Reactions of Neutral Cobalt(II) Complexes of a Dianionic Tetrapodal Pentadentate Ligand: Cobalt(III) Amides from Imido Radicals.
Nurdin, Lucie; Spasyuk, Denis M.; Piers, Warren E.; Maron, Laurent; Inorganic chemistry  (2017) –; doi:10.1021/acs.inorgchem.7b00174

data_4345542
_publ_section_title
;
 Reactions of Neutral Cobalt(II) Complexes of a Dianionic Tetrapodal
 Pentadentate Ligand: Cobalt(III) Amides from Imido Radicals.
;
_journal_name_full               'Inorganic chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.7b00174
_journal_year                    2017
_chemical_formula_moiety         'C37 H29 B2 Co F6 N10, 2(C6 H6)'
_chemical_formula_sum            'C49 H41 B2 Co F6 N10'
_chemical_formula_weight         964.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.228(4)
_cell_length_b                   9.862(2)
_cell_length_c                   22.726(5)
_cell_measurement_reflns_used    65713
_cell_measurement_temperature    173
_cell_measurement_theta_max      24.411
_cell_measurement_theta_min      1.306
_cell_volume                     4533.6(16)
_computing_cell_refinement       'XDS (Kabsch (2010)'
_computing_data_collection       'MxDC, (Fodje, 2012)'
_computing_data_reduction        'XDS (Kabsch (2010)'
_computing_molecular_graphics    'ShelXle (Hubschle, 2011)'
_computing_publication_material  'LinXTL v. 5.7.8 (Spasyuk, 2009)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rayonix MX300HE CCD area detector'
_diffrn_measurement_method       '\k and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68881
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61203
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.306
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.1004
_exptl_absorpt_correction_T_min  0.0687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         4474
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0791P)^2^+7.5941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4233
_reflns_number_total             4474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00174_si_002.cif
_cod_data_source_block           2-CF3
_cod_database_code               4345542
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              88720
_shelx_hkl_checksum              64281