Improvement of Regioselectivity of Alkene Hydrosilylation Catalyzed by [PNSiNP] Pincer Cobalt(III) Hydrides Using Sodium Methoxide as an Additive
Li, Qingshuang; Wei, Lanfeng; Sun, Hongjian; Fuhr, Olaf; Fenske, Dieter; Hinz, Alexander; Li, Xiaoyan; New Journal of Chemistry 49 (2025) 11646–11653; doi:10.1039/D5NJ01460C

data_7063850
_publ_section_title
;
 Improvement of Regioselectivity of Alkene Hydrosilylation Catalyzed by
 [PNSiNP] Pincer Cobalt(III) Hydrides Using Sodium Methoxide as an
 Additive
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11646
_journal_page_last               11653
_journal_paper_doi               10.1039/D5NJ01460C
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C24 H49 Cl Co N2 P3 Si'
_chemical_formula_sum            'C24 H49 Cl Co N2 P3 Si'
_chemical_formula_weight         581.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-05-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-05-05 deposited with the CCDC.	2025-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.2747(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4377(3)
_cell_length_b                   10.88817(18)
_cell_length_c                   18.2030(3)
_cell_measurement_reflns_used    9610
_cell_measurement_temperature    173
_cell_measurement_theta_max      75.7230
_cell_measurement_theta_min      2.9660
_cell_volume                     2921.69(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.940
_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    -85.00  -1.00   1.00    0.10    --  -48.45 113.00-158.00   84
  2  \w     32.00  57.00   1.00    0.10    --   48.45-113.00 109.00   25
  3  \w   -143.00-118.00   1.00    0.45    --  -86.25-113.00 109.00   25
  4  \w    -87.00 -14.00   1.00    0.45    --  -86.25 113.00-158.00   73
  5  \w    114.00 139.00   1.00    0.45    --  106.49 113.00-158.00   25
  6  \w     37.00 112.00   1.00    0.45    --  106.49-113.00 109.00   75
  7  \w   -119.00 -70.00   1.00    0.10    --  -48.45-125.00 150.00   49
  8  \w   -120.00 -33.00   1.00    0.10    --  -48.45 -57.00  90.00   87
  9  \w   -155.00 -84.00   1.00    0.45    --  -86.25 -99.00-120.00   71
 10  \w     34.00 117.00   1.00    0.45    --  106.49-125.00 -30.00   83
 11  \w     93.00 173.00   1.00    0.45    --  106.49 125.00-180.00   80
 12  \w     97.00 177.00   1.00    0.45    --  106.49  57.00 120.00   80
 13  \w     34.00 109.00   1.00    0.45    --  106.49 -99.00 -30.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17586
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.251
_diffrn_reflns_theta_min         2.998
_exptl_absorpt_coefficient_mu    7.501
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
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    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.175
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.00066(11)
_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   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0753P)^2^+9.5001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1537
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5081
_reflns_number_total             5761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01460c2.cif
_cod_data_source_block           191212c
_cod_original_cell_volume        2921.70(9)
_cod_database_code               7063850
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.662
_shelx_estimated_absorpt_t_min   0.552
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C16(H16), C12(H12), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C3(H3), C1(H1)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C17(H17A,H17B,H17C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C8(H8A,
 H8B,H8C), C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C),
 C24(H24A,H24B,H24C)
;
_shelx_res_checksum              74959
_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
;