#------------------------------------------------------------------------------
#$Date: 2019-11-23 05:24:37 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232225 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/72/4347212.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_4347212
loop_
_publ_author_name
'Fliedel, Christophe'
'Rosa, Vitor'
'Vileno, Bertrand'
'Parizel, Nathalie'
'Choua, Sylvie'
'Gourlaouen, Christophe'
'Rosa, Patrick'
'Turek, Philippe'
'Braunstein, Pierre'
_publ_section_title
;
 Zwitterionic Cobalt Complexes with
 Bis(diphenylphosphino)(N-thioether)amine Assembling Ligands: Structural,
 EPR, Magnetic, and Computational Studies.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4183
_journal_page_last               4198
_journal_paper_doi               10.1021/acs.inorgchem.5b02889
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C4 H12 Cl3 Co N S'
_chemical_formula_sum            'C4 H12 Cl3 Co N S'
_chemical_formula_weight         271.49
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.5383(4)
_cell_length_b                   11.1199(5)
_cell_length_c                   18.1015(9)
_cell_measurement_reflns_used    1544
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.26
_cell_measurement_theta_min      0.998
_cell_volume                     2121.22(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4030
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.49
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.508
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'L. Spek, J. Appl.Cryst. 2003, 36, 7, B. Blessing, Acta Cryst, 1995, A51, 33'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0369P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                1672
_reflns_number_total             2165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02889_si_002.cif
_cod_data_source_block           VL_50b
_cod_database_code               4347212
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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
Co1 Co 0.61904(4) 0.11259(3) 0.12584(2) 0.02297(14) Uani 1 1 d
Cl1 Cl 0.48557(7) -0.04136(7) 0.10389(4) 0.0300(2) Uani 1 1 d
Cl2 Cl 0.53252(7) 0.29292(7) 0.10560(5) 0.0349(2) Uani 1 1 d
Cl3 Cl 0.80492(7) 0.09574(6) 0.06403(4) 0.0277(2) Uani 1 1 d
S1 S 0.70461(7) 0.08861(7) 0.24572(4) 0.0272(2) Uani 1 1 d
N1 N 0.7885(3) 0.1489(3) 0.48594(15) 0.0262(6) Uani 1 1 d
C1 C 0.5814(3) 0.0951(3) 0.31571(18) 0.0297(7) Uani 1 1 d
C2 C 0.6357(3) 0.0742(3) 0.39267(18) 0.0277(7) Uani 1 1 d
C3 C 0.7148(3) 0.1790(3) 0.41804(18) 0.0282(7) Uani 1 1 d
C4 C 0.7400(4) -0.0703(3) 0.2447(2) 0.0394(9) Uani 1 1 d
H1 H 0.544(3) 0.175(3) 0.3135(17) 0.034(8) Uiso 1 1 d
H2 H 0.527(3) 0.035(3) 0.3065(17) 0.029(8) Uiso 1 1 d
H3 H 0.571(3) 0.061(3) 0.4266(17) 0.031(8) Uiso 1 1 d
H4 H 0.690(3) 0.004(3) 0.3940(15) 0.021(8) Uiso 1 1 d
H5 H 0.773(3) 0.205(3) 0.3826(18) 0.039(10) Uiso 1 1 d
H6 H 0.666(4) 0.244(4) 0.429(2) 0.062(12) Uiso 1 1 d
H7 H 0.782(3) -0.094(3) 0.288(2) 0.047(10) Uiso 1 1 d
H8 H 0.666(4) -0.113(3) 0.2439(19) 0.045(11) Uiso 1 1 d
H9 H 0.791(3) -0.083(3) 0.201(2) 0.058(12) Uiso 1 1 d
H11 H 0.854(3) 0.095(3) 0.4777(19) 0.047(11) Uiso 1 1 d
H12 H 0.825(3) 0.213(3) 0.5053(17) 0.041(10) Uiso 1 1 d
H13 H 0.741(4) 0.110(3) 0.520(2) 0.069(14) Uiso 1 1 d
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0230(2) 0.0221(2) 0.0238(3) 0.00034(17) -0.00078(17) -0.00057(17)
Cl1 0.0266(4) 0.0275(4) 0.0358(5) -0.0012(4) -0.0007(3) -0.0055(3)
Cl2 0.0302(4) 0.0237(4) 0.0509(5) -0.0008(4) -0.0043(4) 0.0033(3)
Cl3 0.0243(4) 0.0268(4) 0.0320(5) 0.0025(3) 0.0038(3) 0.0009(3)
S1 0.0265(4) 0.0326(4) 0.0225(4) -0.0006(3) -0.0011(3) -0.0016(3)
N1 0.0287(16) 0.0278(15) 0.0221(15) -0.0007(13) -0.0028(12) -0.0007(13)
C1 0.0215(16) 0.040(2) 0.0274(19) -0.0002(16) -0.0017(14) -0.0011(16)
C2 0.0201(16) 0.0391(19) 0.0240(18) 0.0006(15) 0.0028(14) -0.0039(15)
C3 0.0323(18) 0.0256(17) 0.0266(19) 0.0024(15) -0.0024(15) 0.0052(15)
C4 0.048(2) 0.038(2) 0.032(2) 0.0003(18) -0.006(2) 0.0079(19)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Co Co 0.3494 0.9721 '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'
S S 0.1246 0.1234 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Cl2 Co1 Cl1 113.51(3)
Cl2 Co1 Cl3 110.28(3)
Cl1 Co1 Cl3 112.99(3)
Cl2 Co1 S1 114.05(3)
Cl1 Co1 S1 108.33(3)
Cl3 Co1 S1 96.56(3)
C4 S1 C1 101.18(19)
C4 S1 Co1 100.35(13)
C1 S1 Co1 111.29(11)
C3 N1 H11 114(2)
C3 N1 H12 112(2)
H11 N1 H12 105(3)
C3 N1 H13 113(3)
H11 N1 H13 103(3)
H12 N1 H13 110(3)
C2 C1 S1 111.3(2)
C2 C1 H1 109.2(19)
S1 C1 H1 107.3(18)
C2 C1 H2 107(2)
S1 C1 H2 107.4(19)
H1 C1 H2 115(3)
C3 C2 C1 111.6(3)
C3 C2 H3 109(2)
C1 C2 H3 110.5(19)
C3 C2 H4 107.0(17)
C1 C2 H4 111.5(16)
H3 C2 H4 107(3)
N1 C3 C2 111.5(3)
N1 C3 H5 106.9(19)
C2 C3 H5 113(2)
N1 C3 H6 107(2)
C2 C3 H6 111(2)
H5 C3 H6 106(3)
S1 C4 H7 111(2)
S1 C4 H8 109(2)
H7 C4 H8 106(3)
S1 C4 H9 105(2)
H7 C4 H9 113(3)
H8 C4 H9 112(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 Cl2 2.2331(8)
Co1 Cl1 2.2510(8)
Co1 Cl3 2.2636(8)
Co1 S1 2.3650(9)
S1 C4 1.806(4)
S1 C1 1.816(3)
N1 C3 1.492(4)
N1 H11 0.92(4)
N1 H12 0.88(4)
N1 H13 0.91(4)
C1 C2 1.524(4)
C1 H1 0.97(3)
C1 H2 0.90(3)
C2 C3 1.505(5)
C2 H3 0.93(3)
C2 H4 0.96(3)
C3 H5 0.93(3)
C3 H6 0.91(4)
C4 H7 0.94(4)
C4 H8 0.91(4)
C4 H9 0.97(4)
