#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/82/4328285.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_4328285
loop_
_publ_author_name
'Satoru Tsukada'
'Yusuke Shibata'
'Ryota Sakamoto'
'Tetsuya Kambe'
'Tomoji Ozeki'
'Hiroshi Nishihara'
_publ_section_title
;
 Ir3Co6 and Co3Fe3 Dithiolene Cluster Complexes: Multiple Metal-Metal Bond
 Formation and Correlation between Structure and Internuclear Electronic
 Communication
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1228
_journal_page_last               1230
_journal_paper_doi               10.1021/ic202548g
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration syn
_chemical_formula_sum            'C5 H2.5 Co0.5 Fe0.5 O1.5 S'
_chemical_formula_weight         176.02
_space_group_IT_number           188
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c 2'
_symmetry_space_group_name_H-M   'P -6 c 2'
_audit_creation_date             2009-01-15T18:23:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                120.000(5)
_cell_formula_units_Z            12
_cell_length_a                   12.137(5)
_cell_length_b                   12.137(5)
_cell_length_c                   13.995(5)
_cell_measurement_reflns_used    6136
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      31.0024
_cell_measurement_theta_min      1.4550
_cell_volume                     1785.4(12)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
        ????
;
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device
;
        Saturn724 (4x4 bin mode)
;
_diffrn_measurement_method       dtintegrate.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14731
_diffrn_reflns_theta_full        31.01
_diffrn_reflns_theta_max         31.01
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    2.951
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6808
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_description       Block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.455
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(11)
_refine_ls_extinction_coef       0.008(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   1.188
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1900
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_gt           0.0824
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1185P)²+2.1602P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2547
_reflns_number_gt                1628
_reflns_number_total             1900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202548g_si_002_1.cif
_cod_data_source_block           6
_cod_original_formula_sum        'C5 H2.50 Co0.50 Fe0.50 O1.50 S'
_cod_database_code               4328285
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, y, -z+1/2'
'-y, -x, -z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'-x+y, y, -z'
'x, x-y, -z'
'x, x-y, z+1/2'
'-y, x-y, z'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'-x+y, -x, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
C1 C 0.5337(6) 0.2744(8) 0.25 0.0529(11) Uani 1 d SD . .
C2 C 0.5958(7) 0.2001(6) 0.25 0.0529(11) Uani 1 d SD . A
S1 S 0.3641(2) 0.1720(2) 0.25 0.0762(12) Uani 1 d SD . .
S2 S 0.5042(2) 0.0305(2) 0.25 0.0626(8) Uani 1 d SD . .
Co1 Co 0.3379(8) 0.0051(8) 0.1551(17) 0.088(3) Uani 0.477(10) d PD 1 A
C3 C 0.3492(16) -0.0965(14) 0.0544(12) 0.088(4) Uani 0.477(10) d PDU 1 A
H3 H 0.4178 -0.1026 0.0312 0.105 Uiso 0.477(10) calc PR 1 A
C4 C 0.2548(12) -0.1749(19) 0.1206(13) 0.087(4) Uani 0.477(10) d PDU 1 A
H4 H 0.2544 -0.2449 0.1482 0.105 Uiso 0.477(10) calc PR 1 A
C5 C 0.1615(13) -0.1429(13) 0.1430(13) 0.082(4) Uani 0.477(10) d PDU 1 A
H5 H 0.0923 -0.1824 0.1842 0.099 Uiso 0.477(10) calc PR 1 A
C6 C 0.2023(15) -0.0341(15) 0.0854(14) 0.088(4) Uani 0.477(10) d PDU 1 A
H6 H 0.1618 0.0136 0.0826 0.105 Uiso 0.477(10) calc PR 1 A
C7 C 0.3121(14) -0.0065(14) 0.0327(14) 0.090(4) Uani 0.477(10) d PDU 1 A
H7 H 0.3536 0.0609 -0.0099 0.108 Uiso 0.477(10) calc PR 1 A
Fe1 Fe 0.3335(7) 0.0001(7) 0.1749(17) 0.089(3) Uani 0.523(10) d PD 2 .
C8 C 0.401(3) 0.079(3) 0.0366(16) 0.125(6) Uani 0.523(10) d PU 2 .
O8 O 0.4543(18) 0.1116(19) -0.0340(9) 0.138(6) Uani 0.523(10) d PU 2 .
C9 C 0.162(2) -0.051(3) 0.127(2) 0.131(8) Uani 0.523(10) d PU 2 .
O9 O 0.0637(14) -0.081(2) 0.1096(19) 0.147(7) Uani 0.523(10) d PU 2 .
C10 C 0.297(2) -0.160(2) 0.141(4) 0.201(13) Uani 0.523(10) d PU 2 .
O10 O 0.2693(19) -0.2576(17) 0.138(3) 0.219(13) Uani 0.523(10) d PU 2 .
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Fe Fe 0.3463 0.8444 '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'
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
C2 C1 C2 120.0(7) 11_665 .
C2 C1 S1 129.7(7) 11_665 .
C2 C1 S1 110.2(6) . .
C1 C2 C1 120.0(7) 9_655 .
C1 C2 S2 119.7(7) 9_655 .
C1 C2 S2 120.3(6) . .
C1 S1 Fe1 104.4(3) . .
C1 S1 Fe1 104.4(3) . 2
Fe1 S1 Fe1 57.2(11) . 2
C2 S2 Fe1 100.7(3) . .
C2 S2 Fe1 100.7(3) . 2
Fe1 S2 Fe1 57.6(11) . 2
C7 C3 C4 101.4(15) . .
C7 C3 H3 129.3 . .
C4 C3 H3 129.3 . .
C5 C4 C3 117.1(16) . .
C5 C4 H4 121.4 . .
C3 C4 H4 121.4 . .
C4 C5 C6 100.2(15) . .
C4 C5 H5 129.9 . .
C6 C5 H5 129.9 . .
C5 C6 C7 111.8(15) . .
C5 C6 H6 124.1 . .
C7 C6 H6 124.1 . .
C3 C7 C6 109.5(15) . .
C3 C7 H7 125.3 . .
C6 C7 H7 125.3 . .
C10 Fe1 C9 85.5(11) . .
C10 Fe1 Fe1 105.1(18) . 2
C9 Fe1 Fe1 109.7(12) . 2
C10 Fe1 C8 94(2) . .
C9 Fe1 C8 86.9(15) . .
Fe1 Fe1 C8 155.1(8) 2 .
C10 Fe1 S2 90.6(9) . .
C9 Fe1 S2 168.8(15) . .
Fe1 Fe1 S2 61.2(6) 2 .
C8 Fe1 S2 103.9(8) . .
C10 Fe1 S1 166(2) . .
C9 Fe1 S1 96.3(10) . .
Fe1 Fe1 S1 61.4(6) 2 .
C8 Fe1 S1 99.4(9) . .
S2 Fe1 S1 85.0(5) . .
O8 C8 Fe1 165.6(18) . .
O9 C9 Fe1 174(3) . .
O10 C10 Fe1 167(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.367(8) 11_665
C1 C2 1.435(7) .
C1 S1 1.795(6) .
C2 C1 1.367(8) 9_655
C2 S2 1.785(7) .
S1 Fe1 2.196(12) .
S1 Fe1 2.196(12) 2
S2 Fe1 2.184(11) .
S2 Fe1 2.184(11) 2
C3 C7 1.408(12) .
C3 C4 1.409(12) .
C3 H3 0.93 .
C4 C5 1.405(12) .
C4 H4 0.93 .
C5 C6 1.409(12) .
C5 H5 0.93 .
C6 C7 1.409(12) .
C6 H6 0.93 .
C7 H7 0.93 .
Fe1 C10 1.832(19) .
Fe1 C9 1.97(2) .
Fe1 Fe1 2.10(5) 2
Fe1 C8 2.13(3) .
C8 O8 1.14(2) .
C9 O9 1.08(3) .
C10 O10 1.05(3) .
