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_4334736
_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            'C80 H112 Cl2 Co2 N6 O'
_chemical_formula_weight         1362.52
_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                102.117(4)
_cell_angle_beta                 94.450(5)
_cell_angle_gamma                113.268(2)
_cell_formula_units_Z            2
_cell_length_a                   13.552(2)
_cell_length_b                   17.132(3)
_cell_length_c                   19.656(5)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.55
_cell_volume                     4033.0(14)
_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      99(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.970
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36147
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.114
_platon_squeeze_details
;
The unit cell contained one molecule of THF and one molecule of
pentane which were treated as a diffuse contribution 
to the overall scattering through the use of PLATON/SQUEEZE.
;
_refine_diff_density_max         2.839
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         17939
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1742P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2419
_refine_ls_wR_factor_ref         0.2633
_reflns_number_gt                12494
_reflns_number_total             17939
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400352r_si_001_2.cif
_cod_data_source_block           cca37
_cod_original_cell_volume        4033.0(13)
_cod_database_code               4334736