Cobalt N-Heterocyclic Phosphenium Complexes Stabilized by a Chelating Framework: Synthesis and Redox Properties.
Bezpalko, Mark W.; Poitras, Andrew M.; Foxman, Bruce M.; Thomas, Christine M.; Inorganic chemistry 56 (2017) 503–510; doi:10.1021/acs.inorgchem.6b02374

data_4349317
_publ_section_title
;
 Cobalt N-Heterocyclic Phosphenium Complexes Stabilized by a Chelating
 Framework: Synthesis and Redox Properties.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              503
_journal_page_last               510
_journal_paper_doi               10.1021/acs.inorgchem.6b02374
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C35 H47 Co1 N2 P4'
_chemical_formula_sum            'C35 H47 Co N2 P4'
_chemical_formula_weight         678.60
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2015-12-17
_audit_creation_method           CRYSTALS_ver_14.61_build_00000
_cell_angle_alpha                90
_cell_angle_beta                 107.6227(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1093(6)
_cell_length_b                   37.469(2)
_cell_length_c                   10.6957(7)
_cell_measurement_reflns_used    6953
_cell_measurement_temperature    120
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3479.3(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            36410
_diffrn_reflns_theta_full        26.034
_diffrn_reflns_theta_max         26.034
_diffrn_reflns_theta_min         2.070
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6868
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.0039833
_refine_ls_shift/su_mean         0.0002873
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 2.54P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0762
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0762
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              46
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                5303
_reflns_number_total             6868
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.22
_oxford_diffrn_Wilson_scale      93.69
_oxford_refine_ls_r_factor_ref   0.0528
_oxford_refine_ls_scale          0.10936(2)
_oxford_reflns_number_all        6868
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mwb5_082_0m in P2(1)/c'
_cod_data_source_file            ic6b02374_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C35 H47 Co1 N2 P4'
_cod_database_code               4349317