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#$Date: 2016-03-23 22:54:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179495 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/92/4339250.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_4339250
loop_
_publ_author_name
'Zhou, Jian'
'Bian, Guo-Qing'
'Zhang, Yong'
'Zhu, Qin-Yu'
'Li, Chun-Yin'
'Dai, Jie'
_publ_section_title
;
 One-dimensional indium sulfides with transition metal complexes of
 polyamines.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6347
_journal_page_last               6352
_journal_paper_doi               10.1021/ic070334q
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '2(C9 H30 N6 Ni), In4 S8'
_chemical_formula_sum            'C18 H60 In4 N12 Ni2 S8'
_chemical_formula_weight         1277.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      63
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.525(2)
_cell_length_b                   16.531(5)
_cell_length_c                   13.245(3)
_cell_measurement_reflns_used    3189
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.1
_cell_volume                     2085.5(9)
_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      193(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9946
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    3.491
_exptl_absorpt_correction_T_max  0.696
_exptl_absorpt_correction_T_min  0.279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            light-purple
_exptl_crystal_density_diffrn    2.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.049
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1061
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0403
_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)+(0.0627P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                933
_reflns_number_total             1061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070334q-file001.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2085.4(9)
_cod_database_code               4339250
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, 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
In In 0.5000 -0.00021(2) 0.37619(3) 0.0230(3) Uani 1 2 d S
Ni1 Ni 0.0000 0.12192(7) 0.2500 0.0267(4) Uani 1 4 d S
S1 S 0.5000 0.11045(14) 0.2500 0.0299(6) Uani 1 4 d S
S2 S 0.5000 -0.10901(16) 0.2500 0.0452(8) Uani 1 4 d S
S3 S 0.3057(2) 0.0000 0.5000 0.0386(6) Uani 1 2 d S
N1 N 0.1624(8) 0.2090(5) 0.2500 0.064(2) Uani 1 2 d SD
N2 N 0.0000 0.1298(5) 0.4125(6) 0.062(2) Uani 1 2 d S
N3 N 0.1444(8) 0.0257(5) 0.2500 0.062(2) Uani 1 2 d S
C1 C 0.1916(19) 0.2203(10) 0.3636(10) 0.080(5) Uani 0.50 1 d PD
C2 C 0.0640(13) 0.2133(8) 0.4320(8) 0.053(3) Uani 0.50 1 d P
C3 C 0.106(2) 0.2272(11) 0.5429(13) 0.112(7) Uani 0.50 1 d P
C4 C 0.0674(14) -0.0504(6) 0.2231(8) 0.059(4) Uani 0.50 1 d PD
C5 C 0.1247(17) -0.1317(9) 0.2500 0.069(6) Uani 0.50 2 d SPD
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'
Ni Ni 0.3393 1.1124 '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'
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
S2 In S3 116.91(3) . 9_656
S2 In S3 116.91(3) . .
S3 In S3 96.90(6) 9_656 .
S2 In S1 94.68(7) . .
S3 In S1 116.51(3) 9_656 .
S3 In S1 116.51(3) . .
S2 In In 133.02(5) . 9_656
S3 In In 48.45(3) 9_656 9_656
S3 In In 48.45(3) . 9_656
S1 In In 132.29(4) . 9_656
S2 In In 47.10(4) . 10_556
S3 In In 131.55(3) 9_656 10_556
S3 In In 131.55(3) . 10_556
S1 In In 47.58(4) . 10_556
In In In 179.878(14) 9_656 10_556
N3 Ni1 N3 81.7(4) 3 .
N3 Ni1 N1 173.8(3) 3 .
N3 Ni1 N1 92.1(3) . .
N3 Ni1 N1 92.1(3) 3 3
N3 Ni1 N1 173.8(3) . 3
N1 Ni1 N1 94.1(4) . 3
N3 Ni1 N2 92.63(15) 3 .
N3 Ni1 N2 92.63(15) . .
N1 Ni1 N2 87.63(14) . .
N1 Ni1 N2 87.63(14) 3 .
N3 Ni1 N2 92.63(15) 3 10_556
N3 Ni1 N2 92.63(15) . 10_556
N1 Ni1 N2 87.63(14) . 10_556
N1 Ni1 N2 87.63(14) 3 10_556
N2 Ni1 N2 173.1(4) . 10_556
In S1 In 84.83(8) 10_556 .
In S2 In 85.80(9) . 10_556
In S3 In 83.10(6) 9_656 .
C1 N1 C1 154.9(15) . 10_556
C1 N1 Ni1 102.4(7) . .
C1 N1 Ni1 102.4(7) 10_556 .
C2 N2 C2 47.0(10) . 12
C2 N2 Ni1 102.9(5) . .
C2 N2 Ni1 102.9(5) 12 .
C4 N3 Ni1 108.3(6) 10_556 .
C4 N3 Ni1 108.3(6) . .
C2 C1 N1 115.4(12) . .
C2 C2 C1 143.1(7) 12 .
C2 C2 N2 66.5(5) 12 .
C1 C2 N2 106.6(9) . .
C2 C2 C3 104.9(10) 12 .
C1 C2 C3 110.6(13) . .
N2 C2 C3 113.5(11) . .
C2 C3 C3 75.1(10) . 12
C4 C4 C5 76.2(4) 10_556 .
C4 C4 C5 111.4(8) 12 .
C4 C4 C5 101.7(8) 3 .
C4 C4 N3 76.2(4) 10_556 .
C4 C4 N3 119.3(5) 12 .
C4 C4 N3 108.2(6) 3 .
C5 C4 N3 121.3(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
In S2 2.455(2) .
In S3 2.4723(15) 9_656
In S3 2.4723(15) .
In S1 2.4779(18) .
In In 3.2796(10) 9_656
In In 3.3427(10) 10_556
Ni1 N3 2.103(7) 3
Ni1 N3 2.103(7) .
Ni1 N1 2.113(8) .
Ni1 N1 2.113(8) 3
Ni1 N2 2.156(7) .
Ni1 N2 2.156(7) 10_556
S1 In 2.4779(18) 10_556
S2 In 2.455(2) 10_556
S3 In 2.4723(15) 9_656
N1 C1 1.542(13) .
N1 C1 1.542(13) 10_556
N2 C2 1.531(14) .
N2 C2 1.531(14) 12
N3 C4 1.498(14) 10_556
N3 C4 1.498(14) .
C1 C2 1.52(2) .
C2 C2 1.22(2) 12
C2 C3 1.54(2) .
C4 C4 0.71(2) 10_556
C4 C4 1.28(3) 12
C4 C4 1.47(2) 3
C4 C5 1.494(14) .
C5 C4 1.494(14) 10_556
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
S2 In S1 In 0.0 . 10_556
S3 In S1 In 123.25(3) 9_656 10_556
S3 In S1 In -123.25(3) . 10_556
In In S1 In 180.0 9_656 10_556
S3 In S2 In -122.94(3) 9_656 10_556
S3 In S2 In 122.94(3) . 10_556
S1 In S2 In 0.0 . 10_556
In In S2 In 180.0 9_656 10_556
S2 In S3 In 124.93(5) . 9_656
S3 In S3 In 0.0 9_656 9_656
S1 In S3 In -124.25(4) . 9_656
In In S3 In -179.837(19) 10_556 9_656
N1 Ni1 N1 C1 92.0(7) 3 .
N2 Ni1 N1 C1 4.5(7) . .
N2 Ni1 N1 C1 179.5(8) 10_556 .
N1 Ni1 N1 C1 -92.0(7) 3 10_556
N2 Ni1 N1 C1 -179.5(8) . 10_556
N2 Ni1 N1 C1 -4.5(7) 10_556 10_556
N3 Ni1 N2 C2 -163.2(5) 3 .
N3 Ni1 N2 C2 115.0(6) . .
N1 Ni1 N2 C2 23.0(6) . .
N1 Ni1 N2 C2 -71.2(5) 3 .
N3 Ni1 N2 C2 -115.0(6) 3 12
N3 Ni1 N2 C2 163.2(5) . 12
N1 Ni1 N2 C2 71.2(5) . 12
N1 Ni1 N2 C2 -23.0(6) 3 12
N3 Ni1 N3 C4 -14.5(4) 3 10_556
N1 Ni1 N3 C4 165.5(4) . 10_556
N2 Ni1 N3 C4 77.8(5) . 10_556
N2 Ni1 N3 C4 -106.8(5) 10_556 10_556
N3 Ni1 N3 C4 14.5(4) 3 .
N1 Ni1 N3 C4 -165.5(4) . .
N2 Ni1 N3 C4 106.8(5) . .
N2 Ni1 N3 C4 -77.8(5) 10_556 .
C1 N1 C1 C2 155(2) 10_556 .
Ni1 N1 C1 C2 -34.3(13) . .
N1 C1 C2 C2 -16(2) . 12
N1 C1 C2 N2 57.2(14) . .
N1 C1 C2 C3 -178.9(11) . .
Ni1 N2 C2 C2 95.7(3) . 12
C2 N2 C2 C1 -141.2(8) 12 .
Ni1 N2 C2 C1 -45.5(9) . .
C2 N2 C2 C3 96.7(11) 12 .
Ni1 N2 C2 C3 -167.5(10) . .
C2 C2 C3 C3 0.000(3) 12 12
C1 C2 C3 C3 169.7(11) . 12
N2 C2 C3 C3 -70.5(8) . 12
Ni1 N3 C4 C4 -94.7(2) . 10_556
C4 N3 C4 C4 82.1(3) 10_556 12
Ni1 N3 C4 C4 -12.6(4) . 12
C4 N3 C4 C4 52.6(11) 10_556 3
Ni1 N3 C4 C4 -42.0(11) . 3
C4 N3 C4 C5 -64.1(9) 10_556 .
Ni1 N3 C4 C5 -158.8(7) . .
C4 C4 C5 C4 -84.5(3) 12 10_556
C4 C4 C5 C4 -55.8(11) 3 10_556
N3 C4 C5 C4 64.1(9) . 10_556
