Reduction of CO2 by a masked two-coordinate cobalt(i) complex and characterization of a proposed oxodicobalt(ii) intermediate
Roy, Lisa; Al-Afyouni, Malik H.; DeRosha, Daniel E.; Mondal, Bhaskar; DiMucci, Ida M.; Lancaster, Kyle M.; Shearer, Jason; Bill, Eckhard; Brennessel, William W.; Neese, Frank; Ye, Shengfa; Holland, Patrick L.; Chemical Science  (2019) –; doi:10.1039/C8SC02599A

data_1550215
_publ_section_title
;
 Reduction of CO2 by a masked two-coordinate cobalt(i) complex and
 characterization of a proposed oxodicobalt(ii) intermediate
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC02599A
_journal_year                    2019
_chemical_formula_moiety         'C71 H106 Co2 N4 O3'
_chemical_formula_sum            'C71 H106 Co2 N4 O3'
_chemical_formula_weight         1181.46
_chemical_name_common            holma06
_chemical_name_systematic        bis(diketiminate-cobalt(II))(mu-carbonato)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-03-13 deposited with the CCDC.
2018-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 114.237(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.919(2)
_cell_length_b                   28.234(3)
_cell_length_c                   24.420(3)
_cell_measurement_reflns_used    3821
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.33
_cell_volume                     13152(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       '\w 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  0.1037
_diffrn_reflns_av_sigmaI/netI    0.1308
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            102642
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.82
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.9468
_exptl_absorpt_correction_T_min  0.8431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5104
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.272
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
'Flack H D (1983), 17737 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1511
_refine_ls_number_reflns         36193
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0435P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                22440
_reflns_number_total             36193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8sc02599a2.cif
_cod_data_source_block           4
_cod_original_cell_volume        13152(3)
_cod_database_code               1550215