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#$Date: 2016-03-26 17:00:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180367 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/36/7203693.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_7203693
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            'C9.33 H18.33 Cl N3 S6 Sb'
_chemical_formula_weight         522.16
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   26.6252(6)
_cell_length_b                   26.6252
_cell_length_c                   14.6744(7)
_cell_measurement_reflns_used    5366
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.3
_cell_volume                     9009.0(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.039
_diffrn_reflns_av_sigmaI/netI    0.030
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25470
_diffrn_reflns_theta_full        30.0
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.131
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2000 & Blessing, 1995)'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4668
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.34
_refine_diff_density_min         -1.16
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         5864
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.054
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.066P)²+14.783P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.111
_refine_ls_wR_factor_ref         0.118
_reflns_number_gt                4731
_reflns_number_total             5864
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b416493h.txt
_cod_data_source_block           Sb{S2CNMe)2}3
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7203693
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.534459(9) 0.451606(9) 0.116294(16) 0.03913(9) Uani 1 1 d . . .
S1 S 0.61236(4) 0.44154(4) 0.19872(6) 0.0452(2) Uani 1 1 d . . .
S2 S 0.65385(4) 0.53155(4) 0.05499(7) 0.0537(2) Uani 1 1 d . . .
S3 S 0.53320(4) 0.37643(4) 0.00946(6) 0.04344(19) Uani 1 1 d . . .
S4 S 0.44165(5) 0.40708(5) -0.02595(7) 0.0550(2) Uani 1 1 d . . .
S5 S 0.46666(4) 0.36362(3) 0.21153(6) 0.04084(19) Uani 1 1 d . . .
S6 S 0.49832(5) 0.47655(4) 0.29782(8) 0.0585(3) Uani 1 1 d . . .
N1 N 0.72292(12) 0.51126(14) 0.1608(2) 0.0463(7) Uani 1 1 d . . .
N2 N 0.45011(13) 0.32447(15) -0.1125(2) 0.0480(7) Uani 1 1 d . . .
N3 N 0.41995(13) 0.37353(13) 0.3640(2) 0.0450(6) Uani 1 1 d . . .
C1 C 0.66922(14) 0.49746(15) 0.1384(2) 0.0383(6) Uani 1 1 d . . .
C2 C 0.7361(2) 0.4829(2) 0.2345(3) 0.0695(13) Uani 1 1 d . . .
H2A H 0.7099 0.4758 0.2851 0.104 Uiso 1 1 calc R . .
H2B H 0.7758 0.5077 0.2545 0.104 Uiso 1 1 calc R . .
H2C H 0.7313 0.4463 0.2130 0.104 Uiso 1 1 calc R . .
C3 C 0.77381(17) 0.5568(2) 0.1154(3) 0.0640(11) Uani 1 1 d . . .
H3A H 0.7620 0.5692 0.0613 0.096 Uiso 1 1 calc R . .
H3B H 0.7994 0.5423 0.0982 0.096 Uiso 1 1 calc R . .
H3C H 0.7941 0.5895 0.1565 0.096 Uiso 1 1 calc R . .
C4 C 0.47128(14) 0.36539(15) -0.0505(2) 0.0395(7) Uani 1 1 d . . .
C5 C 0.4759(2) 0.2891(2) -0.1370(3) 0.0670(12) Uani 1 1 d . . .
H5A H 0.4862 0.2945 -0.2011 0.101 Uiso 1 1 calc R . .
H5B H 0.4481 0.2486 -0.1256 0.101 Uiso 1 1 calc R . .
H5C H 0.5104 0.3008 -0.1007 0.101 Uiso 1 1 calc R . .
C6 C 0.39842(18) 0.3122(2) -0.1649(3) 0.0618(11) Uani 1 1 d . . .
H6A H 0.3716 0.3170 -0.1261 0.093 Uiso 1 1 calc R . .
H6B H 0.3798 0.2727 -0.1874 0.093 Uiso 1 1 calc R . .
H6C H 0.4095 0.3389 -0.2159 0.093 Uiso 1 1 calc R . .
C7 C 0.45806(14) 0.40295(14) 0.2995(2) 0.0399(7) Uani 1 1 d . . .
C8 C 0.38455(19) 0.31033(17) 0.3631(3) 0.0573(10) Uani 1 1 d . . .
H8A H 0.3482 0.2989 0.3323 0.086 Uiso 1 1 calc R . .
H8B H 0.3769 0.2960 0.4252 0.086 Uiso 1 1 calc R . .
H8C H 0.4051 0.2942 0.3312 0.086 Uiso 1 1 calc R . .
C9 C 0.4063(2) 0.4026(2) 0.4365(3) 0.0661(12) Uani 1 1 d . . .
H9A H 0.4342 0.4438 0.4353 0.099 Uiso 1 1 calc R . .
H9B H 0.4080 0.3867 0.4950 0.099 Uiso 1 1 calc R . .
H9C H 0.3676 0.3967 0.4270 0.099 Uiso 1 1 calc R . .
C10 C 0.3333 0.6667 0.3212(6) 0.336(18) Uiso 1 3 d SD . .
Cl1 Cl 0.34761(15) 0.73829(7) 0.3236(3) 0.0609(8) Uiso 0.33 1 d PD . .
Cl2 Cl 0.3434(2) 0.73267(16) 0.2800(4) 0.0904(13) Uiso 0.33 1 d PD . .
Cl3 Cl 0.3237(5) 0.6895(4) 0.4283(5) 0.177(3) Uiso 0.33 1 d PD . .
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 84.24(3) . . ?
S1 Sb S5 83.20(3) . . ?
S3 Sb S5 83.64(3) . . ?
C1 S1 Sb 94.30(11) . . ?
C4 S3 Sb 94.76(12) . . ?
C7 S5 Sb 95.68(12) . . ?
C1 N1 C3 123.0(3) . . ?
C1 N1 C2 123.0(3) . . ?
C3 N1 C2 114.1(3) . . ?
C4 N2 C6 121.0(3) . . ?
C4 N2 C5 124.2(3) . . ?
C6 N2 C5 114.8(3) . . ?
C7 N3 C8 122.6(3) . . ?
C7 N3 C9 121.8(3) . . ?
C8 N3 C9 115.3(3) . . ?
N1 C1 S2 123.1(3) . . ?
N1 C1 S1 117.8(2) . . ?
S2 C1 S1 119.07(19) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 S4 123.1(3) . . ?
N2 C4 S3 117.6(3) . . ?
S4 C4 S3 119.3(2) . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 S6 123.3(3) . . ?
N3 C7 S5 117.8(2) . . ?
S6 C7 S5 119.0(2) . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Cl2 C10 Cl2 108.7(3) . 2_665 ?
Cl2 C10 Cl2 108.7(3) . 3_565 ?
Cl2 C10 Cl2 108.7(3) 2_665 3_565 ?
Cl2 C10 Cl1 21.58(17) . . ?
Cl2 C10 Cl1 120.9(3) 2_665 . ?
Cl2 C10 Cl1 115.9(3) 3_565 . ?
Cl2 C10 Cl1 115.9(3) . 2_665 ?
Cl2 C10 Cl1 21.58(17) 2_665 2_665 ?
Cl2 C10 Cl1 120.9(3) 3_565 2_665 ?
Cl1 C10 Cl1 119.96(2) . 2_665 ?
Cl2 C10 Cl1 120.9(3) . 3_565 ?
Cl2 C10 Cl1 115.9(3) 2_665 3_565 ?
Cl2 C10 Cl1 21.58(17) 3_565 3_565 ?
Cl1 C10 Cl1 119.96(2) . 3_565 ?
Cl1 C10 Cl1 119.96(2) 2_665 3_565 ?
Cl2 C10 Cl3 86.3(4) . . ?
Cl2 C10 Cl3 110.4(5) 2_665 . ?
Cl2 C10 Cl3 130.4(5) 3_565 . ?
Cl1 C10 Cl3 65.9(4) . . ?
Cl1 C10 Cl3 90.0(5) 2_665 . ?
Cl1 C10 Cl3 110.7(5) 3_565 . ?
Cl2 C10 Cl3 130.4(5) . 2_665 ?
Cl2 C10 Cl3 86.3(4) 2_665 2_665 ?
Cl2 C10 Cl3 110.4(5) 3_565 2_665 ?
Cl1 C10 Cl3 110.7(5) . 2_665 ?
Cl1 C10 Cl3 65.9(4) 2_665 2_665 ?
Cl1 C10 Cl3 90.0(5) 3_565 2_665 ?
Cl3 C10 Cl3 44.8(5) . 2_665 ?
Cl2 C10 Cl3 110.4(5) . 3_565 ?
Cl2 C10 Cl3 130.4(5) 2_665 3_565 ?
Cl2 C10 Cl3 86.3(4) 3_565 3_565 ?
Cl1 C10 Cl3 90.0(5) . 3_565 ?
Cl1 C10 Cl3 110.7(5) 2_665 3_565 ?
Cl1 C10 Cl3 65.9(4) 3_565 3_565 ?
Cl3 C10 Cl3 44.8(5) . 3_565 ?
Cl3 C10 Cl3 44.8(5) 2_665 3_565 ?
C10 Cl1 Cl3 57.07(19) . . ?
C10 Cl2 Cl2 35.66(16) . 2_665 ?
C10 Cl2 Cl2 35.66(16) . 3_565 ?
Cl2 Cl2 Cl2 60.000(1) 2_665 3_565 ?
Cl3 Cl3 Cl3 60.000(5) 3_565 2_665 ?
Cl3 Cl3 C10 67.6(2) 3_565 . ?
Cl3 Cl3 C10 67.6(2) 2_665 . ?
Cl3 Cl3 Cl1 98.2(7) 3_565 . ?
Cl3 Cl3 Cl1 124.6(2) 2_665 . ?
C10 Cl3 Cl1 57.03(19) . . ?
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 2.5282(9) . ?
Sb S3 2.5294(9) . ?
Sb S5 2.5438(9) . ?
S1 C1 1.743(3) . ?
S2 C1 1.692(3) . ?
S3 C4 1.759(3) . ?
S4 C4 1.691(3) . ?
S5 C7 1.747(3) . ?
S6 C7 1.700(3) . ?
N1 C1 1.327(4) . ?
N1 C3 1.452(5) . ?
N1 C2 1.458(5) . ?
N2 C4 1.310(5) . ?
N2 C6 1.464(5) . ?
N2 C5 1.460(5) . ?
N3 C7 1.321(4) . ?
N3 C8 1.461(5) . ?
N3 C9 1.464(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C10 Cl2 1.7480(10) . ?
C10 Cl2 1.7480(10) 2_665 ?
C10 Cl2 1.7481(10) 3_565 ?
C10 Cl1 1.7485(10) . ?
C10 Cl1 1.7485(10) 2_665 ?
C10 Cl1 1.7485(10) 3_565 ?
C10 Cl3 1.7493(10) . ?
C10 Cl3 1.7493(10) 2_665 ?
C10 Cl3 1.7493(10) 3_565 ?
Cl1 Cl3 1.903(10) . ?
Cl2 Cl2 2.841(6) 2_665 ?
Cl2 Cl2 2.841(6) 3_565 ?
Cl3 Cl3 1.333(14) 3_565 ?
Cl3 Cl3 1.333(14) 2_665 ?
