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_4518456
_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            'C26 H49 Co P2'
_chemical_formula_weight         482.52
_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   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                109.71(3)
_cell_angle_beta                 102.20(3)
_cell_angle_gamma                98.68(3)
_cell_formula_units_Z            2
_cell_length_a                   10.482(2)
_cell_length_b                   11.480(2)
_cell_length_c                   12.182(2)
_cell_measurement_reflns_used    28733
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      33.749
_cell_measurement_theta_min      0.401
_cell_volume                     1308.9(6)
_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      225(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0128
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9158
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.823
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       plate
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.054
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.023
_refine_diff_density_min         -2.085
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0544P)^2^+2.8134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4194
_reflns_number_total             4603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c05424_si_003.cif
_cod_data_source_block           PO19070_002
_cod_original_cell_volume        1308.9(5)
_cod_database_code               4518456
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              31136
_shelx_hkl_checksum              78954