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_7134548
_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         'C55 H85 B10 Cu N6 Si3'
_chemical_formula_sum            'C55 H85 B10 Cl0 Cu N6 Si3'
_chemical_formula_weight         1086.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                105.727(4)
_cell_angle_beta                 99.055(4)
_cell_angle_gamma                103.428(4)
_cell_formula_units_Z            2
_cell_length_a                   13.9122(6)
_cell_length_b                   14.0705(7)
_cell_length_c                   19.0390(9)
_cell_measurement_reflns_used    4995
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.4790
_cell_measurement_theta_min      3.3280
_cell_volume                     3391.3(3)
_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      150.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0570
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23490
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.494
_diffrn_reflns_theta_max         67.494
_diffrn_reflns_theta_min         3.360
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32318
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       prism
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         12068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0606P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8254
_reflns_number_total             12068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02098k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7134548--7134551.cif.'
_cod_database_code               7134548
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.782
_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.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C40(H40), C42(H42), C49(H49), C20(H20), C23(H23), C35(H35),
 C51(H51), C5(H5), C22(H22), C21(H21), C9(H9), C8(H8), C7(H7A), C6(H6A)
2.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C37(H37A,H37B,H37C), C28(H28A,H28B,H28C), C33(H33A,H33B,
 H33C), C44(H44A,H44B,H44C), C26(H26A,H26B,H26C), C54(H54A,H54B,H54C), C53(H53A,
 H53B,H53C), C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C30(H30A,H30B,H30C),
 C27(H27A,H27B,H27C), C45(H45A,H45B,H45C), C12(H12A,H12B,H12C), C46(H46A,H46B,
 H46C), C31(H31A,H31B,H31C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C55(H55A,
 H55B,H55C), C17(H17A,H17B,H17C)
2.c Boron cage BH refined with riding coordinates:
 B10(H10), B6(H6), B5(H5A), B1(H1), B9(H9A), B7(H7), B2(H2), B4(H4), B3(H3),
 B8(H8A)
;
_shelx_res_checksum              95118
_shelx_hkl_checksum              27548
_shelx_fab_checksum              8217
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'