Catalytic Hydrogenation Activity and Electronic Structure Determination of Bis(arylimidazol-2-ylidene)pyridine Cobalt Alkyl and Hydride Complexes
Renyuan Pony Yu; Jonathan M. Darmon; Carsten Milsmann; Grant W. Margulieux; S. Chantal E. Stieber; Serena DeBeer; Paul J. Chirik; Journal of the American Chemical Society 135 (2013) 13168–13184; doi:10.1021/ja406608u

data_4120737
_publ_section_title
;
 Catalytic Hydrogenation Activity and Electronic Structure Determination
 of Bis(arylimidazol-2-ylidene)pyridine Cobalt Alkyl and Hydride Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13168
_journal_page_last               13184
_journal_paper_doi               10.1021/ja406608u
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C68 H56 B Co F24 N5'
_chemical_formula_weight         1468.92
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.1920(10)
_cell_angle_beta                 76.7130(10)
_cell_angle_gamma                71.7030(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7593(6)
_cell_length_b                   14.5536(7)
_cell_length_c                   19.8946(9)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.52
_cell_volume                     3504.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP 3 (Farraguia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR 92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56542
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker AXS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       block
_exptl_crystal_F_000             1494
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.072
_platon_squeeze_details
;
1 molecule of benzene solvate per asymmetric unit was treated
as a diffuse contribution to the overall scattering through the
use of platon/squeeze.
;
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         15950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.8968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                13220
_reflns_number_total             15950
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja406608u_si_001_3.cif
_cod_data_source_block           ry22
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C0 C68 H56 B Co F24 N5'
_cod_database_code               4120737