Radical Mechanisms in the Reaction of Organic Halides with Diiminepyridine Cobalt Complexes
Zhu, Di; Korobkov, Ilia; Budzelaar, Peter H. M.; Organometallics 31 (2012) 3958–; doi:10.1021/om300182c

data_4078267
_publ_section_title
;
 Radical Mechanisms in the Reaction of Organic Halides with
 Diiminepyridine Cobalt Complexes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              3958
_journal_paper_doi               10.1021/om300182c
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C32 H32 Cl Co N4'
_chemical_formula_sum            'C32 H32 Cl Co N4'
_chemical_formula_weight         567.00
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   10.9905(8)
_cell_length_b                   14.5602(11)
_cell_length_c                   18.7056(15)
_cell_measurement_reflns_used    6336
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.942
_cell_measurement_theta_min      2.149
_cell_volume                     2993.3(4)
_computing_cell_refinement       'Bruker Smart program suite V6 (Bruker)'
_computing_data_collection       'Bruker Smart program suite V6 (Bruker)'
_computing_data_reduction        'Bruker Saint program suite V6 (Bruker)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker 4-circle, APEX detector'
_diffrn_measurement_method       'area detector \f and \w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19632
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.77
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Tmin/max = 0.804968'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             1184
_exptl_crystal_recrystallization_method 'Toluene, Hexane'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0912P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                3614
_reflns_number_total             5568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300182c_si_001.cif
_cod_data_source_block           p212121
_cod_database_code               4078267