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_7712807
_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         'C39 H63 Cl3 Co N4 P Si3'
_chemical_formula_sum            'C39 H63 Cl3 Co N4 P Si3'
_chemical_formula_weight         868.45
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-09 deposited with the CCDC.	2023-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7072(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.27681(17)
_cell_length_b                   19.2189(3)
_cell_length_c                   15.42856(19)
_cell_measurement_reflns_used    3963
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.0150
_cell_measurement_theta_min      4.8400
_cell_volume                     4507.42(10)
_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    'ShelXT (Sheldrick, 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 0.986
_diffrn_measured_fraction_theta_max 0.941
_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     93.00 164.00   1.00    0.85    --  106.49  38.00  -4.00   71
  2  \w    101.00 178.00   1.00    0.85    --  106.49  19.00 120.00   77
  3  \w     47.00  73.00   1.00    0.10    --   48.45  38.00  -4.00   26
  4  \w     34.00 105.00   1.00    0.85    --  106.49 -77.00  60.00   71
  5  \w     34.00  65.00   1.00    0.85    --  106.49 -57.00  90.00   31
  6  \w     34.00  66.00   1.00    0.85    --  106.49 -57.00 120.00   32
  7  \w     90.00 105.00   1.00    0.85    --  106.49 -77.00-120.00   15
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0545559000
_diffrn_orient_matrix_UB_12      0.0053759000
_diffrn_orient_matrix_UB_13      0.0892764000
_diffrn_orient_matrix_UB_21      -0.0732412000
_diffrn_orient_matrix_UB_22      -0.0381157000
_diffrn_orient_matrix_UB_23      0.0426315000
_diffrn_orient_matrix_UB_31      0.0439032000
_diffrn_orient_matrix_UB_32      -0.0703208000
_diffrn_orient_matrix_UB_33      -0.0163934000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28041
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.583
_diffrn_reflns_theta_min         3.685
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.959
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58583
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0526P)^2^+2.7040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7590
_reflns_number_total             8920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00372h2.cif
_cod_data_source_block           210315a
_cod_original_cell_volume        4507.43(10)
_cod_database_code               7712807
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         CoC
_shelx_estimated_absorpt_t_max   0.587
_shelx_estimated_absorpt_t_min   0.587
_diffrn_oxdiff_digest_frames
;
014bd8f8d260f17071027ccc47cf51b6f4000293117
;
_diffrn_oxdiff_digest_hkl
;
01d8cff3ff9cee1ff4529a37ace71e7c2c9262
;
_reflns_odcompleteness_completeness 62.90
_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.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C2(H2), C35(H35), C3(H3), C34(H34), C32(H32), C21(H21), C6(H6),
 C17(H17), C33(H33), C4(H4), C20(H20), C5(H5), C18(H18), C19(H19)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C), C7(H7A,H7B,H7C),
 C28(H28A,H28B,H28C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C11(H11A,H11B,H11C), C38(H38A,H38B,H38C), C37(H37A,
 H37B,H37C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              47299
_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 1.538
_oxdiff_exptl_absorpt_empirical_full_min 0.657