Reversible Carbon-Carbon Bond Formation Induced by Oxidation and Reduction at a Redox-Active Cobalt Complex
Crisita Carmen Hojilla Atienza; Carsten Milsmann; Scott P. Semproni; Zoë R. Turner; Paul J. Chirik; Inorganic Chemistry 52 (2013) 5403–5417; doi:10.1021/ic400352r

data_4334740
_publ_section_title
;
 Reversible Carbon-Carbon Bond Formation Induced by Oxidation and
 Reduction at a Redox-Active Cobalt Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5403
_journal_page_last               5417
_journal_paper_doi               10.1021/ic400352r
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C33 H43 Co N4 O'
_chemical_formula_weight         570.64
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   8.457(5)
_cell_length_b                   17.761(5)
_cell_length_c                   20.141(5)
_cell_measurement_reflns_used    7209
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.50
_cell_volume                     3025(2)
_computing_cell_refinement       'SHELXL-97 (Sheldrick, 2008)'
_computing_data_collection       'BRUKER APEX II software suite (Bruker AXS)'
_computing_data_reduction        'BRUKER APEX II software suite (Bruker AXS)'
_computing_molecular_graphics    'ORTEP 3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Farrugia, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23711
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       shard
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                5305
_reflns_number_total             6946
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400352r_si_001_6.cif
_cod_data_source_block           cca44
_cod_database_code               4334740