#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/36/7203694.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_7203694
loop_
_publ_author_name
'Liu, Yu'
'Tiekink, Edward R. T.'
_publ_section_title
;
 Supramolecular associations in binary antimony(iii) dithiocarbamates:
 influence of ligand steric bulk, influence on coordination geometry,
 and competition with hydrogen-bonding
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              20
_journal_paper_doi               10.1039/b416493h
_journal_volume                  7
_journal_year                    2005
_chemical_formula_sum            'C19 H31 Cl3 N3 S6 Sb'
_chemical_formula_weight         721.93
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.617(1)
_cell_angle_beta                 110.929(1)
_cell_angle_gamma                106.614(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3916(6)
_cell_length_b                   11.4660(7)
_cell_length_c                   13.7520(9)
_cell_measurement_reflns_used    3878
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      2.4
_cell_volume                     1429.47(15)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'Bruker SHEXLTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'PATTY in DIRDIF92 (Beurskens et al., 1992)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker AXS SMART CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_sigmaI/netI    0.051
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12120
_diffrn_reflns_theta_full        30.1
_diffrn_reflns_theta_max         30.1
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.699
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2000 & Blessing, 1995)'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.48
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         8164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.050
_refine_ls_R_factor_gt           0.039
_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)+(0.039P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.085
_refine_ls_wR_factor_ref         0.090
_reflns_number_gt                6825
_reflns_number_total             8164
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b416493h.txt
_cod_data_source_block           Sb{S2CN(CH2)5}3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203694
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb Sb 0.144681(19) 0.098904(17) 0.211741(13) 0.02501(6) Uani 1 1 d . . .
Cl1 Cl 0.30233(11) 0.38448(10) 0.93368(9) 0.0612(3) Uani 1 1 d . . .
Cl2 Cl 0.02333(12) 0.41662(10) 0.83403(8) 0.0621(3) Uani 1 1 d . . .
Cl3 Cl 0.11564(10) 0.36803(11) 1.04542(7) 0.0581(3) Uani 1 1 d . . .
S1 S 0.24965(9) -0.06634(7) 0.17775(6) 0.03592(17) Uani 1 1 d . . .
S2 S 0.18965(8) 0.07315(7) 0.00796(5) 0.03141(15) Uani 1 1 d . . .
S3 S 0.25826(8) 0.07121(7) 0.40091(5) 0.03209(16) Uani 1 1 d . . .
S4 S -0.05655(8) -0.07668(7) 0.28191(5) 0.03292(16) Uani 1 1 d . . .
S5 S 0.39240(7) 0.27176(7) 0.27393(6) 0.03092(15) Uani 1 1 d . . .
S6 S 0.16123(8) 0.34519(7) 0.31525(6) 0.03416(16) Uani 1 1 d . . .
N1 N 0.2451(3) -0.1393(2) -0.01286(18) 0.0309(5) Uani 1 1 d . . .
N2 N 0.1063(3) -0.0929(2) 0.47652(18) 0.0301(5) Uani 1 1 d . . .
N3 N 0.4332(3) 0.4997(2) 0.36582(19) 0.0316(5) Uani 1 1 d . . .
C1 C 0.2273(3) -0.0528(3) 0.0476(2) 0.0257(5) Uani 1 1 d . . .
C2 C 0.2353(3) -0.1345(3) -0.1213(2) 0.0385(7) Uani 1 1 d . . .
H2A H 0.2247 -0.0554 -0.1370 0.046 Uiso 1 1 calc R . .
H2B H 0.1482 -0.2027 -0.1728 0.046 Uiso 1 1 calc R . .
C3 C 0.3705(3) -0.1459(3) -0.1328(2) 0.0371(7) Uani 1 1 d . . .
H3A H 0.3580 -0.1492 -0.2073 0.044 Uiso 1 1 calc R . .
H3B H 0.4555 -0.0719 -0.0882 0.044 Uiso 1 1 calc R . .
C4 C 0.3995(4) -0.2616(3) -0.1006(2) 0.0417(8) Uani 1 1 d . . .
H4A H 0.4917 -0.2631 -0.1041 0.050 Uiso 1 1 calc R . .
H4B H 0.3200 -0.3365 -0.1500 0.050 Uiso 1 1 calc R . .
C5 C 0.4094(4) -0.2611(3) 0.0123(3) 0.0397(7) Uani 1 1 d . . .
H5A H 0.4226 -0.3381 0.0318 0.048 Uiso 1 1 calc R . .
H5B H 0.4947 -0.1904 0.0623 0.048 Uiso 1 1 calc R . .
C6 C 0.2717(4) -0.2510(3) 0.0206(3) 0.0390(7) Uani 1 1 d . . .
H6A H 0.1877 -0.3255 -0.0247 0.047 Uiso 1 1 calc R . .
H6B H 0.2816 -0.2470 0.0945 0.047 Uiso 1 1 calc R . .
C7 C 0.1000(3) -0.0411(3) 0.3941(2) 0.0269(5) Uani 1 1 d . . .
C8 C 0.2437(3) -0.0776(3) 0.5665(2) 0.0352(6) Uani 1 1 d . . .
H8A H 0.2339 -0.0585 0.6340 0.042 Uiso 1 1 calc R . .
H8B H 0.3238 -0.0081 0.5655 0.042 Uiso 1 1 calc R . .
C9 C 0.2778(4) -0.1954(4) 0.5582(3) 0.0473(8) Uani 1 1 d . . .
H9A H 0.3668 -0.1866 0.6203 0.057 Uiso 1 1 calc R . .
H9B H 0.2970 -0.2095 0.4940 0.057 Uiso 1 1 calc R . .
C10 C 0.1518(4) -0.3077(4) 0.5527(3) 0.0566(10) Uani 1 1 d . . .
H10A H 0.1439 -0.3009 0.6218 0.068 Uiso 1 1 calc R . .
H10B H 0.1722 -0.3844 0.5381 0.068 Uiso 1 1 calc R . .
C11 C 0.0084(4) -0.3153(3) 0.4666(3) 0.0476(8) Uani 1 1 d . . .
H11A H 0.0098 -0.3378 0.3964 0.057 Uiso 1 1 calc R . .
H11B H -0.0723 -0.3809 0.4712 0.057 Uiso 1 1 calc R . .
C12 C -0.0178(3) -0.1931(3) 0.4769(3) 0.0384(7) Uani 1 1 d . . .
H12A H -0.1081 -0.1990 0.4174 0.046 Uiso 1 1 calc R . .
H12B H -0.0297 -0.1745 0.5437 0.046 Uiso 1 1 calc R . .
C13 C 0.3360(3) 0.3843(3) 0.32302(19) 0.0252(5) Uani 1 1 d . . .
C14 C 0.3947(4) 0.6065(3) 0.3951(3) 0.0402(7) Uani 1 1 d . . .
H14A H 0.4651 0.6548 0.4668 0.048 Uiso 1 1 calc R . .
H14B H 0.2967 0.5777 0.3957 0.048 Uiso 1 1 calc R . .
C15 C 0.3967(4) 0.6882(3) 0.3145(3) 0.0510(9) Uani 1 1 d . . .
H15A H 0.3188 0.6424 0.2444 0.061 Uiso 1 1 calc R . .
H15B H 0.3776 0.7632 0.3365 0.061 Uiso 1 1 calc R . .
C16 C 0.5442(4) 0.7262(4) 0.3058(3) 0.0568(10) Uani 1 1 d . . .
H16A H 0.6200 0.7825 0.3729 0.068 Uiso 1 1 calc R . .
H16B H 0.5397 0.7714 0.2485 0.068 Uiso 1 1 calc R . .
C17 C 0.5850(4) 0.6130(4) 0.2829(3) 0.0526(10) Uani 1 1 d . . .
H17A H 0.5160 0.5615 0.2119 0.063 Uiso 1 1 calc R . .
H17B H 0.6838 0.6398 0.2836 0.063 Uiso 1 1 calc R . .
C18 C 0.5806(3) 0.5377(3) 0.3662(3) 0.0406(7) Uani 1 1 d . . .
H18A H 0.6052 0.4636 0.3509 0.049 Uiso 1 1 calc R . .
H18B H 0.6528 0.5878 0.4369 0.049 Uiso 1 1 calc R . .
C19 C 0.1211(3) 0.3393(3) 0.9202(2) 0.0376(7) Uani 1 1 d . . .
H19 H 0.0743 0.2484 0.8891 0.045 Uiso 1 1 calc 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
S1 Sb S3 80.45(2) . . ?
S1 Sb S5 92.01(3) . . ?
S3 Sb S5 81.37(2) . . ?
C1 S1 Sb 95.83(9) . . ?
C7 S3 Sb 95.23(9) . . ?
C13 S5 Sb 94.27(9) . . ?
C1 N1 C6 123.6(2) . . ?
C1 N1 C2 123.1(3) . . ?
C6 N1 C2 113.3(2) . . ?
C7 N2 C12 123.1(2) . . ?
C7 N2 C8 123.8(2) . . ?
C12 N2 C8 111.8(2) . . ?
C13 N3 C14 123.3(2) . . ?
C13 N3 C18 123.3(3) . . ?
C14 N3 C18 112.1(2) . . ?
N1 C1 S2 124.0(2) . . ?
N1 C1 S1 118.4(2) . . ?
S2 C1 S1 117.58(16) . . ?
N1 C2 C3 110.8(2) . . ?
N1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 C2 111.9(3) . . ?
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 C5 109.4(3) . . ?
C3 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
C5 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
C6 C5 C4 110.5(3) . . ?
C6 C5 H5A 109.6 . . ?
C4 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
C4 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N1 C6 C5 110.9(2) . . ?
N1 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
N2 C7 S4 123.3(2) . . ?
N2 C7 S3 118.6(2) . . ?
S4 C7 S3 118.09(15) . . ?
N2 C8 C9 109.4(3) . . ?
N2 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
N2 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 C10 111.6(3) . . ?
C8 C9 H9A 109.3 . . ?
C10 C9 H9A 109.3 . . ?
C8 C9 H9B 109.3 . . ?
C10 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
C9 C10 C11 111.0(3) . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C10 111.4(3) . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
N2 C12 C11 109.9(3) . . ?
N2 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
N2 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
N3 C13 S6 122.4(2) . . ?
N3 C13 S5 117.9(2) . . ?
S6 C13 S5 119.78(16) . . ?
N3 C14 C15 109.1(3) . . ?
N3 C14 H14A 109.9 . . ?
C15 C14 H14A 109.9 . . ?
N3 C14 H14B 109.9 . . ?
C15 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
C16 C15 C14 110.9(3) . . ?
C16 C15 H15A 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 108.0 . . ?
C15 C16 C17 111.1(3) . . ?
C15 C16 H16A 109.4 . . ?
C17 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
C17 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C18 C17 C16 109.6(3) . . ?
C18 C17 H17A 109.7 . . ?
C16 C17 H17A 109.7 . . ?
C18 C17 H17B 109.7 . . ?
C16 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
N3 C18 C17 109.3(3) . . ?
N3 C18 H18A 109.8 . . ?
C17 C18 H18A 109.8 . . ?
N3 C18 H18B 109.8 . . ?
C17 C18 H18B 109.8 . . ?
H18A C18 H18B 108.3 . . ?
Cl1 C19 Cl3 109.94(17) . . ?
Cl1 C19 Cl2 110.97(18) . . ?
Cl3 C19 Cl2 110.86(18) . . ?
Cl1 C19 H19 108.3 . . ?
Cl3 C19 H19 108.3 . . ?
Cl2 C19 H19 108.3 . . ?
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 S1 2.5241(8) . ?
Sb S3 2.5385(7) . ?
Sb S5 2.5424(7) . ?
Cl1 C19 1.738(3) . ?
Cl2 C19 1.756(3) . ?
Cl3 C19 1.745(3) . ?
S1 C1 1.750(3) . ?
S2 C1 1.691(3) . ?
S3 C7 1.740(3) . ?
S4 C7 1.702(3) . ?
S5 C13 1.735(3) . ?
S6 C13 1.702(3) . ?
N1 C1 1.328(3) . ?
N1 C6 1.468(4) . ?
N1 C2 1.465(3) . ?
N2 C7 1.320(3) . ?
N2 C12 1.464(4) . ?
N2 C8 1.467(4) . ?
N3 C13 1.332(3) . ?
N3 C14 1.456(4) . ?
N3 C18 1.465(4) . ?
C2 C3 1.509(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 C4 1.515(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 C5 1.518(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 C6 1.511(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C8 C9 1.495(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 C10 1.525(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 C11 1.509(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.504(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C14 C15 1.522(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 C16 1.520(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 C17 1.515(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C17 C18 1.507(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 H19 0.9900 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30653678
