Zwitterionic Cobalt Complexes with Bis(diphenylphosphino)(N-thioether)amine Assembling Ligands: Structural, EPR, Magnetic, and Computational Studies.
Fliedel, Christophe; Rosa, Vitor; Vileno, Bertrand; Parizel, Nathalie; Choua, Sylvie; Gourlaouen, Christophe; Rosa, Patrick; Turek, Philippe; Braunstein, Pierre; Inorganic chemistry 55 (2016) 4183–4198; doi:10.1021/acs.inorgchem.5b02889

data_4347211
_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         'C56 H58 Cl Co N2 P4 S2, F6 P, C H2 Cl2'
_chemical_formula_sum            'C57 H60 Cl3 Co F6 N2 P5 S2'
_chemical_formula_weight         1271.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 106.959(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.4062(17)
_cell_length_b                   13.0561(6)
_cell_length_c                   22.6438(5)
_cell_measurement_reflns_used    11460
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      0.998
_cell_volume                     12557.3(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction
'HKL Denzo & Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21245
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.354
_diffrn_reflns_theta_min         1.632
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             5240
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         2.419
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       0.00188(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         12792
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0875
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1792P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2473
_refine_ls_wR_factor_ref         0.2750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7484
_reflns_number_total             12792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02889_si_002.cif
_cod_data_source_block           pbvrcf100501a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347211
_shelxl_version_number           2013-4
_shelx_res_checksum              83791
_shelx_hkl_checksum              11909