Additive-Free Cobalt-Catalyzed Hydrogenation of Esters to Alcohols
Yuwen, Jing; Chakraborty, Sumit; Brennessel, William W.; Jones, William D.; ACS Catalysis  (2017) 3735–; doi:10.1021/acscatal.7b00623

data_4514095
_publ_section_title
;
 Additive-Free Cobalt-Catalyzed Hydrogenation of Esters to Alcohols
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              3735
_journal_paper_doi               10.1021/acscatal.7b00623
_journal_year                    2017
_chemical_formula_moiety         'C42 H63 Co N O4 P2, C32 H12 B F24'
_chemical_formula_sum            'C74 H75 B Co F24 N O4 P2'
_chemical_formula_weight         1630.03
_chemical_name_common            jonjy03
_chemical_name_systematic        (CyPNP)Co(O2CPh)2
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                99.053(3)
_cell_angle_beta                 113.620(3)
_cell_angle_gamma                101.693(3)
_cell_formula_units_Z            2
_cell_length_a                   14.722(2)
_cell_length_b                   16.791(3)
_cell_length_c                   17.269(3)
_cell_measurement_reflns_used    4091
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      24.61
_cell_measurement_theta_min      2.31
_cell_volume                     3692.2(11)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016b)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0740
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54850
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.272
_diffrn_reflns_theta_min         1.588
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2016a)'
_exptl_crystal_colour            orange-green
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1237
_refine_ls_number_reflns         13365
_refine_ls_number_restraints     345
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0419P)^2^+3.0242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8387
_reflns_number_total             13365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b00623_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        3692.1(9)
_cod_database_code               4514095
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              67308
_shelx_hkl_checksum              24416