#------------------------------------------------------------------------------
#$Date: 2018-07-10 12:13:45 +0300 (Tue, 10 Jul 2018) $
#$Revision: 208944 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/29/7032943.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7032943
loop_
_publ_author_name
'Vránová, Iva'
'Jambor, Roman'
'R°užička, Aleš'
'Hoffmann, Alexander'
'Herres-Pawlis, Sonja'
'Dostál, Libor'
_publ_section_title
;
 Antimony(III) and bismuth(III) amides containing pendant N-donor
 groups--a combined experimental and theoretical study.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              395
_journal_page_last               400
_journal_paper_doi               10.1039/c4dt02692f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C14 H22 Cl2 N3 Sb, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C14.5 H23 Cl3 N3 Sb'
_chemical_formula_weight         467.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 130.412(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8552(4)
_cell_length_b                   8.2449(3)
_cell_length_c                   14.0093(6)
_cell_measurement_reflns_used    6538
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1746.19(15)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6524
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.037
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.034(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3739
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0162
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0154P)²+1.3047P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0427
_reflns_number_gt                3682
_reflns_number_total             3739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02692f1.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
Adding full bibliography for 7032942--7032945.cif.

2018-06-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C29 H46 Cl6 N6 Sb2'
_cod_original_formula_weight         934.92
_cod_original_formula_moiety         '2(C14 H22 Cl2 N3 Sb), C H2 Cl2'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7032943
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sb1 Sb 0.014231(8) 0.01959(2) 0.355435(11) 0.01283(4) Uani 1 1 d .
Cl1 Cl -0.06706(5) 0.24805(8) 0.18899(7) 0.02443(16) Uani 1 1 d .
Cl2 Cl 0.10631(4) -0.21376(7) 0.50847(6) 0.02123(12) Uani 1 1 d .
N1 N 0.07916(13) -0.0227(2) 0.29106(18) 0.0163(4) Uani 1 1 d .
C2 C 0.15084(14) 0.0306(4) 0.2226(2) 0.0207(4) Uani 1 1 d .
H2 H 0.1872 0.0789 0.2107 0.025 Uiso 1 1 d R
C6 C 0.12106(17) 0.3652(3) 0.4946(2) 0.0214(5) Uani 1 1 d .
H6A H 0.0608 0.4009 0.4279 0.026 Uiso 1 1 d R
H6B H 0.1614 0.4493 0.5105 0.026 Uiso 1 1 d R
C7 C 0.13488(18) 0.3267(3) 0.6121(3) 0.0254(5) Uani 1 1 d .
H7A H 0.0789 0.3056 0.5921 0.030 Uiso 1 1 d R
H7B H 0.1639 0.4165 0.6707 0.030 Uiso 1 1 d R
C8 C 0.19409(17) 0.1744(3) 0.6679(2) 0.0240(5) Uani 1 1 d .
H8A H 0.2471 0.1935 0.7540 0.029 Uiso 1 1 d R
H8B H 0.1625 0.0827 0.6659 0.029 Uiso 1 1 d R
C1 C 0.13536(15) 0.0837(3) 0.2997(2) 0.0173(5) Uani 1 1 d .
Cl3 Cl 0.09607(5) 0.44001(9) 0.09687(6) 0.03116(15) Uani 1 1 d .
N2 N 0.13883(13) 0.2093(2) 0.46055(18) 0.0166(4) Uani 1 1 d .
C9 C 0.21715(15) 0.1443(3) 0.5848(2) 0.0201(5) Uani 1 1 d .
H9A H 0.2708 0.2010 0.6161 0.024 Uiso 1 1 d R
H9B H 0.2247 0.0293 0.5795 0.024 Uiso 1 1 d R
C12 C -0.21278(16) -0.0963(3) 0.0825(2) 0.0234(5) Uani 1 1 d .
H12A H -0.2716 -0.0957 0.0009 0.028 Uiso 1 1 d R
H12B H -0.2022 0.0068 0.1236 0.028 Uiso 1 1 d R
C10 C -0.00042(15) -0.2736(3) 0.1955(2) 0.0193(5) Uani 1 1 d .
H10A H 0.0345 -0.3503 0.2642 0.023 Uiso 1 1 d R
H10B H -0.0296 -0.3319 0.1175 0.023 Uiso 1 1 d R
C13 C -0.20145(16) -0.2383(4) 0.1628(2) 0.0252(5) Uani 1 1 d .
H13A H -0.2041 -0.2003 0.2258 0.030 Uiso 1 1 d R
H13B H -0.2475 -0.3187 0.1109 0.030 Uiso 1 1 d R
C11 C -0.14339(16) -0.1290(3) 0.0707(2) 0.0207(5) Uani 1 1 d .
H11A H -0.1643 -0.2081 0.0055 0.025 Uiso 1 1 d R
H11B H -0.1272 -0.0303 0.0523 0.025 Uiso 1 1 d R
C4 C 0.05770(15) -0.1448(3) 0.2087(2) 0.0170(4) Uani 1 1 d .
C14 C -0.11054(16) -0.3109(3) 0.2244(2) 0.0210(5) Uani 1 1 d .
H14A H -0.0760 -0.3213 0.3142 0.025 Uiso 1 1 d R
H14B H -0.1165 -0.4171 0.1899 0.025 Uiso 1 1 d R
C3 C 0.10033(16) -0.1153(3) 0.1639(2) 0.0209(5) Uani 1 1 d .
H3 H 0.0970 -0.1782 0.1058 0.025 Uiso 1 1 d R
C15 C 0.0000 0.3181(4) 0.0000 0.0247(8) Uani 1 2 d S
H15 H 0.0043 0.2489 -0.0519 0.030 Uiso 1 1 d R
N3 N -0.06749(16) -0.1944(3) 0.1964(2) 0.0164(5) Uani 1 1 d .
C5 C 0.15666(16) 0.2354(3) 0.3735(2) 0.0203(5) Uani 1 1 d .
H5A H 0.2184 0.2633 0.4211 0.024 Uiso 1 1 d R
H5B H 0.1209 0.3244 0.3171 0.024 Uiso 1 1 d R
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 1 0.097
1 0 -1 0.091
0 1 0 0.127
0 -1 0 0.144
-1 0 0 0.119
1 0 0 0.098
-1 -1 1 0.145
1 -1 -1 0.127
1 1 -1 0.136
-1 -1 0 0.133
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
N1 Sb1 N2 72.05(7) . .
N1 Sb1 N3 73.08(8) . .
N2 Sb1 N3 145.05(8) . .
N1 Sb1 Cl2 85.89(6) . .
N2 Sb1 Cl2 94.68(5) . .
N3 Sb1 Cl2 85.02(6) . .
N1 Sb1 Cl1 85.96(6) . .
N2 Sb1 Cl1 82.77(5) . .
N3 Sb1 Cl1 92.62(5) . .
Cl2 Sb1 Cl1 171.85(2) . .
C1 N1 C4 109.6(2) . .
C1 N1 Sb1 124.80(15) . .
C4 N1 Sb1 124.04(16) . .
C1 C2 C3 106.8(2) . .
C1 C2 H2 127.0 . .
C3 C2 H2 126.3 . .
N2 C6 C7 104.7(2) . .
N2 C6 H6A 110.7 . .
C7 C6 H6A 110.6 . .
N2 C6 H6B 111.0 . .
C7 C6 H6B 111.0 . .
H6A C6 H6B 108.9 . .
C6 C7 C8 105.2(2) . .
C6 C7 H7A 110.9 . .
C8 C7 H7A 110.7 . .
C6 C7 H7B 110.5 . .
C8 C7 H7B 110.7 . .
H7A C7 H7B 108.8 . .
C9 C8 C7 104.6(2) . .
C9 C8 H8A 110.8 . .
C7 C8 H8A 110.8 . .
C9 C8 H8B 111.0 . .
C7 C8 H8B 110.7 . .
H8A C8 H8B 108.9 . .
N1 C1 C2 108.3(2) . .
N1 C1 C5 116.6(2) . .
C2 C1 C5 134.6(2) . .
C5 N2 C6 111.64(19) . .
C5 N2 C9 112.68(18) . .
C6 N2 C9 102.75(19) . .
C5 N2 Sb1 106.45(13) . .
C6 N2 Sb1 112.72(14) . .
C9 N2 Sb1 110.74(14) . .
N2 C9 C8 103.4(2) . .
N2 C9 H9A 111.3 . .
C8 C9 H9A 111.2 . .
N2 C9 H9B 111.0 . .
C8 C9 H9B 110.9 . .
H9A C9 H9B 109.0 . .
C11 C12 C13 103.4(2) . .
C11 C12 H12A 111.0 . .
C13 C12 H12A 111.1 . .
C11 C12 H12B 111.0 . .
C13 C12 H12B 111.2 . .
H12A C12 H12B 109.1 . .
C4 C10 N3 108.13(19) . .
C4 C10 H10A 110.1 . .
N3 C10 H10A 110.2 . .
C4 C10 H10B 110.0 . .
N3 C10 H10B 110.0 . .
H10A C10 H10B 108.4 . .
C14 C13 C12 105.7(2) . .
C14 C13 H13A 110.7 . .
C12 C13 H13A 110.6 . .
C14 C13 H13B 110.5 . .
C12 C13 H13B 110.6 . .
H13A C13 H13B 108.7 . .
N3 C11 C12 103.4(2) . .
N3 C11 H11A 110.9 . .
C12 C11 H11A 111.0 . .
N3 C11 H11B 111.2 . .
C12 C11 H11B 111.3 . .
H11A C11 H11B 109.0 . .
C3 C4 N1 108.0(2) . .
C3 C4 C10 137.1(2) . .
N1 C4 C10 114.8(2) . .
N3 C14 C13 105.5(2) . .
N3 C14 H14A 110.6 . .
C13 C14 H14A 110.5 . .
N3 C14 H14B 110.7 . .
C13 C14 H14B 110.7 . .
H14A C14 H14B 108.8 . .
C4 C3 C2 107.3(2) . .
C4 C3 H3 126.1 . .
C2 C3 H3 126.6 . .
Cl3 C15 Cl3 110.8(2) . 2
Cl3 C15 H15 109.5 . .
Cl3 C15 H15 109.5 2 .
C10 N3 C11 112.0(2) . .
C10 N3 C14 112.7(2) . .
C11 N3 C14 103.3(2) . .
C10 N3 Sb1 104.72(15) . .
C11 N3 Sb1 112.31(17) . .
C14 N3 Sb1 112.12(17) . .
N2 C5 C1 109.54(19) . .
N2 C5 H5A 109.7 . .
C1 C5 H5A 109.8 . .
N2 C5 H5B 109.8 . .
C1 C5 H5B 109.8 . .
H5A C5 H5B 108.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 N1 2.0259(19) .
Sb1 N2 2.4521(19) .
Sb1 N3 2.454(2) .
Sb1 Cl2 2.5609(6) .
Sb1 Cl1 2.5903(7) .
N1 C1 1.362(3) .
N1 C4 1.374(3) .
C2 C1 1.372(3) .
C2 C3 1.435(4) .
C2 H2 0.9298 .
C6 N2 1.490(3) .
C6 C7 1.517(4) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C8 1.543(4) .
C7 H7A 0.9698 .
C7 H7B 0.9701 .
C8 C9 1.523(4) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C1 C5 1.498(3) .
Cl3 C15 1.770(2) .
N2 C5 1.489(3) .
N2 C9 1.492(3) .
C9 H9A 0.9700 .
C9 H9B 0.9701 .
C12 C11 1.514(3) .
C12 C13 1.536(4) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C10 C4 1.490(3) .
C10 N3 1.490(3) .
C10 H10A 0.9700 .
C10 H10B 0.9699 .
C13 C14 1.530(4) .
C13 H13A 0.9699 .
C13 H13B 0.9699 .
C11 N3 1.490(3) .
C11 H11A 0.9701 .
C11 H11B 0.9700 .
C4 C3 1.362(3) .
C14 N3 1.498(3) .
C14 H14A 0.9700 .
C14 H14B 0.9699 .
C3 H3 0.9300 .
C15 Cl3 1.771(2) 2
C15 H15 0.9701 .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
