#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:34:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179117 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/79/4307970.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_4307970
loop_
_publ_author_name
'Rongmin Yu'
'Kuppuswamy Arumugam'
'Ashok Manepalli'
'Yvon Tran'
'Russell Schmehl'
'Heiko Jacobsen'
'James P. Donahue'
_publ_contact_author_email       donahue@tulane.edu
_publ_contact_author_fax         504-865-5596
_publ_contact_author_phone       504-862-3562
_publ_section_title
;
Reversible, Electrochemically Controlled Binding of Phosphine to Iron and
Cobalt Bis(dithiolene) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5131
_journal_page_last               5133
_journal_paper_doi               10.1021/ic0624569
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C68 H64 Cl4 Co2 O8 S8'
_chemical_formula_weight         1525.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.5560(10)
_cell_angle_beta                 90.3220(10)
_cell_angle_gamma                90.189(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6052(10)
_cell_length_b                   11.7254(12)
_cell_length_c                   15.3302(16)
_cell_measurement_reflns_used    7097
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.224
_cell_measurement_theta_min      2.413
_cell_volume                     1697.3(3)
_computing_cell_refinement       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_collection       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_reduction        'Bruker SAINT+ (Bruker-AXS, 2004)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX'
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15323
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         7887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0554
_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)+(0.0535P)²+1.1185P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                6380
_reflns_number_total             7887
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic0624569-file006_06.cif
_cod_data_source_block
'[Co(S2C2(C6H4-p-OCH3)2)2]2.2(ClCH2CH2Cl)_1b.2(ClCH2CH2Cl)'
_cod_database_code               4307970
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.08685(4) 0.06447(3) 0.06297(3) 0.01224(11) Uani 1 1 d . . .
Cl1 Cl 0.30325(10) -0.19659(9) 0.35759(8) 0.0416(3) Uani 1 1 d . . .
Cl2 Cl -0.02768(12) -0.14085(10) 0.41766(8) 0.0482(3) Uani 1 1 d . . .
S1 S 0.00472(8) 0.23552(6) 0.05850(5) 0.01391(16) Uani 1 1 d . . .
S2 S 0.14781(8) 0.12632(6) 0.19857(5) 0.01462(16) Uani 1 1 d . . .
S3 S 0.23675(8) -0.07482(7) 0.06835(5) 0.01488(16) Uani 1 1 d . . .
S4 S 0.11501(8) 0.03980(6) -0.07994(5) 0.01303(16) Uani 1 1 d . . .
O1 O -0.2406(2) 0.7492(2) 0.20427(15) 0.0234(5) Uani 1 1 d . . .
O2 O 0.2737(3) 0.5210(2) 0.55613(15) 0.0324(6) Uani 1 1 d . . .
O3 O 0.6930(2) -0.4728(2) -0.06764(18) 0.0298(6) Uani 1 1 d . . .
O4 O 0.4613(2) -0.1080(2) -0.45256(14) 0.0251(5) Uani 1 1 d . . .
C1 C 0.0260(3) 0.3156(3) 0.1620(2) 0.0138(6) Uani 1 1 d . . .
C2 C 0.0954(3) 0.2663(3) 0.2262(2) 0.0144(6) Uani 1 1 d . . .
C3 C 0.3031(3) -0.1095(3) -0.0372(2) 0.0153(6) Uani 1 1 d . . .
C4 C 0.2534(3) -0.0568(3) -0.1037(2) 0.0134(6) Uani 1 1 d . . .
C5 C -0.0347(3) 0.4336(3) 0.17899(19) 0.0147(6) Uani 1 1 d . . .
C6 C -0.1210(3) 0.4684(3) 0.2519(2) 0.0162(6) Uani 1 1 d . . .
H6 H -0.1312 0.4196 0.2946 0.019 Uiso 1 1 calc R . .
C7 C -0.1923(3) 0.5728(3) 0.2634(2) 0.0170(6) Uani 1 1 d . . .
H7 H -0.2522 0.5947 0.3127 0.020 Uiso 1 1 calc R . .
C8 C -0.1746(3) 0.6456(3) 0.2011(2) 0.0167(6) Uani 1 1 d . . .
C9 C -0.0827(3) 0.6140(3) 0.1310(2) 0.0180(7) Uani 1 1 d . . .
H9 H -0.0657 0.6657 0.0911 0.022 Uiso 1 1 calc R . .
C10 C -0.0164(3) 0.5086(3) 0.1189(2) 0.0164(6) Uani 1 1 d . . .
H10 H 0.0426 0.4865 0.0692 0.020 Uiso 1 1 calc R . .
C11 C -0.3529(4) 0.7757(3) 0.2648(2) 0.0276(8) Uani 1 1 d . . .
H11A H -0.4215 0.7126 0.2542 0.041 Uiso 1 1 calc R . .
H11B H -0.3970 0.8481 0.2560 0.041 Uiso 1 1 calc R . .
H11C H -0.3175 0.7848 0.3257 0.041 Uiso 1 1 calc R . .
C12 C 0.1395(3) 0.3342(3) 0.3132(2) 0.0157(6) Uani 1 1 d . . .
C13 C 0.0984(4) 0.3057(3) 0.3934(2) 0.0245(8) Uani 1 1 d . . .
H13 H 0.0394 0.2406 0.3936 0.029 Uiso 1 1 calc R . .
C14 C 0.1430(4) 0.3715(3) 0.4730(2) 0.0273(8) Uani 1 1 d . . .
H14 H 0.1124 0.3524 0.5274 0.033 Uiso 1 1 calc R . .
C15 C 0.2314(4) 0.4646(3) 0.4740(2) 0.0219(7) Uani 1 1 d . . .
C16 C 0.2726(4) 0.4946(3) 0.3954(2) 0.0279(8) Uani 1 1 d . . .
H16 H 0.3328 0.5591 0.3957 0.033 Uiso 1 1 calc R . .
C17 C 0.2256(4) 0.4299(3) 0.3158(2) 0.0273(8) Uani 1 1 d . . .
H17 H 0.2531 0.4516 0.2617 0.033 Uiso 1 1 calc R . .
C18 C 0.3564(5) 0.6232(3) 0.5604(3) 0.0420(11) Uani 1 1 d . . .
H18A H 0.4441 0.6034 0.5291 0.063 Uiso 1 1 calc R . .
H18B H 0.3760 0.6569 0.6226 0.063 Uiso 1 1 calc R . .
H18C H 0.3057 0.6796 0.5325 0.063 Uiso 1 1 calc R . .
C19 C 0.4076(3) -0.2040(3) -0.0491(2) 0.0149(6) Uani 1 1 d . . .
C20 C 0.3831(3) -0.3059(3) -0.1098(2) 0.0195(7) Uani 1 1 d . . .
H20 H 0.3022 -0.3125 -0.1463 0.023 Uiso 1 1 calc R . .
C21 C 0.4756(4) -0.3982(3) -0.1179(2) 0.0219(7) Uani 1 1 d . . .
H21 H 0.4568 -0.4678 -0.1587 0.026 Uiso 1 1 calc R . .
C22 C 0.5948(3) -0.3884(3) -0.0663(2) 0.0191(7) Uani 1 1 d . . .
C23 C 0.6222(3) -0.2853(3) -0.0065(2) 0.0192(7) Uani 1 1 d . . .
H23 H 0.7053 -0.2776 0.0280 0.023 Uiso 1 1 calc R . .
C24 C 0.5284(3) -0.1947(3) 0.0024(2) 0.0167(6) Uani 1 1 d . . .
H24 H 0.5466 -0.1255 0.0440 0.020 Uiso 1 1 calc R . .
C25 C 0.6573(4) -0.5870(3) -0.1126(3) 0.0285(8) Uani 1 1 d . . .
H25A H 0.5678 -0.6101 -0.0906 0.043 Uiso 1 1 calc R . .
H25B H 0.7296 -0.6415 -0.1014 0.043 Uiso 1 1 calc R . .
H25C H 0.6501 -0.5878 -0.1765 0.043 Uiso 1 1 calc R . .
C26 C 0.3105(3) -0.0711(3) -0.1943(2) 0.0140(6) Uani 1 1 d . . .
C27 C 0.2225(3) -0.0746(3) -0.2682(2) 0.0168(6) Uani 1 1 d . . .
H27 H 0.1246 -0.0695 -0.2598 0.020 Uiso 1 1 calc R . .
C28 C 0.2752(3) -0.0855(3) -0.3527(2) 0.0186(7) Uani 1 1 d . . .
H28 H 0.2139 -0.0866 -0.4017 0.022 Uiso 1 1 calc R . .
C29 C 0.4181(3) -0.0949(3) -0.3665(2) 0.0171(6) Uani 1 1 d . . .
C30 C 0.5078(3) -0.0913(3) -0.2946(2) 0.0183(7) Uani 1 1 d . . .
H30 H 0.6055 -0.0967 -0.3034 0.022 Uiso 1 1 calc R . .
C31 C 0.4532(3) -0.0796(3) -0.2095(2) 0.0171(6) Uani 1 1 d . . .
H31 H 0.5149 -0.0774 -0.1605 0.021 Uiso 1 1 calc R . .
C32 C 0.6064(4) -0.1228(4) -0.4684(2) 0.0325(9) Uani 1 1 d . . .
H32A H 0.6570 -0.0553 -0.4360 0.049 Uiso 1 1 calc R . .
H32B H 0.6243 -0.1303 -0.5320 0.049 Uiso 1 1 calc R . .
H32C H 0.6380 -0.1929 -0.4480 0.049 Uiso 1 1 calc R . .
C1S C 0.1548(4) -0.2151(4) 0.2854(3) 0.0373(10) Uani 1 1 d . . .
H1SA H 0.1845 -0.2101 0.2245 0.045 Uiso 1 1 calc R . .
H1SB H 0.1144 -0.2932 0.2840 0.045 Uiso 1 1 calc R . .
C2S C 0.0468(4) -0.1264(3) 0.3144(3) 0.0338(9) Uani 1 1 d . . .
H2SA H -0.0276 -0.1337 0.2687 0.041 Uiso 1 1 calc R . .
H2SB H 0.0888 -0.0482 0.3197 0.041 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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
S2 Co1 S1 88.73(3) . . ?
S2 Co1 S4 153.93(4) . . ?
S1 Co1 S4 88.23(3) . . ?
S2 Co1 S3 84.84(3) . . ?
S1 Co1 S3 160.28(4) . . ?
S4 Co1 S3 89.39(3) . . ?
S2 Co1 S4 101.77(3) . 2 ?
S1 Co1 S4 101.88(3) . 2 ?
S4 Co1 S4 104.19(3) . 2 ?
S3 Co1 S4 97.68(3) . 2 ?
S2 Co1 Co1 151.26(3) . 2 ?
S1 Co1 Co1 98.57(3) . 2 ?
S4 Co1 Co1 54.62(2) . 2 ?
S3 Co1 Co1 95.97(3) . 2 ?
S4 Co1 Co1 49.57(2) 2 2 ?
C1 S1 Co1 106.56(11) . . ?
C2 S2 Co1 107.52(11) . . ?
C3 S3 Co1 105.20(11) . . ?
C4 S4 Co1 105.77(10) . . ?
C4 S4 Co1 108.97(10) . 2 ?
Co1 S4 Co1 75.81(3) . 2 ?
C8 O1 C11 117.8(3) . . ?
C15 O2 C18 117.6(3) . . ?
C22 O3 C25 117.2(3) . . ?
C29 O4 C32 117.2(3) . . ?
C2 C1 C5 123.9(3) . . ?
C2 C1 S1 118.8(2) . . ?
C5 C1 S1 117.2(2) . . ?
C1 C2 C12 122.9(3) . . ?
C1 C2 S2 118.2(2) . . ?
C12 C2 S2 118.5(2) . . ?
C4 C3 C19 124.9(3) . . ?
C4 C3 S3 120.5(2) . . ?
C19 C3 S3 114.4(2) . . ?
C3 C4 C26 125.5(3) . . ?
C3 C4 S4 118.2(2) . . ?
C26 C4 S4 116.3(2) . . ?
C6 C5 C10 118.5(3) . . ?
C6 C5 C1 120.4(3) . . ?
C10 C5 C1 120.9(3) . . ?
C7 C6 C5 121.4(3) . . ?
C6 C7 C8 119.0(3) . . ?
O1 C8 C9 115.8(3) . . ?
O1 C8 C7 124.5(3) . . ?
C9 C8 C7 119.7(3) . . ?
C10 C9 C8 120.5(3) . . ?
C9 C10 C5 120.7(3) . . ?
C17 C12 C13 118.0(3) . . ?
C17 C12 C2 119.5(3) . . ?
C13 C12 C2 122.6(3) . . ?
C14 C13 C12 120.5(3) . . ?
C15 C14 C13 120.6(3) . . ?
O2 C15 C16 124.3(3) . . ?
O2 C15 C14 115.9(3) . . ?
C16 C15 C14 119.8(3) . . ?
C15 C16 C17 119.4(3) . . ?
C16 C17 C12 121.7(3) . . ?
C20 C19 C24 118.9(3) . . ?
C20 C19 C3 120.1(3) . . ?
C24 C19 C3 121.0(3) . . ?
C21 C20 C19 120.9(3) . . ?
C22 C21 C20 119.8(3) . . ?
O3 C22 C21 125.4(3) . . ?
O3 C22 C23 114.8(3) . . ?
C21 C22 C23 119.8(3) . . ?
C24 C23 C22 120.1(3) . . ?
C23 C24 C19 120.5(3) . . ?
C31 C26 C27 117.6(3) . . ?
C31 C26 C4 121.4(3) . . ?
C27 C26 C4 120.9(3) . . ?
C28 C27 C26 121.3(3) . . ?
C27 C28 C29 120.1(3) . . ?
O4 C29 C30 123.9(3) . . ?
O4 C29 C28 116.3(3) . . ?
C30 C29 C28 119.8(3) . . ?
C29 C30 C31 119.4(3) . . ?
C26 C31 C30 121.7(3) . . ?
C2S C1S Cl1 112.0(3) . . ?
C1S C2S Cl2 112.1(3) . . ?
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 S2 2.1498(9) . ?
Co1 S1 2.1701(9) . ?
Co1 S4 2.1751(8) . ?
Co1 S3 2.1934(8) . ?
Co1 S4 2.3299(9) 2 ?
Co1 Co1 2.7703(8) 2 ?
Cl1 C1S 1.788(4) . ?
Cl2 C2S 1.777(4) . ?
S1 C1 1.700(3) . ?
S2 C2 1.697(3) . ?
S3 C3 1.721(3) . ?
S4 C4 1.745(3) . ?
S4 Co1 2.3299(9) 2 ?
O1 C8 1.364(4) . ?
O1 C11 1.424(4) . ?
O2 C15 1.369(4) . ?
O2 C18 1.427(4) . ?
O3 C22 1.367(4) . ?
O3 C25 1.429(4) . ?
O4 C29 1.367(4) . ?
O4 C32 1.422(4) . ?
C1 C2 1.398(4) . ?
C1 C5 1.482(4) . ?
C2 C12 1.481(4) . ?
C3 C4 1.371(4) . ?
C3 C19 1.484(4) . ?
C4 C26 1.477(4) . ?
C5 C6 1.396(4) . ?
C5 C10 1.396(4) . ?
C6 C7 1.388(4) . ?
C7 C8 1.403(4) . ?
C8 C9 1.393(4) . ?
C9 C10 1.376(4) . ?
C12 C17 1.386(5) . ?
C12 C13 1.391(4) . ?
C13 C14 1.383(5) . ?
C14 C15 1.378(5) . ?
C15 C16 1.376(5) . ?
C16 C17 1.386(5) . ?
C19 C20 1.392(4) . ?
C19 C24 1.393(4) . ?
C20 C21 1.390(4) . ?
C21 C22 1.379(5) . ?
C22 C23 1.400(5) . ?
C23 C24 1.384(4) . ?
C26 C31 1.392(4) . ?
C26 C27 1.405(4) . ?
C27 C28 1.378(4) . ?
C28 C29 1.391(4) . ?
C29 C30 1.389(4) . ?
C30 C31 1.392(4) . ?
C1S C2S 1.482(5) . ?
