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_4518458
_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            'C52 H49 Co P4'
_chemical_formula_weight         856.72
_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   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 92.271(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8781(5)
_cell_length_b                   20.7751(13)
_cell_length_c                   20.9768(12)
_cell_measurement_reflns_used    9412
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      31.54
_cell_measurement_theta_min      3.03
_cell_volume                     4301.4(4)
_computing_cell_refinement       'Bruker APEXIII'
_computing_data_collection       'Bruker APEXIII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Photon 100 CMOS detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            191808
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.084
_diffrn_reflns_theta_min         2.946
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.00115(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         13985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0255P)^2^+2.6348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10692
_reflns_number_total             13985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c05424_si_004.cif
_cod_data_source_block           A031_014
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4518458
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.842
_shelx_estimated_absorpt_t_max   0.943
_shelx_res_checksum              73263
_shelx_hkl_checksum              81036