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_4335696
_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         'C39 H54 Co K N7'
_chemical_formula_sum            'C39 H54 Co K N7'
_chemical_formula_weight         718.92
_chemical_name_common            CoL(tBu)K
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.5683(19)
_cell_length_b                   19.1491(18)
_cell_length_c                   24.290(2)
_cell_measurement_reflns_used    9279
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.899
_cell_measurement_theta_min      2.216
_cell_volume                     9567.0(15)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'Bruker APEx-II'
_computing_data_reduction        'SAINT, Bruker'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            92104
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  0.9194
_exptl_absorpt_correction_T_min  0.7972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.998
_exptl_crystal_description       Block
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         11058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0353P)^2^+14.5977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                8345
_reflns_number_total             11058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400292g_si_003.cif
_cod_data_source_block           11077zz
_cod_original_cell_volume        9566.8(15)
_cod_database_code               4335696