#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:43:21 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179074 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/36/4303640.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_4303640
loop_
_publ_author_name
'Libor Dostál'
'Roman Jambor'
'Aleš R°užička'
'Robert Jirásko'
'Václav Lochař'
'Ludvík Beneš'
'Frank de Proft'
_publ_section_title
;
Nonconventional Behavior of NCN-Chelated Organoantimony(III) Sulfide and
Isolation of Cyclic Organoantimony(III) Bis(pentasulfide)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10495
_journal_page_last               10497
_journal_paper_doi               10.1021/ic901873k
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '(C24 H38 N4 S2 Sb2)(C1 H2 Cl2)'
_chemical_formula_sum            'C25 H40 Cl2 N4 S2 Sb2'
_chemical_formula_weight         775.13
_chemical_name_systematic
; 
 ? 
;
_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                78.049(5)
_cell_angle_beta                 84.599(5)
_cell_angle_gamma                77.526(4)
_cell_formula_units_Z            1
_cell_length_a                   8.9911(6)
_cell_length_b                   9.7319(6)
_cell_length_c                   10.3552(5)
_cell_measurement_reflns_used    16442
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     864.36(9)
_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, 1997)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0869
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16376
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.857
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             386
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.861
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0384
_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)+(0.0353P)²+1.0962P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0909
_reflns_number_gt                3442
_reflns_number_total             3949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901873k_si_001_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        864.35(9)
_cod_database_code               4303640
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
Sb1 Sb 0.07338(3) 0.30534(3) 0.54091(2) 0.02436(9) Uani 1 1 d . . .
S1 S 0.03643(12) 0.51553(10) 0.65076(10) 0.0309(2) Uani 1 1 d . . .
Cl1 Cl 0.2510(2) 0.81162(16) 0.0768(2) 0.0819(5) Uani 1 1 d . . .
Cl2 Cl 0.2542(3) 0.55192(19) -0.01485(15) 0.0844(6) Uani 1 1 d . . .
C8 C 0.3344(6) 0.0606(5) 0.7503(5) 0.0421(11) Uani 1 1 d . . .
H8A H 0.4094 0.0294 0.8160 0.051 Uiso 1 1 d R . .
H8B H 0.3826 0.0506 0.6651 0.051 Uiso 1 1 d R . .
H8C H 0.2579 0.0031 0.7711 0.051 Uiso 1 1 d R . .
N2 N 0.1461(4) 0.1590(3) 0.3350(3) 0.0290(7) Uani 1 1 d . . .
N1 N 0.2641(4) 0.2109(4) 0.7490(3) 0.0326(7) Uani 1 1 d . . .
C6 C 0.3566(4) 0.2789(4) 0.3443(4) 0.0290(8) Uani 1 1 d . . .
C1 C 0.3093(4) 0.2974(4) 0.4735(4) 0.0252(8) Uani 1 1 d . . .
C7 C 0.3744(5) 0.3041(4) 0.7030(4) 0.0350(9) Uani 1 1 d . . .
H7A H 0.4657 0.2679 0.7525 0.042 Uiso 1 1 d R . .
H7B H 0.3309 0.4000 0.7181 0.042 Uiso 1 1 d R . .
C5 C 0.5055(5) 0.2877(4) 0.2981(5) 0.0407(11) Uani 1 1 d . . .
H5 H 0.5371 0.2760 0.2122 0.049 Uiso 1 1 d R . .
C11 C 0.0241(5) 0.1513(5) 0.2546(5) 0.0430(11) Uani 1 1 d . . .
H11A H -0.0298 0.2464 0.2204 0.052 Uiso 1 1 d R . .
H11B H -0.0452 0.0975 0.3078 0.052 Uiso 1 1 d R . .
H11C H 0.0676 0.1048 0.1826 0.052 Uiso 1 1 d R . .
C10 C 0.2518(5) 0.2422(4) 0.2576(4) 0.0325(9) Uani 1 1 d . . .
H10A H 0.1943 0.3300 0.2077 0.039 Uiso 1 1 d R . .
H10B H 0.3120 0.1880 0.1952 0.039 Uiso 1 1 d R . .
C2 C 0.4159(4) 0.3096(4) 0.5573(4) 0.0325(9) Uani 1 1 d . . .
C12 C 0.2258(5) 0.0140(4) 0.3911(5) 0.0379(10) Uani 1 1 d . . .
H12A H 0.2632 -0.0379 0.3213 0.045 Uiso 1 1 d R . .
H12B H 0.1566 -0.0349 0.4499 0.045 Uiso 1 1 d R . .
H12C H 0.3099 0.0197 0.4391 0.045 Uiso 1 1 d R . .
C3 C 0.5635(5) 0.3193(4) 0.5086(5) 0.0397(11) Uani 1 1 d . . .
H3 H 0.6335 0.3296 0.5649 0.048 Uiso 1 1 d R . .
C9 C 0.1989(6) 0.2269(6) 0.8810(5) 0.0492(12) Uani 1 1 d . . .
H9A H 0.1348 0.1584 0.9121 0.059 Uiso 1 1 d R . .
H9B H 0.1396 0.3221 0.8781 0.059 Uiso 1 1 d R . .
H9C H 0.2801 0.2102 0.9398 0.059 Uiso 1 1 d R . .
C13 C 0.2725(7) 0.6256(6) 0.1203(5) 0.0575(14) Uani 1 1 d . . .
H13A H 0.3723 0.5850 0.1552 0.069 Uiso 1 1 d R . .
H13B H 0.1962 0.6017 0.1891 0.069 Uiso 1 1 d R . .
C4 C 0.6065(5) 0.3136(5) 0.3785(6) 0.0459(12) Uani 1 1 d . . .
H4 H 0.7030 0.3272 0.3449 0.055 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'
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'
Cl Cl 0.1484 0.1585 '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
0 0 1 0.009
0 0 -1 0.037
-1 0 0 0.248
1 0 0 0.318
0 -1 0 0.126
0 1 0 0.101
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 Sb1 S1 96.20(10) . 2_566 ?
C1 Sb1 S1 98.33(10) . . ?
S1 Sb1 S1 84.40(4) 2_566 . ?
Sb1 S1 Sb1 95.60(4) 2_566 . ?
N1 C8 H8A 109.1 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.7 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 N2 C11 111.0(3) . . ?
C10 N2 C12 110.9(3) . . ?
C11 N2 C12 109.7(3) . . ?
C8 N1 C9 109.3(4) . . ?
C8 N1 C7 111.2(3) . . ?
C9 N1 C7 111.3(4) . . ?
C5 C6 C1 119.3(4) . . ?
C5 C6 C10 119.6(4) . . ?
C1 C6 C10 121.0(3) . . ?
C2 C1 C6 119.3(4) . . ?
C2 C1 Sb1 120.7(3) . . ?
C6 C1 Sb1 120.0(3) . . ?
N1 C7 C2 110.4(3) . . ?
N1 C7 H7A 109.6 . . ?
C2 C7 H7A 109.5 . . ?
N1 C7 H7B 109.6 . . ?
C2 C7 H7B 109.6 . . ?
H7A C7 H7B 108.2 . . ?
C4 C5 C6 120.7(4) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.6 . . ?
N2 C11 H11A 109.4 . . ?
N2 C11 H11B 109.7 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.3 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C10 C6 111.5(3) . . ?
N2 C10 H10A 109.1 . . ?
C6 C10 H10A 109.3 . . ?
N2 C10 H10B 109.5 . . ?
C6 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C1 C2 C3 120.0(4) . . ?
C1 C2 C7 120.2(4) . . ?
C3 C2 C7 119.7(4) . . ?
N2 C12 H12A 109.7 . . ?
N2 C12 H12B 109.4 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.4 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 119.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.8 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.1 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Cl2 C13 Cl1 111.2(3) . . ?
Cl2 C13 H13A 109.4 . . ?
Cl1 C13 H13A 109.2 . . ?
Cl2 C13 H13B 109.5 . . ?
Cl1 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C3 C4 C5 119.6(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.2 . . ?
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
Sb1 C1 2.161(4) . ?
Sb1 S1 2.4789(10) 2_566 ?
Sb1 S1 2.4875(10) . ?
S1 Sb1 2.4790(10) 2_566 ?
Cl1 C13 1.745(6) . ?
Cl2 C13 1.735(6) . ?
C8 N1 1.460(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N2 C10 1.457(5) . ?
N2 C11 1.461(6) . ?
N2 C12 1.464(5) . ?
N1 C9 1.461(6) . ?
N1 C7 1.468(5) . ?
C6 C5 1.393(6) . ?
C6 C1 1.400(6) . ?
C6 C10 1.503(6) . ?
C1 C2 1.390(6) . ?
C7 C2 1.512(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C5 C4 1.382(7) . ?
C5 H5 0.9299 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C10 H10A 0.9699 . ?
C10 H10B 0.9700 . ?
C2 C3 1.391(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C3 C4 1.375(7) . ?
C3 H3 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C13 H13A 0.9701 . ?
C13 H13B 0.9700 . ?
C4 H4 0.9300 . ?
