#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:08:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180027 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/21/7032112.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_7032112
loop_
_publ_author_name
'Xu, Hongwei'
'Williard, Paul G.'
'Bernskoetter, Wesley H.'
_publ_section_title
;
 C-H bond activation and S-atom transfer from cobalt(iii) thiolate and
 isothiocyanate complexes.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14696
_journal_page_last               14700
_journal_paper_doi               10.1039/c4dt01823k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C18 H48 Co2 N2 P4 S2'
_chemical_formula_weight         598.44
_chemical_name_common            wb19mar14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                103.448(5)
_cell_angle_beta                 102.311(5)
_cell_angle_gamma                105.632(4)
_cell_formula_units_Z            1
_cell_length_a                   8.2115(12)
_cell_length_b                   8.6027(12)
_cell_length_c                   11.4434(16)
_cell_measurement_reflns_used    4949
_cell_measurement_temperature    183.(2)
_cell_measurement_theta_max      24.4701
_cell_measurement_theta_min      2.5845
_cell_volume                     723.54(18)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      183.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.880
_diffrn_measured_fraction_theta_max 0.880
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8850
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear pale brown-gold'
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.478
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0436P)²+0.4734P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                1767
_reflns_number_total             2091
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt01823k2.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 7032110--7032112.cif.'
_cod_database_code               7032112
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_posn
_atom_site_occupancy
C C1 0.3249(4) 0.2135(4) 0.4088(4) 0.0342(8) Uani d . . 1
H H1A 0.3638 0.3359 0.4214 0.051 Uiso calc U R 1
H H1B 0.4211 0.1844 0.4555 0.051 Uiso calc U R 1
H H1C 0.2217 0.1815 0.4393 0.051 Uiso calc U R 1
C C2 0.4479(4) -0.0218(4) 0.2471(4) 0.0299(8) Uani d . . 1
H H2A 0.3922 -0.1454 0.2134 0.045 Uiso calc U R 1
H H2B 0.5113 0.0098 0.3366 0.045 Uiso calc U R 1
H H2C 0.5315 0.0166 0.2017 0.045 Uiso calc U R 1
C C3 0.4225(5) 0.5047(4) 0.2283(5) 0.0446(11) Uani d . . 1
H H3A 0.5187 0.5867 0.2137 0.067 Uiso calc U R 1
H H3B 0.4152 0.5491 0.3133 0.067 Uiso calc U R 1
H H3C 0.3103 0.4856 0.1666 0.067 Uiso calc U R 1
C C4 0.6830(4) 0.3755(4) 0.3270(4) 0.0383(9) Uani d . . 1
H H4A 0.7624 0.4728 0.3133 0.057 Uiso calc U R 1
H H4B 0.7317 0.2826 0.3176 0.057 Uiso calc U R 1
H H4C 0.6716 0.4089 0.412 0.057 Uiso calc U R 1
C C5 0.5184(5) 0.2702(5) 0.0640(4) 0.0430(10) Uani d . . 1
H H5A 0.4125 0.2479 -0.0048 0.064 Uiso calc U R 1
H H5B 0.5595 0.1724 0.0499 0.064 Uiso calc U R 1
H H5C 0.6117 0.3712 0.0669 0.064 Uiso calc U R 1
C C6 -0.1101(5) -0.1073(5) 0.3050(4) 0.0440(10) Uani d . . 1
H H6A -0.1921 -0.0989 0.2326 0.066 Uiso calc U R 1
H H6B -0.0766 -0.0046 0.3763 0.066 Uiso calc U R 1
H H6C -0.1678 -0.2066 0.3278 0.066 Uiso calc U R 1
C C7 0.1884(5) -0.1952(5) 0.3931(4) 0.0426(10) Uani d . . 1
H H7A 0.0993 -0.2883 0.4038 0.064 Uiso calc U R 1
H H7B 0.2359 -0.0992 0.4707 0.064 Uiso calc U R 1
H H7C 0.2847 -0.2336 0.3742 0.064 Uiso calc U R 1
C C8 -0.0031(5) -0.3270(4) 0.1360(4) 0.0439(10) Uani d . . 1
H H8A 0.0921 -0.3505 0.1039 0.066 Uiso calc U R 1
H H8B -0.0924 -0.3176 0.0685 0.066 Uiso calc U R 1
H H8C -0.0579 -0.4197 0.1664 0.066 Uiso calc U R 1
C C9 0.0955(4) -0.1094(4) -0.0570(4) 0.0231(7) Uani d . . 1
Co Co1 0.26003(5) 0.08844(5) 0.22595(4) 0.02308(16) Uani d . . 1
N N1 0.1802(3) -0.0311(3) 0.0459(3) 0.0256(7) Uani d . . 1
P P1 0.46552(11) 0.30526(10) 0.21192(9) 0.0274(2) Uani d . . 1
P P2 0.08733(11) -0.12942(10) 0.26437(9) 0.0285(2) Uani d . . 1
S S1 -0.03427(10) -0.21937(10) -0.20048(9) 0.0288(2) Uani d . . 1
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_site_symmetry_3
_geom_angle
Co1 C1 H1A . 109.5
Co1 C1 H1B . 109.5
H1A C1 H1B . 109.5
Co1 C1 H1C . 109.5
H1A C1 H1C . 109.5
H1B C1 H1C . 109.5
Co1 C2 H2A . 109.5
Co1 C2 H2B . 109.5
H2A C2 H2B . 109.5
Co1 C2 H2C . 109.5
H2A C2 H2C . 109.5
H2B C2 H2C . 109.5
P1 C3 H3A . 109.5
P1 C3 H3B . 109.5
H3A C3 H3B . 109.5
P1 C3 H3C . 109.5
H3A C3 H3C . 109.5
H3B C3 H3C . 109.5
P1 C4 H4A . 109.5
P1 C4 H4B . 109.5
H4A C4 H4B . 109.5
P1 C4 H4C . 109.5
H4A C4 H4C . 109.5
H4B C4 H4C . 109.5
P1 C5 H5A . 109.5
P1 C5 H5B . 109.5
H5A C5 H5B . 109.5
P1 C5 H5C . 109.5
H5A C5 H5C . 109.5
H5B C5 H5C . 109.5
P2 C6 H6A . 109.5
P2 C6 H6B . 109.5
H6A C6 H6B . 109.5
P2 C6 H6C . 109.5
H6A C6 H6C . 109.5
H6B C6 H6C . 109.5
P2 C7 H7A . 109.5
P2 C7 H7B . 109.5
H7A C7 H7B . 109.5
P2 C7 H7C . 109.5
H7A C7 H7C . 109.5
H7B C7 H7C . 109.5
P2 C8 H8A . 109.5
P2 C8 H8B . 109.5
H8A C8 H8B . 109.5
P2 C8 H8C . 109.5
H8A C8 H8C . 109.5
H8B C8 H8C . 109.5
N1 C9 S1 . 176.8(3)
N1 Co1 C1 . 175.88(11)
N1 Co1 C2 . 89.41(13)
C1 Co1 C2 . 94.50(15)
N1 Co1 P1 . 94.26(7)
C1 Co1 P1 . 87.28(10)
C2 Co1 P1 . 86.47(9)
N1 Co1 P2 . 91.69(8)
C1 Co1 P2 . 87.24(10)
C2 Co1 P2 . 86.87(9)
P1 Co1 P2 . 171.01(4)
N1 Co1 S1 2 90.53(7)
C1 Co1 S1 2 85.55(10)
C2 Co1 S1 2 179.77(9)
P1 Co1 S1 2 93.76(3)
P2 Co1 S1 2 92.91(3)
C9 N1 Co1 . 164.6(2)
C5 P1 C3 . 101.77(19)
C5 P1 C4 . 102.38(18)
C3 P1 C4 . 101.11(18)
C5 P1 Co1 . 115.13(12)
C3 P1 Co1 . 117.71(12)
C4 P1 Co1 . 116.33(11)
C8 P2 C7 . 101.71(19)
C8 P2 C6 . 102.07(19)
C7 P2 C6 . 101.07(18)
C8 P2 Co1 . 115.39(12)
C7 P2 Co1 . 116.52(13)
C6 P2 Co1 . 117.59(12)
C9 S1 Co1 2 102.93(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 Co1 . 1.997(4)
C1 H1A . 0.98
C1 H1B . 0.98
C1 H1C . 0.98
C2 Co1 . 2.019(3)
C2 H2A . 0.98
C2 H2B . 0.98
C2 H2C . 0.98
C3 P1 . 1.819(3)
C3 H3A . 0.98
C3 H3B . 0.98
C3 H3C . 0.98
C4 P1 . 1.826(4)
C4 H4A . 0.98
C4 H4B . 0.98
C4 H4C . 0.98
C5 P1 . 1.815(4)
C5 H5A . 0.98
C5 H5B . 0.98
C5 H5C . 0.98
C6 P2 . 1.824(3)
C6 H6A . 0.98
C6 H6B . 0.98
C6 H6C . 0.98
C7 P2 . 1.816(4)
C7 H7A . 0.98
C7 H7B . 0.98
C7 H7C . 0.98
C8 P2 . 1.814(4)
C8 H8A . 0.98
C8 H8B . 0.98
C8 H8C . 0.98
C9 N1 . 1.164(4)
C9 S1 . 1.647(4)
Co1 N1 . 1.952(3)
Co1 P1 . 2.2160(9)
Co1 P2 . 2.2212(9)
Co1 S1 2 2.4162(8)
S1 Co1 2 2.4162(8)
