#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:32:08 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179065 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/27/4302714.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_4302714
loop_
_publ_author_name
'Minoru Mitsumi'
'Yuji Yoshida'
'Akihisa Kohyama'
'Yasutaka Kitagawa'
'Yoshiki Ozawa'
'Mototada Kobayashi'
'Koshiro Toriumi'
'Makoto Tadokoro'
'Naoshi Ikeda'
'Mitsutaka Okumura'
'Mohamedally Kurmoo'
_publ_contact_author_address
; 
Department of Material Science
Graduate School of Material Science
University of Hyogo
3-2-1 Kouto, Kamigori-cho, Ako-gun, Hyogo 678-1297, Japan 
;
_publ_contact_author_email       mitsumi@sci.u-hyogo.ac.jp
_publ_contact_author_fax         +81-791-58-0154
_publ_contact_author_name        'Mitsumi, Minoru'
_publ_contact_author_phone       +81-791-58-0153
_publ_section_title
;
Syntheses, Structures and Solid-State Properties of MMX Mixed-Valence
Chains, [NiII/III2(RCS2)4I]∞ (R = Et,n-Pr andn-Bu): Evidence of a
Spin-Peierls Transition
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6680
_journal_page_last               6691
_journal_paper_doi               10.1021/ic900630a
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C12 H20 I Ni2 S8'
_chemical_formula_sum            'C12 H20 I Ni2 S8'
_chemical_formula_weight         665.11
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 114.459(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.274(3)
_cell_length_b                   8.3751(14)
_cell_length_c                   16.745(3)
_cell_measurement_reflns_used    4370
_cell_measurement_temperature    292(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     2205.1(7)
_computing_cell_refinement       'CRYSTAL CLEAR 1.3 (Rigaku, 2000)'
_computing_data_collection       'CRYSTAL CLEAR 1.3 (Rigaku, 2000)'
_computing_data_reduction        'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (A. Altomare, 1999)'
_diffrn_ambient_temperature      292(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9977
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    3.859
_exptl_absorpt_correction_T_max  0.6762
_exptl_absorpt_correction_T_min  0.6338
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         2455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0276
_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)+(0.0210P)²+2.4239P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                2264
_reflns_number_total             2455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900630a_si_001.cif
_cod_data_source_block           '[Pt2(EtCS2)4I]_292K'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4302714
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.0000 -0.27790(3) 0.2500 0.03535(9) Uani 1 2 d S . .
Ni1 Ni 0.0000 0.07058(5) 0.2500 0.02015(10) Uani 1 2 d S . .
Ni2 Ni 0.0000 0.37481(5) 0.2500 0.02095(10) Uani 1 2 d S . .
S1 S 0.12753(4) 0.05773(7) 0.36290(4) 0.02799(14) Uani 1 1 d . . .
S2 S 0.14112(4) 0.39100(7) 0.30709(4) 0.02901(14) Uani 1 1 d . . .
S3 S -0.06543(4) 0.05609(7) 0.33982(4) 0.02798(14) Uani 1 1 d . . .
S4 S 0.00357(4) 0.38492(7) 0.38482(4) 0.02888(14) Uani 1 1 d . . .
C1 C 0.18208(15) 0.2224(3) 0.36137(15) 0.0259(5) Uani 1 1 d . . .
C2 C 0.27785(16) 0.2151(3) 0.40971(18) 0.0368(6) Uani 1 1 d . . .
H2A H 0.2934 0.1342 0.4552 0.044 Uiso 1 1 calc R . .
H2B H 0.2992 0.3171 0.4376 0.044 Uiso 1 1 calc R . .
C3 C 0.31774(19) 0.1757(4) 0.3468(2) 0.0533(8) Uani 1 1 d . . .
H3A H 0.2955 0.0760 0.3182 0.080 Uiso 1 1 calc R . .
H3B H 0.3783 0.1673 0.3788 0.080 Uiso 1 1 calc R . .
H3C H 0.3047 0.2587 0.3037 0.080 Uiso 1 1 calc R . .
C4 C -0.04401(15) 0.2215(3) 0.40111(15) 0.0265(5) Uani 1 1 d . . .
C5 C -0.07084(19) 0.2248(4) 0.47622(18) 0.0414(7) Uani 1 1 d . . .
H5A H -0.0528 0.1264 0.5094 0.050 Uiso 1 1 calc R . .
H5B H -0.0421 0.3124 0.5151 0.050 Uiso 1 1 calc R . .
C6 C -0.1642(2) 0.2435(5) 0.4473(3) 0.0751(12) Uani 1 1 d . . .
H6A H -0.1832 0.3371 0.4113 0.113 Uiso 1 1 calc R . .
H6B H -0.1767 0.2542 0.4978 0.113 Uiso 1 1 calc R . .
H6C H -0.1928 0.1513 0.4142 0.113 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'
I I -0.4742 1.8119 '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'
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
Ni2 I1 Ni1 180.0 1_545 . ?
S3 Ni1 S3 173.75(4) 2 . ?
S3 Ni1 S1 91.39(3) 2 2 ?
S3 Ni1 S1 88.31(3) . 2 ?
S3 Ni1 S1 88.31(3) 2 . ?
S3 Ni1 S1 91.39(3) . . ?
S1 Ni1 S1 174.48(4) 2 . ?
S3 Ni1 Ni2 93.124(18) 2 . ?
S3 Ni1 Ni2 93.124(18) . . ?
S1 Ni1 Ni2 92.761(18) 2 . ?
S1 Ni1 Ni2 92.761(18) . . ?
S3 Ni1 I1 86.876(18) 2 . ?
S3 Ni1 I1 86.876(18) . . ?
S1 Ni1 I1 87.239(18) 2 . ?
S1 Ni1 I1 87.239(18) . . ?
Ni2 Ni1 I1 180.0 . . ?
S2 Ni2 S2 173.01(4) . 2 ?
S2 Ni2 S4 89.93(2) . 2 ?
S2 Ni2 S4 89.80(2) 2 2 ?
S2 Ni2 S4 89.80(2) . . ?
S2 Ni2 S4 89.93(2) 2 . ?
S4 Ni2 S4 175.66(4) 2 . ?
S2 Ni2 Ni1 93.495(18) . . ?
S2 Ni2 Ni1 93.494(18) 2 . ?
S4 Ni2 Ni1 92.172(18) 2 . ?
S4 Ni2 Ni1 92.171(18) . . ?
S2 Ni2 I1 86.504(18) . 1_565 ?
S2 Ni2 I1 86.506(18) 2 1_565 ?
S4 Ni2 I1 87.828(18) 2 1_565 ?
S4 Ni2 I1 87.829(18) . 1_565 ?
Ni1 Ni2 I1 180.0 . 1_565 ?
C1 S1 Ni1 108.12(8) . . ?
C1 S2 Ni2 108.94(9) . . ?
C4 S3 Ni1 108.91(9) . . ?
C4 S4 Ni2 108.86(8) . . ?
C2 C1 S2 116.66(19) . . ?
C2 C1 S1 117.12(18) . . ?
S2 C1 S1 126.14(14) . . ?
C1 C2 C3 110.4(2) . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
C3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 S3 117.40(19) . . ?
C5 C4 S4 117.44(19) . . ?
S3 C4 S4 125.15(14) . . ?
C6 C5 C4 113.3(3) . . ?
C6 C5 H5A 108.9 . . ?
C4 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
C4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
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
I1 Ni2 2.9085(6) 1_545 ?
I1 Ni1 2.9186(6) . ?
Ni1 S3 2.2276(7) 2 ?
Ni1 S3 2.2276(7) . ?
Ni1 S1 2.2338(7) 2 ?
Ni1 S1 2.2339(7) . ?
Ni1 Ni2 2.5479(7) . ?
Ni2 S2 2.2237(7) . ?
Ni2 S2 2.2238(7) 2 ?
Ni2 S4 2.2343(7) 2 ?
Ni2 S4 2.2343(7) . ?
Ni2 I1 2.9085(6) 1_565 ?
S1 C1 1.676(2) . ?
S2 C1 1.670(2) . ?
S3 C4 1.672(2) . ?
S4 C4 1.676(2) . ?
C1 C2 1.512(3) . ?
C2 C3 1.514(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 C5 1.510(3) . ?
C5 C6 1.487(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S3 Ni1 Ni2 S2 -61.07(3) 2 . . . ?
S3 Ni1 Ni2 S2 118.93(3) . . . . ?
S1 Ni1 Ni2 S2 -152.62(2) 2 . . . ?
S1 Ni1 Ni2 S2 27.38(2) . . . . ?
S3 Ni1 Ni2 S2 118.93(3) 2 . . 2 ?
S3 Ni1 Ni2 S2 -61.07(3) . . . 2 ?
S1 Ni1 Ni2 S2 27.38(2) 2 . . 2 ?
S1 Ni1 Ni2 S2 -152.62(2) . . . 2 ?
S3 Ni1 Ni2 S4 28.99(2) 2 . . 2 ?
S3 Ni1 Ni2 S4 -151.01(2) . . . 2 ?
S1 Ni1 Ni2 S4 -62.55(3) 2 . . 2 ?
S1 Ni1 Ni2 S4 117.45(3) . . . 2 ?
S3 Ni1 Ni2 S4 -151.01(2) 2 . . . ?
S3 Ni1 Ni2 S4 28.99(2) . . . . ?
S1 Ni1 Ni2 S4 117.44(3) 2 . . . ?
S1 Ni1 Ni2 S4 -62.55(3) . . . . ?
S3 Ni1 S1 C1 64.97(9) 2 . . . ?
S3 Ni1 S1 C1 -121.28(9) . . . . ?
Ni2 Ni1 S1 C1 -28.08(9) . . . . ?
I1 Ni1 S1 C1 151.92(9) . . . . ?
S4 Ni2 S2 C1 -115.72(9) 2 . . . ?
S4 Ni2 S2 C1 68.62(9) . . . . ?
Ni1 Ni2 S2 C1 -23.55(9) . . . . ?
I1 Ni2 S2 C1 156.45(9) 1_565 . . . ?
S1 Ni1 S3 C4 -119.05(9) 2 . . . ?
S1 Ni1 S3 C4 66.47(9) . . . . ?
Ni2 Ni1 S3 C4 -26.37(9) . . . . ?
I1 Ni1 S3 C4 153.63(9) . . . . ?
S2 Ni2 S4 C4 -122.25(9) . . . . ?
S2 Ni2 S4 C4 64.73(9) 2 . . . ?
Ni1 Ni2 S4 C4 -28.76(9) . . . . ?
I1 Ni2 S4 C4 151.24(9) 1_565 . . . ?
Ni2 S2 C1 C2 -176.34(16) . . . . ?
Ni2 S2 C1 S1 7.06(18) . . . . ?
Ni1 S1 C1 C2 -159.08(16) . . . . ?
Ni1 S1 C1 S2 17.51(18) . . . . ?
S2 C1 C2 C3 -80.5(3) . . . . ?
S1 C1 C2 C3 96.4(3) . . . . ?
Ni1 S3 C4 C5 -170.66(17) . . . . ?
Ni1 S3 C4 S4 10.32(19) . . . . ?
Ni2 S4 C4 C5 -163.14(18) . . . . ?
Ni2 S4 C4 S3 15.88(18) . . . . ?
S3 C4 C5 C6 -73.7(3) . . . . ?
S4 C4 C5 C6 105.4(3) . . . . ?
