Mixed-Valent Dicobalt and Iron-Cobalt Complexes with High-Spin Configurations and Short Metal-Metal Bonds
Christopher M. Zall; Laura J. Clouston; Victor G. Young; Keying Ding; Hyun Jung Kim; Danylo Zherebetskyy; Yu-Sheng Chen; Eckhard Bill; Laura Gagliardi; Connie C. Lu; Inorganic Chemistry 52 (2013) 9216–9228; doi:10.1021/ic400292g

data_4335694
_publ_section_title
;
 Mixed-Valent Dicobalt and Iron-Cobalt Complexes with High-Spin
 Configurations and Short Metal-Metal Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9216
_journal_page_last               9228
_journal_paper_doi               10.1021/ic400292g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'Co K O C49 H50 N7'
_chemical_formula_sum            'C49 H50 Co K N7 O'
_chemical_formula_weight         850.99
_chemical_name_common            CoL(Ph)K(THF)
_space_group_IT_number           14
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.4940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3407(5)
_cell_length_b                   21.5502(10)
_cell_length_c                   17.9220(8)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.467
_cell_measurement_theta_min      2.293
_cell_volume                     4375.9(3)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49826
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.9010
_exptl_absorpt_correction_T_min  0.7406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       Block
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         10090
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0446
_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/[\s^2^(Fo^2^)+(0.0628P)^2^+0.6790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                6643
_reflns_number_total             10090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400292g_si_001.cif
_cod_data_source_block           12235_0m
_cod_database_code               4335694