Cobalt-Hydride-Catalyzed Hydrosilylation of 3-Alkynes Accompanying π-Bond Migration
Kim, Yeong Bum; Kim, Dongwook; Dighe, Shashikant U.; Chang, Sukbok; Park, Jung-Woo; ACS Catalysis  (2021) 1548–1553; doi:10.1021/acscatal.0c05424

data_4518457
_publ_section_title
;
 Cobalt-Hydride-Catalyzed Hydrosilylation of 3-Alkynes Accompanying
 \p-Bond Migration
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              1548
_journal_page_last               1553
_journal_paper_doi               10.1021/acscatal.0c05424
_journal_year                    2021
_chemical_formula_sum            'C29 H53 Co P2'
_chemical_formula_weight         522.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 91.33(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2890(19)
_cell_length_b                   9.1000(18)
_cell_length_c                   16.695(3)
_cell_measurement_reflns_used    27434
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      33.575
_cell_measurement_theta_min      0.418
_cell_volume                     1410.8(5)
_computing_cell_refinement       HKL3000sm
_computing_data_collection       'PAL BL2D-SMDC Program'
_computing_data_reduction        HKL3000sm
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.792
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.730
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.792
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14330
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.792
_diffrn_reflns_theta_full        25.976
_diffrn_reflns_theta_max         33.577
_diffrn_reflns_theta_min         2.507
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1009P)^2^+0.5970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1893
_refine_ls_wR_factor_ref         0.2104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2923
_reflns_number_total             4076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c05424_si_005.cif
_cod_data_source_block           PO19082_014
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4518457
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              67255
_shelx_hkl_checksum              67804