Unprecedented bis(silylene)-supported silylone–metal complexes with Si0→ CuI, Si0→ NiI, and Si0→ NiII dative bonds
Shan, Changkai; Dai, Chenshu; Yao, Shenglai; Zhu, Jun; Driess, Matthias; Chemical Communications 61 (2025) 8875–8878; doi:10.1039/D5CC02098K

data_7134550
_publ_section_title
;
 Unprecedented bis(silylene)-supported silylone--metal complexes with
 Si0\\rightarrow CuI, Si0\\rightarrow NiI, and Si0\\rightarrow NiII dative
 bonds
;
_journal_issue                   49
_journal_name_full               'Chemical Communications'
_journal_page_first              8875
_journal_page_last               8878
_journal_paper_doi               10.1039/D5CC02098K
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C61 H97 B10 N6 Ni Si3, 2(C7 H8)'
_chemical_formula_sum            'C75 H113 B10 N6 Ni Si3'
_chemical_formula_weight         1349.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-05-02
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-02 deposited with the CCDC.	2025-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.870(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2917(4)
_cell_length_b                   15.5689(2)
_cell_length_c                   25.7309(4)
_cell_measurement_reflns_used    5990
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.5070
_cell_measurement_theta_min      3.5440
_cell_volume                     7779.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14261
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.496
_diffrn_reflns_theta_max         67.496
_diffrn_reflns_theta_min         3.590
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       prism
_exptl_crystal_F_000             2900
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         6912
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0783P)^2^+2.9488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5782
_reflns_number_total             6912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02098k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7134548--7134551.cif.'
_cod_database_code               7134550
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.798
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26-C21 \\sim C26B-C21
 with sigma of 0.02
 C27B-C26B \\sim C26-C27
 with sigma of 0.02
 C26-C28 \\sim C28B-C26B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C26 \\sim C28 \\sim C27: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C26B \\sim C28B \\sim C27B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Others
 Fixed Sof: C26(0.5) H26(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C28(0.5)
 H28A(0.5) H28B(0.5) H28C(0.5) C26B(0.5) H26B(0.5) C27B(0.5) H27D(0.5)
 H27E(0.5) H27F(0.5) C28B(0.5) H28D(0.5) H28E(0.5) H28F(0.5)
5.a Ternary CH refined with riding coordinates:
 C29(H29), C26(H26), C26B(H26B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C17(H17), C22(H22), C23(H23),
 C24(H24), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C27B(H27D,H27E,H27F), C28B(H28D,H28E,H28F), C32(H32A,H32B,H32C)
5.d Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4A), B5(H5A)
;
_shelx_res_checksum              68404
_shelx_hkl_checksum              54349
_olex2_submission_special_instructions 'No special instructions were received'