C8 H20 Cl4 N Sb'
_chemical_formula_weight         393.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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                   5.750(2)
_cell_length_b                   19.314(3)
_cell_length_c                   14.248(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.99(2)
_cell_angle_gamma                90
_cell_volume                     1547.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18539
_cell_measurement_theta_min      0.64895
_cell_measurement_theta_max      1.00000

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    2.444
_shelx_estimated_absorpt_T_min   0.628
_shelx_estimated_absorpt_T_max   0.810
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 8.3359
_diffrn_reflns_number            25845
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.108
_diffrn_reflns_theta_max         36.715
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7121
_reflns_number_gt                6024
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0461P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7121
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0803
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.146
_refine_ls_shift/su_max          0.004
_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
N1 N 0.0495(2) 0.37242(7) 0.17974(10) 0.0194(2) Uani 1 1 d . . . . .
H11 H -0.0580 0.3897 0.1291 0.023 Uiso 1 1 calc R U . . .
H12 H 0.1928 0.3706 0.1623 0.023 Uiso 1 1 calc R U . . .
C1 C -0.0236(3) 0.29995(9) 0.19954(12) 0.0227(3) Uani 1 1 d . . . . .
H1A H -0.1627 0.3022 0.2304 0.027 Uiso 1 1 calc R U . . .
H1B H 0.1081 0.2775 0.2452 0.027 Uiso 1 1 calc R U . . .
C2 C -0.0862(4) 0.25626(10) 0.11020(14) 0.0322(4) Uani 1 1 d . . . . .
H2A H -0.2176 0.2795 0.0639 0.039 Uiso 1 1 calc R U . . .
C3 C 0.1235(7) 0.24682(16) 0.0627(3) 0.0744(12) Uani 1 1 d . . . . .
H3A H 0.0760 0.2182 0.0051 0.112 Uiso 1 1 calc R U . . .
H3B H 0.1774 0.2922 0.0448 0.112 Uiso 1 1 calc R U . . .
H3C H 0.2532 0.2240 0.1075 0.112 Uiso 1 1 calc R U . . .
C4 C -0.1739(5) 0.18632(12) 0.13753(19) 0.0441(5) Uani 1 1 d . . . . .
H4A H -0.2156 0.1572 0.0802 0.066 Uiso 1 1 calc R U . . .
H4B H -0.0483 0.1638 0.1846 0.066 Uiso 1 1 calc R U . . .
H4C H -0.3145 0.1929 0.1654 0.066 Uiso 1 1 calc R U . . .
C5 C 0.0682(3) 0.42155(9) 0.26328(13) 0.0223(3) Uani 1 1 d . . . . .
H5A H -0.0941 0.4323 0.2723 0.027 Uiso 1 1 calc R U . . .
H5B H 0.1401 0.4654 0.2471 0.027 Uiso 1 1 calc R U . . .
C6 C 0.2140(3) 0.39445(10) 0.35750(12) 0.0260(3) Uani 1 1 d . . . . .
H6A H 0.1408 0.3503 0.3738 0.031 Uiso 1 1 calc R U . . .
C7 C 0.1976(5) 0.44807(15) 0.43527(15) 0.0425(5) Uani 1 1 d . . . . .
H7A H 0.2901 0.4321 0.4971 0.064 Uiso 1 1 calc R U . . .
H7B H 0.2612 0.4924 0.4186 0.064 Uiso 1 1 calc R U . . .
H7C H 0.0309 0.4540 0.4398 0.064 Uiso 1 1 calc R U . . .
C8 C 0.4725(3) 0.38012(11) 0.35230(14) 0.0288(4) Uani 1 1 d . . . . .
H8A H 0.5589 0.3628 0.4145 0.043 Uiso 1 1 calc R U . . .
H8B H 0.4775 0.3453 0.3027 0.043 Uiso 1 1 calc R U . . .
H8C H 0.5469 0.4230 0.3364 0.043 Uiso 1 1 calc R U . . .
Sb Sb 0.55258(2) 0.57559(2) 0.11500(2) 0.01589(4) Uani 1 1 d . . . . .
Cl1 Cl 0.13017(7) 0.57096(2) 0.08170(4) 0.02767(9) Uani 1 1 d . . . . .
Cl2 Cl 0.51161(7) 0.41853(2) 0.09812(3) 0.02025(7) Uani 1 1 d . . . . .
Cl3 Cl 0.54923(9) 0.69956(2) 0.12430(3) 0.03104(10) Uani 1 1 d . . . . .
Cl4 Cl 0.58826(9) 0.56385(2) 0.28558(3) 0.02902(9) 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
N1 C1 1.505(2) . ?
N1 C5 1.508(2) . ?
N1 H11 0.9100 . ?
N1 H12 0.9100 . ?
C1 C2 1.507(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.511(4) . ?
C2 C4 1.521(3) . ?
C2 H2A 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.520(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C8 1.529(3) . ?
C6 C7 1.534(3) . ?
C6 H6A 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Sb Cl1 2.3777(9) . ?
Sb Cl3 2.3983(6) . ?
Sb Cl4 2.4069(7) . ?
Sb Cl2 2.9839(8) 3_665 ?
Sb Cl2 3.0482(6) . ?
Sb Cl1 3.4523(12) 1_655 ?

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
C1 N1 C5 114.46(13) . . ?
C1 N1 H11 108.6 . . ?
C5 N1 H11 108.6 . . ?
C1 N1 H12 108.6 . . ?
C5 N1 H12 108.6 . . ?
H11 N1 H12 107.6 . . ?
N1 C1 C2 112.92(14) . . ?
N1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C1 C2 C3 111.9(2) . . ?
C1 C2 C4 108.36(17) . . ?
C3 C2 C4 110.2(2) . . ?
C1 C2 H2A 108.8 . . ?
C3 C2 H2A 108.8 . . ?
C4 C2 H2A 108.8 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 C6 114.58(14) . . ?
N1 C5 H5A 108.6 . . ?
C6 C5 H5A 108.6 . . ?
N1 C5 H5B 108.6 . . ?
C6 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 C8 112.52(14) . . ?
C5 C6 C7 107.46(17) . . ?
C8 C6 C7 111.32(17) . . ?
C5 C6 H6A 108.5 . . ?
C8 C6 H6A 108.5 . . ?
C7 C6 H6A 108.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Cl1 Sb Cl3 91.661(16) . . ?
Cl1 Sb Cl4 93.85(3) . . ?
Cl3 Sb Cl4 92.188(16) . . ?
Cl1 Sb Cl2 83.86(3) . 3_665 ?
Cl3 Sb Cl2 91.005(13) . 3_665 ?
Cl4 Sb Cl2 176.129(14) . 3_665 ?
Cl1 Sb Cl2 83.559(14) . . ?
Cl3 Sb Cl2 175.202(15) . . ?
Cl4 Sb Cl2 88.563(15) . . ?
Cl2 Sb Cl2 88.074(11) 3_665 . ?
Cl1 Sb Cl1 160.66(2) . 1_655 ?
Cl3 Sb Cl1 93.007(15) . 1_655 ?
Cl4 Sb Cl1 104.70(3) . 1_655 ?
Cl2 Sb Cl1 77.31(2) 3_665 1_655 ?
Cl2 Sb Cl1 91.385(11) . 1_655 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 168.90(15) . . . . ?
N1 C1 C2 C3 62.4(2) . . . . ?
N1 C1 C2 C4 -175.96(16) . . . . ?
C1 N1 C5 C6 49.84(19) . . . . ?
N1 C5 C6 C8 61.5(2) . . . . ?
N1 C5 C6 C7 -175.61(16) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H11 Cl2 0.91 2.48 3.1962(18) 135.3 1_455
N1 H12 Cl2 0.91 2.40 3.2390(17) 153.8 .

_refine_diff_density_max         1.190
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.129

_shelxl_version_number           2014-3


#==== end of cif
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method water
