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_1575459
_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         'C27 H46 N4 Ni'
_chemical_formula_sum            'C27 H46 N4 Ni'
_chemical_formula_weight         485.39
_chemical_name_systematic        Ni(Cy-allene)(iPrIM)2
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-17
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7308)
;
_audit_update_record
;
2025-08-01 deposited with the CCDC.	2025-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.959(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0604(5)
_cell_length_b                   9.9004(3)
_cell_length_c                   19.0001(6)
_cell_measurement_reflns_used    8583
_cell_measurement_temperature    173
_cell_measurement_theta_max      31.0190
_cell_measurement_theta_min      2.6380
_cell_volume                     2826.23(16)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_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 0.805
_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      0.00  72.00   0.50    2.50    --    5.81  57.00   0.00  144
  2  \w    -67.00 -24.00   0.50    2.50    --    5.81 -38.00 -90.00   86
  3  \w     11.00  37.00   0.50    2.50    --    5.81 -99.00 -30.00   52
  4  \w    -57.00 -16.00   0.50    2.50    --   -4.71 -57.00 120.00   82
  5  \w     13.00  46.00   0.50    2.50    --    5.81-116.00 170.60   66
;
_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      0.0006450000
_diffrn_orient_matrix_UB_12      0.0014715000
_diffrn_orient_matrix_UB_13      -0.0372846000
_diffrn_orient_matrix_UB_21      0.0041604000
_diffrn_orient_matrix_UB_22      0.0713510000
_diffrn_orient_matrix_UB_23      0.0010498000
_diffrn_orient_matrix_UB_31      0.0470224000
_diffrn_orient_matrix_UB_32      -0.0062782000
_diffrn_orient_matrix_UB_33      0.0030237000
_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  0.0336
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20853
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.818
_diffrn_reflns_theta_min         2.460
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71106
_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    1.141
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         7128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0355P)^2^+0.4627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5501
_reflns_number_total             7128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03463a2.cif
_cod_data_source_block           ys250716_auto
_cod_depositor_comments
'Adding full bibliography for 1575458--1575459.cif.'
_cod_database_code               1575459
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni C30 H30 N4'
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.916
_diffrn_oxdiff_digest_hkl
;
43ce2f472105ce122acfe1c8dbe5a9813d6cf1
;
_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:
 C25(H25), C13(H13), C16(H16), C4(H4), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C5(H5a,H5b), C9(H9a,H9b), C6(H6a,H6b), C8(H8a,H8b), C7(H7a,H7b)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C20(H20), C12(H12), C21(H21)
2.d Idealised Me refined as rotating group:
 C27(H27a,H27b,H27c), C17(H17a,H17b,H17c), C26(H26a,H26b,H26c), C18(H18a,H18b,
 H18c), C15(H15a,H15b,H15c), C14(H14a,H14b,H14c), C24(H24a,H24b,H24c), C23(H23a,
 H23b,H23c)
;
_shelx_res_checksum              64269
_shelx_hkl_checksum              9835
_olex2_submission_original_sample_id Ys250716
_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 1.494
_oxdiff_exptl_absorpt_empirical_full_min 0.709