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#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/22/7022246.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_7022246
loop_
_publ_author_name
'Zhou, Jian'
'Liu, Xing'
'An, Litao'
'Hu, Feilong'
'Kan, Yuhe'
'Li, Rong'
'Shen, Zhenming'
_publ_section_title
;
 Solvothermal synthesis and characterization of thioindate-thioantimonates
 with transition-metal complexes: the first examples of the incorporation
 of transition metal ions into In-S-Sb frameworks.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1735
_journal_page_last               1742
_journal_paper_doi               10.1039/c2dt32132g
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C6 H18 Co In N4 S4 Sb '
_chemical_formula_sum            'C6 H18 Co In N4 S4 Sb'
_chemical_formula_weight         570.03
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.788(2)
_cell_length_b                   13.689(3)
_cell_length_c                   11.116(2)
_cell_measurement_reflns_used    16860
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      1.95
_cell_volume                     1591.2(7)
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_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  0.1304
_diffrn_reflns_av_sigmaI/netI    0.1476
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17848
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    4.662
_exptl_absorpt_correction_T_max  0.8355
_exptl_absorpt_correction_T_min  0.6281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.656
_refine_diff_density_min         -2.316
_refine_diff_density_rms         0.330
_refine_ls_extinction_coef       0.0021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2909
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0875
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+82.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1907
_refine_ls_wR_factor_ref         0.1999
_reflns_number_gt                1662
_reflns_number_total             2909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32132g.txt
_cod_data_source_block           3
_cod_original_cell_volume        1591.3(6)
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7022246
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.07992(14) 0.26194(11) 0.25961(17) 0.0376(5) Uani 1 1 d .
In1 In 0.11859(15) 0.42358(11) 0.54933(17) 0.0379(5) Uani 1 1 d .
Co1 Co 0.2206(3) 0.4614(2) 0.1318(3) 0.0396(8) Uani 1 1 d .
S1 S 0.0567(5) 0.3475(4) 0.0586(6) 0.0403(15) Uani 1 1 d .
S2 S 0.2437(6) 0.1459(4) 0.2779(6) 0.0410(15) Uani 1 1 d .
S3 S 0.2400(6) 0.3638(4) 0.4313(7) 0.0442(16) Uani 1 1 d .
S4 S 0.1138(6) 0.6043(4) 0.5533(7) 0.0479(16) Uani 1 1 d .
N4 N 0.184(2) 0.5279(16) -0.050(2) 0.062(7) Uani 1 1 d .
H4C H 0.1872 0.4816 -0.1059 0.075 Uiso 1 1 calc R
H4D H 0.1026 0.5503 -0.0881 0.075 Uiso 1 1 calc R
N2 N 0.185(2) 0.5670(15) 0.244(2) 0.052(6) Uani 1 1 d .
H2C H 0.1232 0.6065 0.1857 0.062 Uiso 1 1 calc R
H2D H 0.1532 0.5366 0.2939 0.062 Uiso 1 1 calc R
N1 N 0.3882(17) 0.5589(14) 0.1937(18) 0.046(5) Uani 1 1 d D
N3 N 0.3668(16) 0.3598(14) 0.192(2) 0.051(5) Uani 1 1 d U
H3C H 0.3681 0.3259 0.2616 0.061 Uiso 1 1 calc R
H3D H 0.3465 0.3175 0.1228 0.061 Uiso 1 1 calc R
C6 C 0.265(3) 0.607(3) -0.047(3) 0.091(11) Uani 1 1 d DU
H6A H 0.2258 0.6692 -0.0451 0.109 Uiso 1 1 calc R
H6B H 0.2772 0.6057 -0.1275 0.109 Uiso 1 1 calc R
C5 C 0.391(3) 0.597(3) 0.077(3) 0.095(11) Uani 1 1 d DU
H5A H 0.4453 0.5559 0.0545 0.115 Uiso 1 1 calc R
H5B H 0.4306 0.6614 0.0991 0.115 Uiso 1 1 calc R
C3 C 0.502(2) 0.5019(17) 0.258(3) 0.074(8) Uani 1 1 d DU
H3A H 0.5358 0.5110 0.3553 0.089 Uiso 1 1 calc R
H3B H 0.5635 0.5289 0.2328 0.089 Uiso 1 1 calc R
C2 C 0.289(3) 0.627(3) 0.334(4) 0.098(13) Uani 1 1 d D
H2A H 0.3290 0.5994 0.4244 0.118 Uiso 1 1 calc R
H2B H 0.2578 0.6921 0.3393 0.118 Uiso 1 1 calc R
C4 C 0.494(3) 0.3941(17) 0.232(4) 0.081(8) Uani 1 1 d DU
H4A H 0.5175 0.3805 0.1604 0.097 Uiso 1 1 calc R
H4B H 0.5536 0.3601 0.3129 0.097 Uiso 1 1 calc R
C1 C 0.383(3) 0.634(2) 0.280(4) 0.100(12) Uani 1 1 d DU
H1A H 0.3680 0.6949 0.2304 0.120 Uiso 1 1 calc R
H1B H 0.4678 0.6384 0.3568 0.120 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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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_
_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
S3 Sb1 S1 99.5(2) . .
S3 Sb1 S2 90.6(2) . .
S1 Sb1 S2 98.1(2) . .
S4 In1 S2 115.2(2) 3_566 4_566
S4 In1 S4 97.68(18) 3_566 .
S2 In1 S4 112.0(2) 4_566 .
S4 In1 S3 119.5(2) 3_566 .
S2 In1 S3 101.6(2) 4_566 .
S4 In1 S3 111.3(2) . .
S4 In1 In1 49.01(14) 3_566 3_566
S2 In1 In1 127.47(18) 4_566 3_566
S4 In1 In1 48.66(14) . 3_566
S3 In1 In1 130.49(18) . 3_566
N3 Co1 N4 112.2(9) . .
N3 Co1 N2 130.0(9) . .
N4 Co1 N2 105.8(8) . .
N3 Co1 N1 79.3(7) . .
N4 Co1 N1 78.1(7) . .
N2 Co1 N1 78.0(8) . .
N3 Co1 S1 95.5(5) . .
N4 Co1 S1 100.8(6) . .
N2 Co1 S1 108.2(6) . .
N1 Co1 S1 173.7(5) . .
Co1 S1 Sb1 106.3(2) . .
Sb1 S2 In1 95.3(2) . 4_565
Sb1 S3 In1 100.2(2) . .
In1 S4 In1 82.32(18) 3_566 .
C6 N4 Co1 118.0(18) . .
C6 N4 H4C 107.8 . .
Co1 N4 H4C 107.8 . .
C6 N4 H4D 107.8 . .
Co1 N4 H4D 107.8 . .
H4C N4 H4D 107.1 . .
C2 N2 Co1 118.5(18) . .
C2 N2 H2C 107.7 . .
Co1 N2 H2C 107.7 . .
C2 N2 H2D 107.7 . .
Co1 N2 H2D 107.7 . .
H2C N2 H2D 107.1 . .
C5 N1 C1 112(3) . .
C5 N1 C3 105(2) . .
C1 N1 C3 112(2) . .
C5 N1 Co1 109.5(16) . .
C1 N1 Co1 109.7(17) . .
C3 N1 Co1 108.8(15) . .
C4 N3 Co1 118.5(15) . .
C4 N3 H3C 107.7 . .
Co1 N3 H3C 107.7 . .
C4 N3 H3D 107.7 . .
Co1 N3 H3D 107.7 . .
H3C N3 H3D 107.1 . .
N4 C6 C5 109(3) . .
N4 C6 H6A 109.9 . .
C5 C6 H6A 109.9 . .
N4 C6 H6B 109.9 . .
C5 C6 H6B 109.9 . .
H6A C6 H6B 108.3 . .
N1 C5 C6 116(3) . .
N1 C5 H5A 108.2 . .
C6 C5 H5A 108.2 . .
N1 C5 H5B 108.2 . .
C6 C5 H5B 108.2 . .
H5A C5 H5B 107.3 . .
N1 C3 C4 119(2) . .
N1 C3 H3A 107.6 . .
C4 C3 H3A 107.6 . .
N1 C3 H3B 107.6 . .
C4 C3 H3B 107.6 . .
H3A C3 H3B 107.0 . .
N2 C2 C1 108(3) . .
N2 C2 H2A 110.1 . .
C1 C2 H2A 110.1 . .
N2 C2 H2B 110.1 . .
C1 C2 H2B 110.1 . .
H2A C2 H2B 108.4 . .
N3 C4 C3 110(2) . .
N3 C4 H4A 109.7 . .
C3 C4 H4A 109.7 . .
N3 C4 H4B 109.7 . .
C3 C4 H4B 109.7 . .
H4A C4 H4B 108.2 . .
N1 C1 C2 120(3) . .
N1 C1 H1A 107.4 . .
C2 C1 H1A 107.4 . .
N1 C1 H1B 107.4 . .
C2 C1 H1B 107.4 . .
H1A C1 H1B 106.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 S3 2.413(6) .
Sb1 S1 2.424(6) .
Sb1 S2 2.435(6) .
In1 S4 2.463(6) 3_566
In1 S2 2.465(6) 4_566
In1 S4 2.476(6) .
In1 S3 2.484(7) .
In1 In1 3.251(3) 3_566
Co1 N3 2.071(18) .
Co1 N4 2.07(2) .
Co1 N2 2.08(2) .
Co1 N1 2.21(2) .
Co1 S1 2.318(6) .
S2 In1 2.465(6) 4_565
S4 In1 2.463(6) 3_566
N4 C6 1.44(4) .
N4 H4C 0.9000 .
N4 H4D 0.9000 .
N2 C2 1.43(4) .
N2 H2C 0.9000 .
N2 H2D 0.9000 .
N1 C5 1.418(19) .
N1 C1 1.421(19) .
N1 C3 1.423(19) .
N3 C4 1.43(3) .
N3 H3C 0.9000 .
N3 H3D 0.9000 .
C6 C5 1.492(10) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C3 C4 1.500(10) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C2 C1 1.495(10) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
