Effects of silylene ligands on performance of carbonyl hydrosilylation catalyzed by cobalt phosphine complexes
Fan, Qingqing; Du, Xinyu; Yang, Wenjing; Li, Qingshuang; Huang, Wei; Sun, Hongjian; Hinz, Alexander; Li, Xiaoyan; Dalton Transactions  (2023) –; doi:10.1039/D3DT00372H

data_7712808
_publ_section_title
;
 Effects of silylene ligands on performance of carbonyl hydrosilylation
 catalyzed by cobalt phosphine complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00372H
_journal_year                    2023
_chemical_formula_moiety         'C15 H35 Cl Co P3 Si'
_chemical_formula_sum            'C15 H35 Cl Co P3 Si'
_chemical_formula_weight         430.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-21 deposited with the CCDC.	2023-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.062(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.1266(7)
_cell_length_b                   12.8624(3)
_cell_length_c                   12.9099(3)
_cell_measurement_reflns_used    6134
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.6430
_cell_measurement_theta_min      4.8220
_cell_volume                     4501.52(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     29.00  78.00   1.00    0.80    --   48.45  72.00 128.00   49
  2  \w      2.00  69.00   1.00    0.80    --   48.45 -72.00  -1.00   67
  3  \w    -69.00  11.00   1.00    0.80    --  -48.45  72.00 128.00   80
  4  \w   -120.00 -74.00   1.00    0.80    --  -48.45-125.00  60.00   46
  5  \w   -106.00 -28.00   1.00    0.80    --  -48.45 -72.00  -1.00   78
  6  \w    -81.00 -56.00   1.00    3.99    --  -86.25  72.00 128.00   25
  7  \w   -158.00-133.00   1.00    3.99    --  -86.25 -72.00  -1.00   25
  8  \w     86.00 171.00   1.00    3.99    --  106.49  72.00 128.00   85
  9  \w     94.00 177.00   1.00    3.99    --  106.49  19.00  90.00   83
 10  \w     94.00 171.00   1.00    3.99    --  106.49  19.00-150.00   77
 11  \w     38.00 105.00   1.00    3.99    --  106.49 -77.00  60.00   67
 12  \w     47.00  91.00   1.00    3.99    --  106.49 -72.00  -1.00   44
 13  \w     40.00 101.00   1.00    3.99    --  106.49 -77.00 -60.00   61
 14  \w     34.00 101.00   1.00    3.99    --  106.49 -77.00-120.00   67
 15  \w     36.00 106.00   1.00    3.99    --  106.49 -99.00-150.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0463950000
_diffrn_orient_matrix_UB_12      0.0425068000
_diffrn_orient_matrix_UB_13      0.0475071000
_diffrn_orient_matrix_UB_21      -0.0551677000
_diffrn_orient_matrix_UB_22      0.0867864000
_diffrn_orient_matrix_UB_23      -0.0300730000
_diffrn_orient_matrix_UB_31      -0.0951344000
_diffrn_orient_matrix_UB_32      -0.0707992000
_diffrn_orient_matrix_UB_33      -0.0083553000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13144
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.260
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    9.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.919
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0693P)^2^+47.3247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3525
_reflns_number_total             3996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00372h2.cif
_cod_data_source_block           210319a
_cod_database_code               7712808
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CoC
_shelx_estimated_absorpt_t_max   0.449
_shelx_estimated_absorpt_t_min   0.449
_diffrn_oxdiff_digest_frames
;
011bd4f28ddb80efc0692d2c7f061aa9ba00030b8e5
;
_diffrn_oxdiff_digest_hkl
;
01b9aa27e84872630bd5bb4791c0c30bade88a
;
_reflns_odcompleteness_completeness 98.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Si(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Co1) = Uanis(P1)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C2(H2), C3(H3), C6(H6)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C13(H13A,H13B,
 H13C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,
 H8C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              62282
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.945
_oxdiff_exptl_absorpt_empirical_full_min 0.627