Reactivity of a <i>cis</i>-(silyl)(boryl) moiety with a nickel center involving the oxidative addition and reductive elimination of a silylborane.
Suga, Yuto; Sunada, Yusuke; Chemical communications (Cambridge, England) 61 (2025) 14370–14373; doi:10.1039/d5cc03463a

data_1575458
_publ_section_title
;
 Reactivity of a <i>cis</i>-(silyl)(boryl) moiety with a nickel center
 involving the oxidative addition and reductive elimination of a
 silylborane.
;
_journal_issue                   75
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14370
_journal_page_last               14373
_journal_paper_doi               10.1039/d5cc03463a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C32 H55 B N4 Ni O2 Si'
_chemical_formula_sum            'C32 H55 B N4 Ni O2 Si'
_chemical_formula_weight         625.41
_chemical_name_systematic        Ni(SiMe2Ph)(Bpin)(iPrIM)2
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-04-06
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-06-10 deposited with the CCDC.	2025-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.687(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7704(5)
_cell_length_b                   18.1839(7)
_cell_length_c                   18.7207(6)
_cell_measurement_reflns_used    8984
_cell_measurement_temperature    297
_cell_measurement_theta_max      27.2050
_cell_measurement_theta_min      2.9210
_cell_volume                     3654.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      297
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.820
_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      7.00  33.00   0.50   12.00    --    5.96 -90.00 130.00   52
  2  \w    -41.00   0.00   0.50   12.00    --    5.96 -90.00 130.00   82
  3  \w    -11.00  24.00   0.50   12.00    --    5.96 -99.00   0.00   70
  4  \w    -11.00  38.00   0.50   12.00    --    5.96 -99.00-150.00   98
  5  \w      7.00  37.00   0.50   12.00    --    5.96 -99.00  30.00   60
  6  \w     -8.00  38.00   0.50   12.00    --    5.96 -99.00  60.00   92
  7  \w      1.00  38.00   0.50   12.00    --    5.96 -99.00 -90.00   74
  8  \w    -18.00  35.00   0.50   12.00    --    5.96  90.00-114.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0279295000
_diffrn_orient_matrix_UB_12      0.0353135000
_diffrn_orient_matrix_UB_13      -0.0003618000
_diffrn_orient_matrix_UB_21      -0.0244640000
_diffrn_orient_matrix_UB_22      0.0049736000
_diffrn_orient_matrix_UB_23      -0.0360165000
_diffrn_orient_matrix_UB_31      -0.0546313000
_diffrn_orient_matrix_UB_32      0.0158137000
_diffrn_orient_matrix_UB_33      0.0121895000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.820
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40330
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.927
_diffrn_reflns_theta_min         2.389
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_preparation       'Ni(iPrIM)2(cod)n + PhMe2Si-Bpin'
_exptl_crystal_recrystallization_method 'cooling saturated pentane solution'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         9505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0459P)^2^+1.1149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5848
_reflns_number_total             9505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03463a2.cif
_cod_data_source_block           ys250120_auto
_cod_depositor_comments
'Adding full bibliography for 1575458--1575459.cif.'
_cod_original_cell_volume        3654.2(2)
_cod_database_code               1575458
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Ni Si C N H B O'
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.895
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C25(H25), C16(H16), C28(H28), C19(H19)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C6(H6), C5(H5), C22(H22), C23(H23), C32(H32), C7(H7), C31(H31)
2.c Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C1(H1a,H1b,H1c), C17(H17a,H17b,H17c), C27(H27a,H27b,H27c),
 C26(H26a,H26b,H26c), C18(H18a,H18b,H18c), C30(H30a,H30b,H30c), C14(H14a,H14b,
 H14c), C20(H20a,H20b,H20c), C29(H29a,H29b,H29c), C13(H13a,H13b,H13c), C21(H21a,
 H21b,H21c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c)
;
_shelx_res_checksum              81811
_shelx_hkl_checksum              94977
_olex2_exptl_crystal_mounting_method loop
_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 1.388
_oxdiff_exptl_absorpt_empirical_full_min 0.530