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_4120735
_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            'C46.67 H54.67 Cl1.33 Co1.33 N6.67'
_chemical_formula_weight         834.81
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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            6
_cell_length_a                   20.1648(4)
_cell_length_b                   20.1648(4)
_cell_length_c                   16.4142(5)
_cell_measurement_reflns_used    9737
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.62
_cell_measurement_theta_min      3.10
_cell_volume                     6674.3(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42595
_diffrn_reflns_theta_full        66.02
_diffrn_reflns_theta_max         66.02
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    4.996
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.5711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker AXS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       shard
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.094
_platon_squeeze_details
;
1 molecule of tetrahydrofuran solvate per asymmetric unit was treated
as a diffuse contribution to the overall scattering through the
use of platon/squeeze.
;
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.021(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+1.1760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                5114
_reflns_number_total             5754
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja406608u_si_001_1.cif
_cod_data_source_block           ry20
_cod_database_code               4120735