Synthetic, structural and reactivity studies of a boryl-ethynyl Silylene.
Chen, Wenhao; Hu, Haisheng; Feng, Jie; Zhu, Lei; Wu, Di; Chemical communications (Cambridge, England) 60 (2024) 5828–5831; doi:10.1039/d4cc00922c

data_7133025
_publ_section_title
;
 Synthetic, structural and reactivity studies of a boryl-ethynyl Silylene.
;
_journal_issue                   45
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5828
_journal_page_last               5831
_journal_paper_doi               10.1039/d4cc00922c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C43 H59 B N4 Si'
_chemical_formula_sum            'C43 H59 B N4 Si'
_chemical_formula_weight         670.84
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-02
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-05-02 deposited with the CCDC.	2024-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.635(2)
_cell_angle_beta                 90.829(2)
_cell_angle_gamma                106.097(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4740(4)
_cell_length_b                   13.9943(5)
_cell_length_c                   16.2737(6)
_cell_measurement_reflns_used    9437
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      2.54
_cell_volume                     2072.54(14)
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'zju Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43950
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.128
_diffrn_reflns_theta_min         1.980
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1441 before and 0.0464 after correction.
The Ratio of minimum to maximum transmission is 0.9675.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0099(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         9132
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0586P)^2^+0.6534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7782
_reflns_number_total             9132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00922c2.cif
_cod_data_source_block           220614_wd_fj0613_si
_cod_depositor_comments
'Adding full bibliography for 7133025--7133030.cif.'
_cod_original_cell_volume        2072.53(14)
_cod_database_code               7133025
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.965
_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. Restrained distances
 N4-C40 \\sim N4-C40A
 with sigma of 0.02
 C40-C43 \\sim C40A-C43A
 with sigma of 0.02
 C40-C42 \\sim C40A-C42A
 with sigma of 0.02
 C40-C41 \\sim C40A-C41A
 with sigma of 0.02
 N4-C43 \\sim N4-C43A
 with sigma of 0.04
 N4-C42 \\sim N4-C42A
 with sigma of 0.04
 N4-C41 \\sim N4-C41A
 with sigma of 0.04
 C43-C42 \\sim C43A-C42A
 with sigma of 0.04
 C43-C41 \\sim C43A-C41A
 with sigma of 0.04
 C42-C41 \\sim C42A-C41A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N4 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C40A \\sim C41A \\sim C42A
\\sim C43A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
4. Others
 Sof(C40A)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42A)=Sof(H42D)=
 Sof(H42E)=Sof(H42F)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(1)
 Sof(C40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C23(H23), C26(H26)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C19(H19), C20(H20), C21(H21),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C41A(H41D,H41E,
 H41F), C42A(H42D,H42E,H42F), C43A(H43D,H43E,H43F)
;
_olex2_submission_special_instructions 'No special instructions were received'