#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:46:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179077 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/39/4303970.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_4303970
loop_
_publ_author_name
'Mitsushiro Nomura'
'Marc Fourmigué'
_publ_section_title
;
Dinuclear Cp* Cobalt Complexes of the 1,2,4,5-Benzenetetrathiolate
Bischelating Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1301
_journal_page_last               1312
_journal_paper_doi               10.1021/ic700778b
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C26 H32 Co2 S4'
_chemical_formula_weight         590.62
_chemical_name_common            Cp*Co(btt)CoCp*
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 112.959(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4903(6)
_cell_length_b                   13.3205(7)
_cell_length_c                   15.9026(7)
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.00
_cell_volume                     2631.3(2)
_computing_data_collection       'Bruker SMART (BRUKER 1996)'
_computing_data_reduction        'Bruker SAINTPLUS V6.02 (BRUKER 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0886
_diffrn_reflns_av_sigmaI/netI    0.1219
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28293
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.591
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0927P)²+0.2601P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1778
_reflns_number_gt                3407
_reflns_number_total             6038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700778b-file003.cif
_cod_data_source_block           mnii422_0m
_cod_database_code               4303970
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Co1 Co 0.72587(5) 0.82066(5) 0.23865(4) 0.0128(2) Uani 1 1 d . . .
Co2 Co 0.27513(5) 1.25210(5) 0.25359(4) 0.0130(2) Uani 1 1 d . . .
S1 S 0.69658(9) 0.89329(10) 0.34629(8) 0.0154(3) Uani 1 1 d . . .
S2 S 0.59877(9) 0.89959(10) 0.13523(8) 0.0142(3) Uani 1 1 d . . .
S3 S 0.30243(9) 1.17861(10) 0.14549(8) 0.0146(3) Uani 1 1 d . . .
S4 S 0.40098(9) 1.17111(10) 0.35562(8) 0.0154(3) Uani 1 1 d . . .
C1 C 0.5863(3) 0.9720(4) 0.2907(3) 0.0123(10) Uani 1 1 d . . .
C2 C 0.5418(3) 0.9756(4) 0.1944(3) 0.0118(10) Uani 1 1 d . . .
C3 C 0.4541(3) 1.0380(4) 0.1502(3) 0.0129(11) Uani 1 1 d . . .
H3 H 0.4237 1.0397 0.0867 0.016 Uiso 1 1 calc R . .
C4 C 0.4112(3) 1.0976(4) 0.1991(3) 0.0119(11) Uani 1 1 d . . .
C5 C 0.4564(3) 1.0944(4) 0.2961(3) 0.0111(10) Uani 1 1 d . . .
C6 C 0.5436(3) 1.0313(4) 0.3405(3) 0.0152(11) Uani 1 1 d . . .
H6 H 0.5735 1.0288 0.4039 0.018 Uiso 1 1 calc R . .
C7 C 0.7512(4) 0.7077(4) 0.1618(3) 0.0175(11) Uani 1 1 d . . .
C8 C 0.7538(4) 0.6714(4) 0.2477(3) 0.0171(12) Uani 1 1 d . . .
C9 C 0.8397(4) 0.7207(4) 0.3198(3) 0.0149(11) Uani 1 1 d . . .
C10 C 0.8868(4) 0.7916(4) 0.2787(3) 0.0165(11) Uani 1 1 d . . .
C11 C 0.8322(4) 0.7827(4) 0.1801(3) 0.0148(11) Uani 1 1 d . . .
C12 C 0.1783(4) 1.3672(4) 0.1803(3) 0.0190(12) Uani 1 1 d . . .
C13 C 0.2571(4) 1.4022(4) 0.2646(3) 0.0169(11) Uani 1 1 d . . .
C14 C 0.2422(4) 1.3519(4) 0.3378(3) 0.0156(11) Uani 1 1 d . . .
C15 C 0.1548(4) 1.2816(4) 0.2984(3) 0.0203(12) Uani 1 1 d . . .
C16 C 0.1154(4) 1.2926(4) 0.2010(3) 0.0186(12) Uani 1 1 d . . .
C17 C 0.6777(4) 0.6698(4) 0.0704(3) 0.0230(13) Uani 1 1 d . . .
H17A H 0.6314 0.6191 0.0780 0.034 Uiso 1 1 calc R . .
H17B H 0.7196 0.6418 0.0393 0.034 Uiso 1 1 calc R . .
H17C H 0.6349 0.7243 0.0351 0.034 Uiso 1 1 calc R . .
C18 C 0.6813(4) 0.5942(4) 0.2595(3) 0.0205(12) Uani 1 1 d . . .
H18A H 0.6315 0.5724 0.2007 0.031 Uiso 1 1 calc R . .
H18B H 0.6424 0.6222 0.2932 0.031 Uiso 1 1 calc R . .
H18C H 0.7232 0.5380 0.2924 0.031 Uiso 1 1 calc R . .
C19 C 0.8732(4) 0.7038(4) 0.4193(3) 0.0257(13) Uani 1 1 d . . .
H19A H 0.8293 0.6523 0.4293 0.038 Uiso 1 1 calc R . .
H19B H 0.8647 0.7649 0.4479 0.038 Uiso 1 1 calc R . .
H19C H 0.9473 0.6835 0.4452 0.038 Uiso 1 1 calc R . .
C20 C 0.9772(4) 0.8626(4) 0.3282(3) 0.0230(12) Uani 1 1 d . . .
H20A H 0.9931 0.9023 0.2846 0.035 Uiso 1 1 calc R . .
H20B H 1.0399 0.8250 0.3648 0.035 Uiso 1 1 calc R . .
H20C H 0.9564 0.9059 0.3667 0.035 Uiso 1 1 calc R . .
C21 C 0.8594(4) 0.8416(4) 0.1137(3) 0.0257(13) Uani 1 1 d . . .
H21A H 0.9176 0.8865 0.1457 0.039 Uiso 1 1 calc R . .
H21B H 0.7976 0.8797 0.0759 0.039 Uiso 1 1 calc R . .
H21C H 0.8806 0.7971 0.0763 0.039 Uiso 1 1 calc R . .
C22 C 0.1624(5) 1.4029(4) 0.0871(3) 0.0313(14) Uani 1 1 d . . .
H22A H 0.2147 1.4537 0.0916 0.047 Uiso 1 1 calc R . .
H22B H 0.0913 1.4304 0.0578 0.047 Uiso 1 1 calc R . .
H22C H 0.1708 1.3476 0.0517 0.047 Uiso 1 1 calc R . .
C23 C 0.3410(4) 1.4812(4) 0.2742(4) 0.0273(13) Uani 1 1 d . . .
H23A H 0.3342 1.5032 0.2148 0.041 Uiso 1 1 calc R . .
H23B H 0.4114 1.4534 0.3062 0.041 Uiso 1 1 calc R . .
H23C H 0.3307 1.5372 0.3079 0.041 Uiso 1 1 calc R . .
C24 C 0.3039(4) 1.3693(5) 0.4380(3) 0.0263(13) Uani 1 1 d . . .
H24A H 0.2775 1.3252 0.4723 0.039 Uiso 1 1 calc R . .
H24B H 0.2947 1.4377 0.4525 0.039 Uiso 1 1 calc R . .
H24C H 0.3789 1.3563 0.4532 0.039 Uiso 1 1 calc R . .
C25 C 0.1121(4) 1.2128(4) 0.3493(4) 0.0281(13) Uani 1 1 d . . .
H25A H 0.0539 1.1743 0.3069 0.042 Uiso 1 1 calc R . .
H25B H 0.0865 1.2512 0.3878 0.042 Uiso 1 1 calc R . .
H25C H 0.1683 1.1684 0.3861 0.042 Uiso 1 1 calc R . .
C26 C 0.0238(4) 1.2345(5) 0.1339(4) 0.0295(14) Uani 1 1 d . . .
H26A H -0.0041 1.1890 0.1662 0.044 Uiso 1 1 calc R . .
H26B H 0.0485 1.1972 0.0943 0.044 Uiso 1 1 calc R . .
H26C H -0.0320 1.2800 0.0984 0.044 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'
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
C8 Co1 C10 69.3(2) . . ?
C8 Co1 C7 41.4(2) . . ?
C10 Co1 C7 69.12(19) . . ?
C8 Co1 C11 69.3(2) . . ?
C10 Co1 C11 41.53(19) . . ?
C7 Co1 C11 40.6(2) . . ?
C8 Co1 C9 41.08(19) . . ?
C10 Co1 C9 40.8(2) . . ?
C7 Co1 C9 69.04(19) . . ?
C11 Co1 C9 69.10(19) . . ?
C8 Co1 S1 118.50(14) . . ?
C10 Co1 S1 109.99(14) . . ?
C7 Co1 S1 159.66(15) . . ?
C11 Co1 S1 148.85(14) . . ?
C9 Co1 S1 96.69(14) . . ?
C8 Co1 S2 127.75(14) . . ?
C10 Co1 S2 140.28(15) . . ?
C7 Co1 S2 99.96(14) . . ?
C11 Co1 S2 105.39(14) . . ?
C9 Co1 S2 168.34(14) . . ?
S1 Co1 S2 92.89(5) . . ?
C13 Co2 C15 69.1(2) . . ?
C13 Co2 C14 40.8(2) . . ?
C15 Co2 C14 41.2(2) . . ?
C13 Co2 C12 40.8(2) . . ?
C15 Co2 C12 68.9(2) . . ?
C14 Co2 C12 68.64(19) . . ?
C13 Co2 C16 68.6(2) . . ?
C15 Co2 C16 40.9(2) . . ?
C14 Co2 C16 68.68(19) . . ?
C12 Co2 C16 40.6(2) . . ?
C13 Co2 S4 121.35(14) . . ?
C15 Co2 S4 109.67(15) . . ?
C14 Co2 S4 98.18(14) . . ?
C12 Co2 S4 162.10(15) . . ?
C16 Co2 S4 147.25(16) . . ?
C13 Co2 S3 125.87(15) . . ?
C15 Co2 S3 141.07(15) . . ?
C14 Co2 S3 166.43(14) . . ?
C12 Co2 S3 99.02(14) . . ?
C16 Co2 S3 106.00(14) . . ?
S4 Co2 S3 92.56(5) . . ?
C1 S1 Co1 104.66(16) . . ?
C2 S2 Co1 105.07(16) . . ?
C4 S3 Co2 105.44(16) . . ?
C5 S4 Co2 105.43(16) . . ?
C6 C1 C2 120.2(4) . . ?
C6 C1 S1 120.7(4) . . ?
C2 C1 S1 119.1(3) . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 S2 122.6(3) . . ?
C1 C2 S2 118.3(3) . . ?
C4 C3 C2 121.2(4) . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 S3 122.3(3) . . ?
C5 C4 S3 118.0(3) . . ?
C6 C5 C4 119.2(4) . . ?
C6 C5 S4 122.2(3) . . ?
C4 C5 S4 118.5(3) . . ?
C1 C6 C5 120.6(4) . . ?
C11 C7 C8 108.0(4) . . ?
C11 C7 C17 127.0(5) . . ?
C8 C7 C17 125.0(5) . . ?
C11 C7 Co1 69.9(3) . . ?
C8 C7 Co1 68.1(3) . . ?
C17 C7 Co1 128.8(3) . . ?
C9 C8 C7 108.6(4) . . ?
C9 C8 C18 125.8(4) . . ?
C7 C8 C18 125.6(4) . . ?
C9 C8 Co1 71.1(3) . . ?
C7 C8 Co1 70.5(3) . . ?
C18 C8 Co1 125.4(4) . . ?
C10 C9 C8 107.6(4) . . ?
C10 C9 C19 125.6(5) . . ?
C8 C9 C19 126.8(5) . . ?
C10 C9 Co1 69.1(3) . . ?
C8 C9 Co1 67.8(3) . . ?
C19 C9 Co1 127.4(3) . . ?
C9 C10 C11 108.0(4) . . ?
C9 C10 C20 126.3(4) . . ?
C11 C10 C20 125.7(5) . . ?
C9 C10 Co1 70.2(3) . . ?
C11 C10 Co1 69.5(3) . . ?
C20 C10 Co1 126.2(4) . . ?
C7 C11 C10 107.7(4) . . ?
C7 C11 C21 127.8(4) . . ?
C10 C11 C21 124.5(5) . . ?
C7 C11 Co1 69.5(3) . . ?
C10 C11 Co1 68.9(3) . . ?
C21 C11 Co1 127.3(4) . . ?
C16 C12 C13 107.7(4) . . ?
C16 C12 C22 125.7(5) . . ?
C13 C12 C22 126.6(5) . . ?
C16 C12 Co2 69.7(3) . . ?
C13 C12 Co2 68.6(3) . . ?
C22 C12 Co2 127.9(4) . . ?
C14 C13 C12 108.8(4) . . ?
C14 C13 C23 125.8(4) . . ?
C12 C13 C23 125.4(5) . . ?
C14 C13 Co2 70.5(3) . . ?
C12 C13 Co2 70.5(3) . . ?
C23 C13 Co2 125.8(3) . . ?
C13 C14 C15 107.7(4) . . ?
C13 C14 C24 126.7(5) . . ?
C15 C14 C24 125.6(5) . . ?
C13 C14 Co2 68.7(3) . . ?
C15 C14 Co2 69.2(3) . . ?
C24 C14 Co2 128.4(3) . . ?
C16 C15 C14 107.3(4) . . ?
C16 C15 C25 126.5(5) . . ?
C14 C15 C25 126.2(5) . . ?
C16 C15 Co2 69.8(3) . . ?
C14 C15 Co2 69.6(3) . . ?
C25 C15 Co2 127.0(4) . . ?
C12 C16 C15 108.5(4) . . ?
C12 C16 C26 126.7(5) . . ?
C15 C16 C26 124.8(5) . . ?
C12 C16 Co2 69.7(3) . . ?
C15 C16 Co2 69.3(3) . . ?
C26 C16 Co2 126.7(4) . . ?
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
Co1 C8 2.018(5) . ?
Co1 C10 2.047(4) . ?
Co1 C7 2.049(5) . ?
Co1 C11 2.055(5) . ?
Co1 C9 2.062(5) . ?
Co1 S1 2.1330(13) . ?
Co1 S2 2.1331(13) . ?
Co2 C13 2.030(5) . ?
Co2 C15 2.050(5) . ?
Co2 C14 2.054(5) . ?
Co2 C12 2.055(5) . ?
Co2 C16 2.056(5) . ?
Co2 S4 2.1284(13) . ?
Co2 S3 2.1313(13) . ?
S1 C1 1.752(5) . ?
S2 C2 1.751(5) . ?
S3 C4 1.752(5) . ?
S4 C5 1.747(5) . ?
C1 C6 1.393(7) . ?
C1 C2 1.411(6) . ?
C2 C3 1.392(6) . ?
C3 C4 1.386(7) . ?
C4 C5 1.421(6) . ?
C5 C6 1.393(7) . ?
C7 C11 1.424(7) . ?
C7 C8 1.437(7) . ?
C7 C17 1.492(7) . ?
C8 C9 1.432(7) . ?
C8 C18 1.480(7) . ?
C9 C10 1.431(7) . ?
C9 C19 1.484(7) . ?
C10 C11 1.454(7) . ?
C10 C20 1.500(7) . ?
C11 C21 1.472(7) . ?
C12 C16 1.425(8) . ?
C12 C13 1.426(7) . ?
C12 C22 1.491(7) . ?
C13 C14 1.424(7) . ?
C13 C23 1.508(7) . ?
C14 C15 1.443(7) . ?
C14 C24 1.501(7) . ?
C15 C16 1.436(7) . ?
C15 C25 1.479(8) . ?
C16 C26 1.496(7) . ?
