Cobalt-Group 13 Complexes Catalyze CO2 Hydrogenation via a Co(−I)/Co(I) Redox Cycle
Vollmer, Matthew V.; Ye, Jingyun; Linehan, John C.; Graziano, Brendan J.; Preston, Andrew; Wiedner, Eric S.; Lu, Connie C.; ACS Catalysis  (2020) 2459–2470; doi:10.1021/acscatal.9b03534

data_4517373
_publ_section_title
;
 Cobalt-Group 13 Complexes Catalyze CO2 Hydrogenation via a
 Co(&#x2212;I)/Co(I) Redox Cycle
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              2459
_journal_page_last               2470
_journal_paper_doi               10.1021/acscatal.9b03534
_journal_year                    2020
_chemical_formula_moiety         'C39 H61 N4 P3 Al Co, 0.5(C6 H6)'
_chemical_formula_sum            'C42 H64 Al Co N4 P3'
_chemical_formula_weight         803.79
_chemical_name_common            19092_AlCoH
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 105.97(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.329(6)
_cell_length_b                   27.522(13)
_cell_length_c                   12.652(7)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.23
_cell_volume                     4127(4)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX3, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'Shelxle-(Rev. 825) (Huebschle, C. B.,2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker PHOTON-II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1079
_diffrn_reflns_av_unetI/netI     0.1124
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            117044
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.596
_diffrn_reflns_theta_min         2.173
_diffrn_source                   'micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            'dichroic blue-yellow'
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   0.722
_exptl_transmission_factor_min   0.603
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.192(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         25258
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0416P)^2^+0.0869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.960
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                17421
_reflns_number_total             25258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b03534_si_002.cif
_cod_data_source_block           mo_19092_0m_a
_cod_depositor_comments
;

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 4517371--4517374.cif.
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_moiety     '2(C39 H61 N4 P3 Al Co), C6 H6'
_cod_original_formula_sum        'C84 H128 Al2 Co2 N8 P6'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1607.58
_cod_database_code               4517373
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.640
_shelx_estimated_absorpt_t_max   0.773
_shelx_res_checksum              50749
_shelx_hkl_checksum              90566