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_4519096
_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         '0.5(C48 H40 O4 Si4)'
_chemical_formula_sum            'C24 H20 O2 Si2'
_chemical_formula_weight         396.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                83.3240(10)
_cell_angle_beta                 83.8100(10)
_cell_angle_gamma                76.0750(10)
_cell_formula_units_Z            4
_cell_length_a                   10.66780(10)
_cell_length_b                   10.72300(10)
_cell_length_c                   18.8751(3)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.914
_cell_measurement_theta_min      3.728
_cell_volume                     2074.32(4)
_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      172.99
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34805
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.935
_diffrn_reflns_theta_min         3.711
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0987 before and 0.0457 after correction. The Ratio of minimum to maximum transmission is 0.8296. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.8014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7231
_reflns_number_total             7848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c04141_si_003.cif
_cod_data_source_block           mj19759_0m
_cod_database_code               4519096
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.854
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48)
;
_shelx_res_checksum              56532
_shelx_hkl_checksum              44736
_olex2_submission_special_instructions 'No special instructions were received'