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_1550214
_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         'C70 H106 Co2 N4 O'
_chemical_formula_sum            'C70 H106 Co2 N4 O'
_chemical_formula_weight         1137.44
_chemical_name_common            holma07
_chemical_name_systematic        bis(diketiminate-cobalt(II))(mu-oxo)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_audit_update_record
;
2018-03-13 deposited with the CCDC.
2018-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                95.195(3)
_cell_angle_beta                 102.214(2)
_cell_angle_gamma                97.097(3)
_cell_formula_units_Z            4
_cell_length_a                   13.4757(15)
_cell_length_b                   21.712(2)
_cell_length_c                   25.061(3)
_cell_measurement_reflns_used    4073
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      24.45
_cell_measurement_theta_min      2.17
_cell_volume                     7059.9(13)
_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-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1729
_diffrn_reflns_av_unetI/netI     0.1316
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            170497
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.030
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.190
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_description       plate
_exptl_crystal_F_000             2464
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_platon_squeeze_details
; 
 See above in "_refine_special_details."
;
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1456
_refine_ls_number_reflns         24927
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0972P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1714
_refine_ls_wR_factor_ref         0.1960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12485
_reflns_number_total             24927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02599a2.cif
_cod_data_source_block           3
_cod_original_cell_volume        7060.1(14)
_cod_database_code               1550214
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.905
_diffrn_source_monochromator     graphite
_shelxl_version_number           2012-5
_shelx_res_checksum              12848