Dinuclear Cobalt Complex-Catalyzed Stereodivergent Semireduction of Alkynes: Switchable Selectivities Controlled by H2O
Chen, Ke; Zhu, Hongdan; Li, Yuling; Peng, Qian; Guo, Yinlong; Wang, Xiaoming; ACS Catalysis  (2021) 13696–13705; doi:10.1021/acscatal.1c04141

data_4519097
_publ_section_title
;
 Dinuclear Cobalt Complex-Catalyzed Stereodivergent Semireduction of
 Alkynes: Switchable Selectivities Controlled by H2O
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              13696
_journal_page_last               13705
_journal_paper_doi               10.1021/acscatal.1c04141
_journal_year                    2021
_chemical_formula_moiety         'C16 H24 Cl Co N3 O, C F3 O3 S, 2(C2 H3 N)'
_chemical_formula_sum            'C21 H30 Cl Co F3 N5 O4 S'
_chemical_formula_weight         599.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.313(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.228(2)
_cell_length_b                   16.9453(19)
_cell_length_c                   9.6916(12)
_cell_measurement_reflns_used    4418
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      53.82
_cell_measurement_theta_min      4.58
_cell_volume                     2662.9(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      169.97
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1244
_diffrn_reflns_av_unetI/netI     0.1088
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19882
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.212
_diffrn_reflns_theta_min         4.575
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.913
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.3854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1513 before and 0.0905 after correction. The Ratio of minimum to maximum transmission is 0.5133. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.168
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1673
_refine_ls_R_factor_gt           0.0971
_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^)+(0.1000P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2199
_refine_ls_wR_factor_ref         0.2630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2793
_reflns_number_total             4948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c04141_si_002.cif
_cod_data_source_block           mj20023
_cod_original_cell_volume        2662.8(6)
_cod_database_code               4519097
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.695
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Riding coordinates:
 O1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              32337
_shelx_hkl_checksum              93152
_olex2_submission_special_instructions 'No special instructions were received'