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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/42/4324247.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_4324247
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 N6 Ni '
_chemical_formula_sum            'C9 H30 In N6 Ni S7 Sb3'
_chemical_formula_weight         985.67
_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                 117.05(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.668(2)
_cell_length_b                   16.207(3)
_cell_length_c                   18.247(6)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.14
_cell_volume                     2809.7(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1064
_diffrn_reflns_av_sigmaI/netI    0.2276
_diffrn_reflns_limit_h_max       11
_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       -15
_diffrn_reflns_number            15162
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    4.844
_exptl_absorpt_correction_T_max  0.7938
_exptl_absorpt_correction_T_min  0.6179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.330
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.667
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.292
_refine_ls_extinction_coef       0.0033(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   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4975
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0897
_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)+(0.0821P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2146
_reflns_number_gt                2426
_reflns_number_total             4975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101912s_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C9 H30 In N6 Ni S7 Sb3 '
_cod_database_code               4324247
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 -0.04568(13) -0.10429(9) -0.08969(8) 0.0386(5) Uani 1 1 d .
Sb2 Sb 0.34594(14) 0.09751(9) -0.11295(9) 0.0401(5) Uani 1 1 d .
Sb3 Sb 0.1715(6) 0.1632(4) -0.3408(4) 0.0439(14) Uani 0.60 1 d P
Sb3' Sb 0.2163(8) 0.1836(6) -0.3236(6) 0.0323(17) Uani 0.40 1 d P
In1 In 0.30289(13) -0.00806(8) 0.05709(8) 0.0315(5) Uani 1 1 d .
S1 S 0.0276(6) -0.2458(4) -0.1002(4) 0.058(2) Uani 1 1 d .
S2 S -0.2520(6) -0.1355(4) -0.0707(5) 0.068(2) Uani 1 1 d .
S3 S 0.1101(5) -0.0913(3) 0.0567(3) 0.0339(13) Uani 1 1 d .
S4 S 0.3113(6) -0.0404(3) -0.0712(3) 0.0432(15) Uani 1 1 d .
S5 S 0.1234(5) 0.0967(4) -0.2396(4) 0.0572(19) Uani 1 1 d .
S6 S 0.4863(5) 0.0529(4) -0.1798(3) 0.0436(15) Uani 1 1 d .
S7' S 0.3267(11) 0.2782(7) -0.2266(7) 0.071(3) Uani 0.60 1 d P
S7 S 0.0458(16) 0.0615(9) -0.4415(8) 0.050(4) Uani 0.40 1 d P
Ni1 Ni 0.2094(3) -0.30875(17) 0.19729(17) 0.0423(8) Uani 1 1 d .
N1 N 0.1905(18) -0.1931(12) 0.2447(11) 0.069(3) Uani 1 1 d DU
H1D H 0.1737 -0.1537 0.2066 0.083 Uiso 1 1 calc R
H1E H 0.1175 -0.1942 0.2567 0.083 Uiso 1 1 calc R
N2 N 0.3957(19) -0.3067(12) 0.3126(11) 0.072(3) Uani 1 1 d DU
H2B H 0.4062 -0.3561 0.3373 0.086 Uiso 1 1 calc R
H2C H 0.4709 -0.2984 0.3035 0.086 Uiso 1 1 calc R
N3 N 0.0117(18) -0.2976(13) 0.0920(12) 0.071(3) Uani 1 1 d DU
H3C H -0.0043 -0.2443 0.0768 0.085 Uiso 1 1 calc R
H3D H 0.0129 -0.3264 0.0501 0.085 Uiso 1 1 calc R
N4 N 0.0812(17) -0.3682(12) 0.2428(11) 0.070(3) Uani 1 1 d DU
H4D H 0.1203 -0.4168 0.2659 0.084 Uiso 1 1 calc R
H4E H 0.0759 -0.3366 0.2819 0.084 Uiso 1 1 calc R
N5 N 0.3139(19) -0.2636(11) 0.1319(12) 0.069(3) Uani 1 1 d DU
H5B H 0.2579 -0.2274 0.0936 0.083 Uiso 1 1 calc R
H5C H 0.3924 -0.2368 0.1667 0.083 Uiso 1 1 calc R
N6 N 0.260(2) -0.4238(12) 0.1567(12) 0.073(3) Uani 1 1 d DU
H6C H 0.2943 -0.4599 0.1988 0.087 Uiso 1 1 calc R
H6D H 0.1811 -0.4457 0.1162 0.087 Uiso 1 1 calc R
C1 C 0.315(3) -0.1025(15) 0.3618(16) 0.092(6) Uani 1 1 d DU
H1A H 0.2686 -0.0587 0.3238 0.138 Uiso 1 1 calc R
H1B H 0.4101 -0.0862 0.3982 0.138 Uiso 1 1 calc R
H1C H 0.2659 -0.1143 0.3933 0.138 Uiso 1 1 calc R
C2 C 0.318(2) -0.1741(12) 0.3178(13) 0.072(4) Uani 1 1 d DU
H2A H 0.3804 -0.1568 0.2946 0.087 Uiso 1 1 calc R
C3 C 0.391(3) -0.2434(13) 0.3662(13) 0.079(4) Uani 1 1 d DU
H3A H 0.3435 -0.2637 0.3969 0.095 Uiso 1 1 calc R
H3B H 0.4861 -0.2276 0.4051 0.095 Uiso 1 1 calc R
C4 C -0.245(2) -0.3342(16) 0.0490(15) 0.083(6) Uani 1 1 d DU
H4A H -0.2637 -0.2962 0.0048 0.125 Uiso 1 1 calc R
H4B H -0.3033 -0.3213 0.0747 0.125 Uiso 1 1 calc R
H4C H -0.2639 -0.3894 0.0277 0.125 Uiso 1 1 calc R
C5 C -0.0999(19) -0.3278(15) 0.1084(13) 0.077(4) Uani 1 1 d DU
H5A H -0.1096 -0.2781 0.1360 0.092 Uiso 1 1 calc R
C6 C -0.0583(19) -0.3822(14) 0.1771(12) 0.072(4) Uani 1 1 d DU
H6A H -0.0637 -0.4385 0.1578 0.087 Uiso 1 1 calc R
H6B H -0.1253 -0.3769 0.1992 0.087 Uiso 1 1 calc R
C7 C 0.385(3) -0.4754(16) 0.0834(16) 0.094(6) Uani 1 1 d DU
H7A H 0.3854 -0.5268 0.1096 0.141 Uiso 1 1 calc R
H7B H 0.4743 -0.4679 0.0832 0.141 Uiso 1 1 calc R
H7C H 0.3115 -0.4760 0.0278 0.141 Uiso 1 1 calc R
C8 C 0.362(3) -0.4094(13) 0.1273(15) 0.074(4) Uani 1 1 d DU
H8A H 0.4506 -0.4065 0.1781 0.088 Uiso 1 1 calc R
C9 C 0.351(3) -0.3296(12) 0.0925(15) 0.077(4) Uani 1 1 d DU
H9A H 0.2806 -0.3318 0.0353 0.092 Uiso 1 1 calc R
H9B H 0.4401 -0.3162 0.0936 0.092 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'
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'
Ni Ni 0.3393 1.1124 '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 S2 94.1(2) . .
S3 Sb1 S1 94.82(19) . .
S2 Sb1 S1 99.0(2) . .
S6 Sb2 S4 95.7(2) . .
S6 Sb2 S5 94.6(2) . .
S4 Sb2 S5 94.04(19) . .
Sb3' Sb3 S7 154(2) . .
Sb3' Sb3 S5 105(2) . .
S7 Sb3 S5 92.4(4) . .
Sb3' Sb3 S1 104.4(19) . 2_554
S7 Sb3 S1 90.3(4) . 2_554
S5 Sb3 S1 99.6(3) . 2_554
Sb3' Sb3 S7' 23.0(19) . .
S7 Sb3 S7' 177.2(6) . .
S5 Sb3 S7' 89.2(4) . .
S1 Sb3 S7' 91.7(4) 2_554 .
Sb3 Sb3' S7' 152(2) . .
Sb3 Sb3' S5 62.8(19) . .
S7' Sb3' S5 96.4(5) . .
Sb3 Sb3' S1 63.8(18) . 2_554
S7' Sb3' S1 99.3(5) . 2_554
S5 Sb3' S1 89.8(3) . 2_554
Sb3 Sb3' S7 21.0(18) . .
S7' Sb3' S7 172.5(7) . .
S5 Sb3' S7 77.7(4) . .
S1 Sb3' S7 76.3(4) 2_554 .
S2 In1 S4 114.3(2) 3 .
S2 In1 S6 110.2(2) 3 3_655
S4 In1 S6 113.1(2) . 3_655
S2 In1 S3 107.50(19) 3 .
S4 In1 S3 106.00(18) . .
S6 In1 S3 104.99(19) 3_655 .
Sb3 S1 Sb1 111.1(2) 2_544 .
Sb1 S1 Sb3' 100.2(3) . 2_544
In1 S2 Sb1 94.2(2) 3 .
Sb1 S3 In1 101.7(2) . .
In1 S4 Sb2 100.34(19) . .
Sb3 S5 Sb2 105.7(2) . .
Sb2 S5 Sb3' 95.0(3) . .
Sb2 S6 In1 98.6(2) . 3_655
N5 Ni1 N1 95.6(8) . .
N5 Ni1 N3 91.3(7) . .
N1 Ni1 N3 93.1(7) . .
N5 Ni1 N4 169.0(7) . .
N1 Ni1 N4 92.5(8) . .
N3 Ni1 N4 80.8(7) . .
N5 Ni1 N2 93.3(8) . .
N1 Ni1 N2 78.6(7) . .
N3 Ni1 N2 170.9(8) . .
N4 Ni1 N2 95.6(7) . .
N5 Ni1 N6 80.1(7) . .
N1 Ni1 N6 172.1(7) . .
N3 Ni1 N6 93.6(8) . .
N4 Ni1 N6 92.6(8) . .
N2 Ni1 N6 94.9(7) . .
C2 N1 Ni1 110.1(13) . .
C2 N1 H1D 109.6 . .
Ni1 N1 H1D 109.6 . .
C2 N1 H1E 109.6 . .
Ni1 N1 H1E 109.6 . .
H1D N1 H1E 108.1 . .
C3 N2 Ni1 112.2(14) . .
C3 N2 H2B 109.2 . .
Ni1 N2 H2B 109.2 . .
C3 N2 H2C 109.2 . .
Ni1 N2 H2C 109.2 . .
H2B N2 H2C 107.9 . .
C5 N3 Ni1 111.0(13) . .
C5 N3 H3C 109.4 . .
Ni1 N3 H3C 109.4 . .
C5 N3 H3D 109.4 . .
Ni1 N3 H3D 109.4 . .
H3C N3 H3D 108.0 . .
C6 N4 Ni1 110.5(15) . .
C6 N4 H4D 109.5 . .
Ni1 N4 H4D 109.5 . .
C6 N4 H4E 109.5 . .
Ni1 N4 H4E 109.5 . .
H4D N4 H4E 108.1 . .
C9 N5 Ni1 111.1(15) . .
C9 N5 H5B 109.4 . .
Ni1 N5 H5B 109.4 . .
C9 N5 H5C 109.4 . .
Ni1 N5 H5C 109.4 . .
H5B N5 H5C 108.0 . .
C8 N6 Ni1 109.6(14) . .
C8 N6 H6C 109.8 . .
Ni1 N6 H6C 109.8 . .
C8 N6 H6D 109.8 . .
Ni1 N6 H6D 109.8 . .
H6C N6 H6D 108.2 . .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C1 C2 C3 116.1(19) . .
C1 C2 N1 116.6(19) . .
C3 C2 N1 115.2(18) . .
C1 C2 H2A 101.7 . .
C3 C2 H2A 101.7 . .
N1 C2 H2A 101.7 . .
C2 C3 N2 108.7(19) . .
C2 C3 H3A 109.9 . .
N2 C3 H3A 109.9 . .
C2 C3 H3B 109.9 . .
N2 C3 H3B 109.9 . .
H3A C3 H3B 108.3 . .
C5 C4 H4A 109.5 . .
C5 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C5 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C6 C5 C4 114.6(18) . .
C6 C5 N3 115.9(17) . .
C4 C5 N3 125(2) . .
C6 C5 H5A 96.8 . .
C4 C5 H5A 96.8 . .
N3 C5 H5A 96.8 . .
C5 C6 N4 115.0(18) . .
C5 C6 H6A 108.5 . .
N4 C6 H6A 108.5 . .
C5 C6 H6B 108.5 . .
N4 C6 H6B 108.5 . .
H6A C6 H6B 107.5 . .
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 C7 116(2) . .
C9 C8 N6 113(2) . .
C7 C8 N6 116(2) . .
C9 C8 H8A 103.1 . .
C7 C8 H8A 103.1 . .
N6 C8 H8A 103.1 . .
C8 C9 N5 116(2) . .
C8 C9 H9A 108.3 . .
N5 C9 H9A 108.3 . .
C8 C9 H9B 108.3 . .
N5 C9 H9B 108.3 . .
H9A C9 H9B 107.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 S3 2.430(5) .
Sb1 S2 2.433(6) .
Sb1 S1 2.458(6) .
Sb2 S6 2.431(6) .
Sb2 S4 2.443(6) .
Sb2 S5 2.446(5) .
Sb3 Sb3' 0.548(8) .
Sb3 S7 2.377(14) .
Sb3 S5 2.387(10) .
Sb3 S1 2.401(9) 2_554
Sb3 S7' 2.724(12) .
Sb3' S7' 2.230(13) .
Sb3' S5 2.587(12) .
Sb3' S1 2.593(11) 2_554
Sb3' S7 2.881(15) .
In1 S2 2.427(6) 3
In1 S4 2.440(6) .
In1 S6 2.453(5) 3_655
In1 S3 2.457(5) .
S1 Sb3 2.401(9) 2_544
S1 Sb3' 2.593(11) 2_544
S2 In1 2.427(6) 3
S6 In1 2.453(5) 3_655
Ni1 N5 2.10(2) .
Ni1 N1 2.112(19) .
Ni1 N3 2.119(17) .
Ni1 N4 2.13(2) .
Ni1 N2 2.138(18) .
Ni1 N6 2.162(19) .
N1 C2 1.44(3) .
N1 H1D 0.9000 .
N1 H1E 0.9000 .
N2 C3 1.43(3) .
N2 H2B 0.9000 .
N2 H2C 0.9000 .
N3 C5 1.44(3) .
N3 H3C 0.9000 .
N3 H3D 0.9000 .
N4 C6 1.44(3) .
N4 H4D 0.9000 .
N4 H4E 0.9000 .
N5 C9 1.44(3) .
N5 H5B 0.9000 .
N5 H5C 0.9000 .
N6 C8 1.43(4) .
N6 H6C 0.9000 .
N6 H6D 0.9000 .
C1 C2 1.42(3) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 C3 1.42(3) .
C2 H2A 0.9800 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C5 1.43(3) .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 C6 1.43(3) .
C5 H5A 0.9800 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C8 1.42(4) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C9 1.42(3) .
C8 H8A 0.9800 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
