#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006447.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2006447
loop_
_publ_author_name
'Fourmigu\'e, M.'
'Perrocheau, V.'
_publ_section_title
;
 Two Heteroleptic Cobalt(III) Cyclopentadienyl/Dithiolene Complexes
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1213
_journal_page_last               1215
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         '[Co (C5 H5 )(C3 S5 )]'
_chemical_formula_sum            'C8 H5 Co S5'
_chemical_formula_weight         320.35
_chemical_name_common            CpCo(dmit)
_chemical_name_systematic
;
(4,5-disulfanyl-1,3-dithiole-2-thionato)(\h-cyclopentadienyl)cobalt(III)
;
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 97.180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.9564(8)
_cell_length_b                   7.8830(3)
_cell_length_c                   23.2930(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.5
_cell_measurement_theta_min      8.3
_cell_volume                     1085.13(15)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.1874
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            2338
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.494
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'SHELXTL/PC (Sheldrick, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.476
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_obs          0.0316
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.8520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0864
_refine_ls_wR_factor_obs         0.0733
_reflns_number_observed          1484
_reflns_number_total             2126
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    ab1475.cif
_[local]_cod_data_source_block   I
_cod_original_cell_volume        1085.1(5)
_cod_database_code               2006447
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_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co 0.0354(3) 0.0396(3) 0.0224(2) 0.0011(2) 0.0075(2) 0.0001(2)
S1 0.0338(5) 0.0511(6) 0.0292(5) -0.0104(4) 0.0085(4) -0.0024(4)
S2 0.0358(5) 0.0544(6) 0.0263(5) -0.0108(5) 0.0035(4) -0.0053(5)
S3 0.0395(5) 0.0491(6) 0.0261(5) -0.0064(5) 0.0043(4) -0.0060(4)
S4 0.0385(5) 0.0526(6) 0.0299(5) -0.0101(5) 0.0108(4) -0.0002(5)
S5 0.0638(7) 0.0536(7) 0.0256(5) -0.0010(6) 0.0144(4) 0.0000(5)
C1 0.032(2) 0.031(2) 0.023(2) -0.0012(14) 0.0044(13) -0.0010(14)
C2 0.033(2) 0.034(2) 0.024(2) -0.002(2) 0.0068(14) -0.001(2)
C3 0.043(2) 0.035(2) 0.027(2) 0.003(2) 0.0084(15) 0.003(2)
C4 0.064(3) 0.066(3) 0.038(2) -0.014(3) 0.020(2) 0.005(2)
C5 0.077(3) 0.057(3) 0.040(3) 0.021(3) 0.030(2) 0.006(2)
C6 0.147(7) 0.101(5) 0.030(3) -0.076(5) 0.037(3) -0.030(3)
C7 0.041(3) 0.238(10) 0.021(2) 0.021(4) 0.002(2) 0.014(4)
C8 0.110(5) 0.077(4) 0.044(3) 0.043(4) 0.031(3) 0.027(3)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Co 0.06733(8) 0.76359(7) 0.13245(2) 0.0322(2) Uani d . 1 Co
S1 0.2647(2) 0.84254(14) 0.21009(4) 0.0376(2) Uani d . 1 S
S2 -0.1977(2) 0.66868(15) 0.17672(4) 0.0389(3) Uani d . 1 S
S3 0.1738(2) 0.82773(14) 0.33537(4) 0.0382(2) Uani d . 1 S
S4 -0.2622(2) 0.67148(15) 0.30416(4) 0.0398(3) Uani d . 1 S
S5 -0.1139(2) 0.75788(15) 0.42773(4) 0.0469(3) Uani d . 1 S
C1 0.0979(6) 0.7928(4) 0.26205(15) 0.0284(8) Uani d . 1 C
C2 -0.1091(6) 0.7165(4) 0.2472(2) 0.0303(8) Uani d . 1 C
C3 -0.0687(6) 0.7523(5) 0.3588(2) 0.0349(8) Uani d . 1 C
C4 0.2789(9) 0.8511(7) 0.0765(2) 0.0548(12) Uani d . 1 C
H4 0.4159(9) 0.9066(7) 0.0866(2) 0.066 Uiso calc R 1 H
C5 0.2531(9) 0.6796(7) 0.0707(2) 0.0559(13) Uani d . 1 C
H5 0.3689(9) 0.5999(7) 0.0762(2) 0.067 Uiso calc R 1 H
C6 0.0258(14) 0.6440(9) 0.0554(2) 0.090(2) Uani d . 1 C
H6 -0.0402(14) 0.5377(9) 0.0490(2) 0.109 Uiso calc R 1 H
C7 -0.0870(9) 0.8059(13) 0.0516(2) 0.100(3) Uani d . 1 C
H7 -0.2411(9) 0.8245(13) 0.0417(2) 0.120 Uiso calc R 1 H
C8 0.0762(12) 0.9277(8) 0.0654(2) 0.075(2) Uani d . 1 C
H8 0.0507(12) 1.0440(8) 0.0668(2) 0.090 Uiso calc R 1 H
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'
S S 0.1246 0.1234 '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_publ_flag
C6 Co C7 41.9(3) no
C6 Co C5 40.0(2) no
C7 Co C5 67.6(2) ?
C6 Co C8 68.0(3) ?
C7 Co C8 39.7(3) ?
C5 Co C8 66.1(2) ?
C6 Co C4 66.8(2) ?
C7 Co C4 66.0(2) ?
C5 Co C4 39.2(2) ?
C8 Co C4 38.5(2) ?
C6 Co S1 152.7(3) ?
C7 Co S1 152.4(3) ?
C5 Co S1 113.9(2) ?
C8 Co S1 113.8(2) ?
C4 Co S1 97.15(15) ?
C6 Co S2 104.5(2) ?
C7 Co S2 103.4(2) ?
C5 Co S2 137.0(2) ?
C8 Co S2 133.5(2) ?
C4 Co S2 169.32(15) ?
S1 Co S2 93.20(4) ?
C1 S1 Co 103.14(13) ?
C2 S2 Co 103.30(12) ?
C3 S3 C1 97.6(2) ?
C3 S4 C2 97.0(2) ?
C2 C1 S1 120.3(3) ?
C2 C1 S3 115.6(3) ?
S1 C1 S3 124.0(2) ?
C1 C2 S2 120.0(3) ?
C1 C2 S4 115.8(3) ?
S2 C2 S4 124.2(2) ?
S5 C3 S3 122.9(2) ?
S5 C3 S4 123.2(2) ?
S3 C3 S4 113.9(2) ?
C8 C4 C5 109.8(5) ?
C8 C4 Co 70.4(3) ?
C5 C4 Co 70.0(3) ?
C4 C5 C6 108.7(5) ?
C4 C5 Co 70.9(3) ?
C6 C5 Co 69.3(3) ?
C5 C6 C7 105.7(5) ?
C5 C6 Co 70.7(3) ?
C7 C6 Co 69.2(3) ?
C8 C7 C6 107.1(5) ?
C8 C7 Co 70.8(3) ?
C6 C7 Co 69.0(3) ?
C4 C8 C7 108.8(6) ?
C4 C8 Co 71.1(3) ?
C7 C8 Co 69.5(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Co C6 2.014(5) no
Co C7 2.017(5) no
Co C5 2.031(4) no
Co C8 2.034(5) no
Co C4 2.043(4) no
Co S1 2.1233(11) no
Co S2 2.1266(11) no
S1 C1 1.705(3) no
S2 C2 1.702(4) no
S3 C3 1.714(4) no
S3 C1 1.733(3) no
S4 C3 1.728(4) no
S4 C2 1.738(4) no
S5 C3 1.661(4) no
C1 C2 1.377(5) no
C4 C8 1.346(7) no
C4 C5 1.366(7) no
C5 C6 1.385(8) no
C6 C7 1.440(10) no
C7 C8 1.376(9) no