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_4335695
_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         'C45 H42 Co Fe N7'
_chemical_formula_sum            'C45 H42 Co Fe N7'
_chemical_formula_weight         795.64
_chemical_name_common            FeCoL(Ph)
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.9559(19)
_cell_length_b                   14.9559(19)
_cell_length_c                   29.250(4)
_cell_measurement_reflns_used    3812
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.72
_cell_volume                     5666.1(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            13888
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.72
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.9499
_exptl_absorpt_correction_T_min  0.7456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.054
_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     163
_refine_ls_number_reflns         2900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+7.3680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                1992
_reflns_number_total             2900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400292g_si_002.cif
_cod_data_source_block           12045_0m
_cod_original_cell_volume        5666.0(12)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4335695