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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/4/32/42/4324246.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_4324246
loop_
_publ_author_name
'Jian Zhou'
'Litao An'
'Feng Zhang'
_publ_section_title
;
 [M(dap)3]InSb3S7 (M = Co, Ni): Two Novel Open-Framework
 Thioindate-Thioantimonates with 8-, 12-, and 16-Ring Intersecting
 Channels
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              415
_journal_page_last               417
_journal_paper_doi               10.1021/ic101912s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'In S7 Sb3, C9 H30 Co N6 '
_chemical_formula_sum            'C9 H30 Co In N6 S7 Sb3'
_chemical_formula_weight         985.91
_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                 117.15(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.716(2)
_cell_length_b                   16.219(3)
_cell_length_c                   18.237(6)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.30
_cell_volume                     2820.4(13)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1543
_diffrn_reflns_av_sigmaI/netI    0.2565
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16601
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    4.746
_exptl_absorpt_correction_T_max  0.7973
_exptl_absorpt_correction_T_min  0.6747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.322
_exptl_crystal_description       block
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.220
_refine_diff_density_min         -1.377
_refine_diff_density_rms         0.314
_refine_ls_extinction_coef       0.0060(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4995
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.0892
_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)+(0.0773P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2037
_refine_ls_wR_factor_ref         0.2176
_reflns_number_gt                2323
_reflns_number_total             4995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101912s_si_001.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4324246
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 0.45454(15) -0.10321(8) -0.08968(9) 0.0403(5) Uani 1 1 d U
Sb2 Sb 1.15157(15) -0.09740(8) 0.11160(9) 0.0429(5) Uani 1 1 d .
Sb3 Sb 1.3094(2) -0.17275(11) 0.33308(11) 0.0707(7) Uani 1 1 d U
In1 In 0.80273(15) -0.00796(8) 0.05756(9) 0.0342(5) Uani 1 1 d .
S1 S 0.2506(6) -0.1362(3) -0.0696(5) 0.067(2) Uani 1 1 d U
S2 S 0.5277(6) -0.2444(4) -0.1014(4) 0.0629(19) Uani 1 1 d U
S3 S 0.6110(6) -0.0921(3) 0.0568(3) 0.0388(13) Uani 1 1 d .
S4 S 1.0131(6) -0.0517(4) 0.1795(3) 0.0429(14) Uani 1 1 d .
S5 S 1.1873(6) 0.0409(3) 0.0706(3) 0.0424(14) Uani 1 1 d .
S6 S 1.3734(6) -0.0982(4) 0.2372(4) 0.066(2) Uani 1 1 d .
S7' S 1.4466(16) -0.0622(9) 0.4372(10) 0.078(4) Uani 0.493(12) 1 d PU
S7 S 1.1702(16) -0.2789(9) 0.2248(8) 0.082(4) Uani 0.507(12) 1 d PU
Co1 Co 0.7093(3) -0.30889(17) 0.19642(19) 0.0439(8) Uani 1 1 d .
N1 N 0.824(2) -0.2642(11) 0.1354(12) 0.076(3) Uani 1 1 d DU
H1A H 0.7732 -0.2255 0.0987 0.091 Uiso 1 1 calc R
H1B H 0.9038 -0.2403 0.1727 0.091 Uiso 1 1 calc R
N2 N 0.764(2) -0.4222(12) 0.1576(12) 0.076(3) Uani 1 1 d DU
H2A H 0.8009 -0.4571 0.2006 0.091 Uiso 1 1 calc R
H2B H 0.6859 -0.4456 0.1183 0.091 Uiso 1 1 calc R
N3 N 0.6855(19) -0.1896(12) 0.2427(12) 0.075(3) Uani 1 1 d DU
H3A H 0.6652 -0.1507 0.2037 0.090 Uiso 1 1 calc R
H3B H 0.6154 -0.1914 0.2570 0.090 Uiso 1 1 calc R
N4 N 0.899(2) -0.3075(12) 0.3125(12) 0.078(3) Uani 1 1 d DU
H4A H 0.9088 -0.3557 0.3390 0.094 Uiso 1 1 calc R
H4B H 0.9743 -0.3005 0.3035 0.094 Uiso 1 1 calc R
N5 N 0.5805(19) -0.3704(13) 0.2440(12) 0.077(3) Uani 1 1 d DU
H5A H 0.6194 -0.4192 0.2661 0.092 Uiso 1 1 calc R
H5B H 0.5770 -0.3394 0.2839 0.092 Uiso 1 1 calc R
N6 N 0.5030(19) -0.2971(13) 0.0920(12) 0.072(3) Uani 1 1 d DU
H6A H 0.4864 -0.2437 0.0771 0.086 Uiso 1 1 calc R
H6B H 0.5006 -0.3256 0.0490 0.086 Uiso 1 1 calc R
C1 C 0.892(3) -0.4771(15) 0.0872(17) 0.090(5) Uani 1 1 d DU
H1C H 0.9625 -0.4617 0.0711 0.135 Uiso 1 1 calc R
H1D H 0.8082 -0.4931 0.0394 0.135 Uiso 1 1 calc R
H1E H 0.9255 -0.5226 0.1251 0.135 Uiso 1 1 calc R
C2 C 0.862(3) -0.4084(12) 0.1263(16) 0.075(4) Uani 1 1 d DU
H2C H 0.9499 -0.4053 0.1778 0.090 Uiso 1 1 calc R
C3 C 0.859(3) -0.3281(12) 0.0936(16) 0.081(4) Uani 1 1 d DU
H3C H 0.7912 -0.3277 0.0358 0.097 Uiso 1 1 calc R
H3D H 0.9505 -0.3163 0.0970 0.097 Uiso 1 1 calc R
C4 C 0.816(3) -0.1038(15) 0.3642(16) 0.101(6) Uani 1 1 d DU
H4C H 0.9044 -0.1013 0.4127 0.151 Uiso 1 1 calc R
H4D H 0.7423 -0.1119 0.3800 0.151 Uiso 1 1 calc R
H4E H 0.7998 -0.0531 0.3341 0.151 Uiso 1 1 calc R
C5 C 0.816(2) -0.1709(13) 0.3134(14) 0.083(4) Uani 1 1 d DU
H5C H 0.8761 -0.1514 0.2896 0.100 Uiso 1 1 calc R
C6 C 0.889(3) -0.2410(13) 0.3614(14) 0.088(4) Uani 1 1 d DU
H6C H 0.8418 -0.2605 0.3923 0.106 Uiso 1 1 calc R
H6D H 0.9833 -0.2243 0.4007 0.106 Uiso 1 1 calc R
C7 C 0.253(2) -0.3341(17) 0.0496(16) 0.094(6) Uani 1 1 d DU
H7A H 0.1976 -0.3576 0.0735 0.140 Uiso 1 1 calc R
H7B H 0.2479 -0.3689 0.0057 0.140 Uiso 1 1 calc R
H7C H 0.2173 -0.2803 0.0281 0.140 Uiso 1 1 calc R
C8 C 0.3960(19) -0.3273(15) 0.1115(13) 0.078(4) Uani 1 1 d DU
H8A H 0.3861 -0.2780 0.1395 0.094 Uiso 1 1 calc R
C9 C 0.441(2) -0.3834(14) 0.1793(13) 0.072(4) Uani 1 1 d DU
H9C H 0.4353 -0.4390 0.1584 0.086 Uiso 1 1 calc R
H9A H 0.3762 -0.3797 0.2028 0.086 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'
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'
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'
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 93.9(2) . .
S3 Sb1 S2 94.4(2) . .
S1 Sb1 S2 98.7(2) . .
S6 Sb2 S4 94.8(2) . .
S6 Sb2 S5 94.0(2) . .
S4 Sb2 S5 95.30(18) . .
S6 Sb3 S2 95.8(2) . 4_656
S6 Sb3 S7 92.1(4) . .
S2 Sb3 S7 95.6(3) 4_656 .
S6 Sb3 S7' 86.0(3) . .
S2 Sb3 S7' 85.7(4) 4_656 .
S7 Sb3 S7' 177.8(4) . .
S4 In1 S1 110.7(2) . 3_655
S4 In1 S5 112.47(18) . 3_755
S1 In1 S5 114.1(2) 3_655 3_755
S4 In1 S3 105.42(19) . .
S1 In1 S3 107.62(18) 3_655 .
S5 In1 S3 105.90(18) 3_755 .
Sb1 S1 In1 93.8(2) . 3_655
Sb1 S2 Sb3 106.2(2) . 4_455
Sb1 S3 In1 101.70(18) . .
In1 S4 Sb2 98.57(19) . .
In1 S5 Sb2 99.95(18) 3_755 .
Sb2 S6 Sb3 101.6(2) . .
N1 Co1 N2 79.0(7) . .
N1 Co1 N4 89.9(8) . .
N2 Co1 N4 93.2(7) . .
N1 Co1 N6 96.4(7) . .
N2 Co1 N6 96.2(8) . .
N4 Co1 N6 169.6(7) . .
N1 Co1 N3 95.7(7) . .
N2 Co1 N3 171.8(7) . .
N4 Co1 N3 80.5(7) . .
N6 Co1 N3 90.5(7) . .
N1 Co1 N5 170.7(8) . .
N2 Co1 N5 93.2(7) . .
N4 Co1 N5 95.6(8) . .
N6 Co1 N5 79.3(7) . .
N3 Co1 N5 92.6(8) . .
C3 N1 Co1 112.7(15) . .
C3 N1 H1A 109.0 . .
Co1 N1 H1A 109.0 . .
C3 N1 H1B 109.0 . .
Co1 N1 H1B 109.0 . .
H1A N1 H1B 107.8 . .
C2 N2 Co1 111.2(13) . .
C2 N2 H2A 109.4 . .
Co1 N2 H2A 109.4 . .
C2 N2 H2B 109.4 . .
Co1 N2 H2B 109.4 . .
H2A N2 H2B 108.0 . .
C5 N3 Co1 107.4(14) . .
C5 N3 H3A 110.2 . .
Co1 N3 H3A 110.2 . .
C5 N3 H3B 110.2 . .
Co1 N3 H3B 110.2 . .
H3A N3 H3B 108.5 . .
C6 N4 Co1 108.3(15) . .
C6 N4 H4A 110.0 . .
Co1 N4 H4A 110.0 . .
C6 N4 H4B 110.0 . .
Co1 N4 H4B 110.0 . .
H4A N4 H4B 108.4 . .
C9 N5 Co1 110.5(14) . .
C9 N5 H5A 109.5 . .
Co1 N5 H5A 109.5 . .
C9 N5 H5B 109.5 . .
Co1 N5 H5B 109.5 . .
H5A N5 H5B 108.1 . .
C8 N6 Co1 111.2(13) . .
C8 N6 H6A 109.4 . .
Co1 N6 H6A 109.4 . .
C8 N6 H6B 109.4 . .
Co1 N6 H6B 109.4 . .
H6A N6 H6B 108.0 . .
C2 C1 H1C 109.5 . .
C2 C1 H1D 109.5 . .
H1C C1 H1D 109.5 . .
C2 C1 H1E 109.5 . .
H1C C1 H1E 109.5 . .
H1D C1 H1E 109.5 . .
C3 C2 N2 115.4(19) . .
C3 C2 C1 118.0(19) . .
N2 C2 C1 116.7(19) . .
C3 C2 H2C 100.6 . .
N2 C2 H2C 100.6 . .
C1 C2 H2C 100.6 . .
C2 C3 N1 113.5(19) . .
C2 C3 H3C 108.9 . .
N1 C3 H3C 108.9 . .
C2 C3 H3D 108.9 . .
N1 C3 H3D 108.9 . .
H3C C3 H3D 107.7 . .
C5 C4 H4C 109.5 . .
C5 C4 H4D 109.5 . .
H4C C4 H4D 109.5 . .
C5 C4 H4E 109.5 . .
H4C C4 H4E 109.5 . .
H4D C4 H4E 109.5 . .
C4 C5 C6 112(2) . .
C4 C5 N3 117(2) . .
C6 C5 N3 115(2) . .
C4 C5 H5C 103.8 . .
C6 C5 H5C 103.8 . .
N3 C5 H5C 103.8 . .
C5 C6 N4 113(2) . .
C5 C6 H6C 108.9 . .
N4 C6 H6C 108.9 . .
C5 C6 H6D 108.9 . .
N4 C6 H6D 108.9 . .
H6C C6 H6D 107.8 . .
C8 C7 H7A 109.5 . .
C8 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C8 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C9 C8 N6 116.1(18) . .
C9 C8 C7 116.7(18) . .
N6 C8 C7 121(2) . .
C9 C8 H8A 98.1 . .
N6 C8 H8A 98.1 . .
C7 C8 H8A 98.1 . .
C8 C9 N5 115.6(19) . .
C8 C9 H9C 108.4 . .
N5 C9 H9C 108.4 . .
C8 C9 H9A 108.4 . .
N5 C9 H9A 108.4 . .
H9C C9 H9A 107.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 S3 2.428(6) .
Sb1 S1 2.435(6) .
Sb1 S2 2.461(6) .
Sb2 S6 2.435(6) .
Sb2 S4 2.441(5) .
Sb2 S5 2.449(5) .
Sb3 S6 2.467(6) .
Sb3 S2 2.481(6) 4_656
Sb3 S7 2.530(17) .
Sb3 S7' 2.537(17) .
In1 S4 2.440(6) .
In1 S1 2.441(6) 3_655
In1 S5 2.447(5) 3_755
In1 S3 2.461(5) .
S1 In1 2.441(6) 3_655
S2 Sb3 2.481(6) 4_455
S5 In1 2.447(5) 3_755
Co1 N1 2.129(18) .
Co1 N2 2.143(19) .
Co1 N4 2.17(2) .
Co1 N6 2.17(2) .
Co1 N3 2.171(19) .
Co1 N5 2.178(19) .
N1 C3 1.43(3) .
N1 H1A 0.9000 .
N1 H1B 0.9000 .
N2 C2 1.42(4) .
N2 H2A 0.9000 .
N2 H2B 0.9000 .
N3 C5 1.44(3) .
N3 H3A 0.9000 .
N3 H3B 0.9000 .
N4 C6 1.43(3) .
N4 H4A 0.9000 .
N4 H4B 0.9000 .
N5 C9 1.44(3) .
N5 H5A 0.9000 .
N5 H5B 0.9000 .
N6 C8 1.43(3) .
N6 H6A 0.9000 .
N6 H6B 0.9000 .
C1 C2 1.44(4) .
C1 H1C 0.9600 .
C1 H1D 0.9600 .
C1 H1E 0.9600 .
C2 C3 1.43(3) .
C2 H2C 0.9800 .
C3 H3C 0.9700 .
C3 H3D 0.9700 .
C4 C5 1.43(3) .
C4 H4C 0.9600 .
C4 H4D 0.9600 .
C4 H4E 0.9600 .
C5 C6 1.43(3) .
C5 H5C 0.9800 .
C6 H6C 0.9700 .
C6 H6D 0.9700 .
C7 C8 1.43(3) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C9 1.43(3) .
C8 H8A 0.9800 .
C9 H9C 0.9700 .
C9 H9A 0.9700 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A S3 0.90 2.66 3.48(2) 151.4 .
N1 H1B S7 0.90 2.64 3.31(3) 131.7 .
N2 H2A S4 0.90 2.67 3.53(2) 160.7 2_745
N2 H2B S7' 0.90 2.30 3.11(3) 149.2 2_745
N3 H3A S3 0.90 2.65 3.49(2) 156.1 .
N3 H3B S6 0.90 2.88 3.618(19) 140.4 1_455
N4 H4A S5 0.90 2.85 3.64(2) 146.9 2_745
N5 H5A S5 0.90 2.82 3.47(2) 130.0 2_745
N5 H5B S2 0.90 2.74 3.63(2) 171.4 4_556
N6 H6B S7' 0.90 2.59 3.46(2) 162.2 4_455
