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_4334737
_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            'C94 H116 Co2 N8 O2'
_chemical_formula_weight         1507.81
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 95.023(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   10.651(5)
_cell_length_b                   16.597(5)
_cell_length_c                   23.856(5)
_cell_measurement_reflns_used    8651
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.72
_cell_measurement_theta_min      5.65
_cell_volume                     4201(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20250
_diffrn_reflns_theta_full        65.97
_diffrn_reflns_theta_max         65.97
_diffrn_reflns_theta_min         5.65
_exptl_absorpt_coefficient_mu    3.491
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.6176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       rod
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         7174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0735P)^2^+0.3906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                6029
_reflns_number_total             7174
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400352r_si_001_3.cif
_cod_data_source_block           cca42
_cod_database_code               4334737