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_7133030
_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         'C47.987 H59 B F5 N5 Si'
_chemical_formula_sum            'C48 H59 B F5 N5 Si'
_chemical_formula_weight         839.90
_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             2024-04-09
_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
_cell_angle_beta                 103.424(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2831(16)
_cell_length_b                   10.4515(8)
_cell_length_c                   24.172(2)
_cell_measurement_reflns_used    7256
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.96
_cell_measurement_theta_min      2.44
_cell_volume                     4738.5(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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  0.1101
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            66249
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.398
_diffrn_reflns_theta_min         2.132
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1460 before and 0.0675 after correction.
The Ratio of minimum to maximum transmission is 0.9146.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       plate
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         10558
_refine_ls_number_restraints     966
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0590P)^2^+3.1402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6237
_reflns_number_total             10558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00922c2.cif
_cod_data_source_block           mo_220706_fj0704_sinf_0m
_cod_depositor_comments
'Adding full bibliography for 7133025--7133030.cif.'
_cod_original_cell_volume        4738.4(7)
_cod_database_code               7133030
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.964
_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
 Si1-F1 \\sim Si1A-F1A
 with sigma of 0.02
 C41-C43 \\sim C41A-C43A
 with sigma of 0.04
 Si1-C28 \\sim Si1A-C28
 with sigma of 0.02
 Si1-C44 \\sim Si1A-C44
 with sigma of 0.02
 F3-C46 \\sim F3A-C46A
 with sigma of 0.02
 N3-C30 \\sim N3A-C30A
 with sigma of 0.02
 C42-C41 \\sim C42A-C41A
 with sigma of 0.04
 F2-C45 \\sim F2A-C45A
 with sigma of 0.02
 N4-C40 \\sim N4A-C40A
 with sigma of 0.02
 N5-C48 \\sim N5-C48A
 with sigma of 0.04
 C29-C34 \\sim C29A-C34A
 with sigma of 0.02
 C34-C39 \\sim C34A-C39A
 with sigma of 0.02
 C34-C35 \\sim C34A-C35A
 with sigma of 0.02
 C39-C38 \\sim C39A-C38A
 with sigma of 0.02
 C30-C32 \\sim C30A-C32A
 with sigma of 0.02
 C30-C31 \\sim C30A-C31A
 with sigma of 0.02
 C30-C33 \\sim C30A-C33A
 with sigma of 0.02
 N5-C46 \\sim N5-C46A
 with sigma of 0.02
 F2-C44 \\sim F2A-C44
 with sigma of 0.04
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 C38-C37 \\sim C38A-C37A
 with sigma of 0.02
 C36-C37 \\sim C36A-C37A
 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
 C40-C43 \\sim C40A-C43A
 with sigma of 0.02
 C32-C33 \\sim C32A-C33A
 with sigma of 0.04
 C44-C48 \\sim C44-C48A
 with sigma of 0.02
 F5-C47 \\sim F5A-C47A
 with sigma of 0.04
 F4-C48 \\sim F4A-C48A
 with sigma of 0.04
 F3-N5 \\sim F3A-N5
 with sigma of 0.04
 C44-C46 \\sim C44-C46A
 with sigma of 0.04
 Si1-N3 \\sim Si1A-N3A
 with sigma of 0.04
 C35-C37 \\sim C35A-C37A
 with sigma of 0.04
 Si1-N4 \\sim Si1A-N4A
 with sigma of 0.04
 Si1-C29 \\sim Si1A-C29A
 with sigma of 0.04
 Si1-C34 \\sim Si1A-C34A
 with sigma of 0.04
 C38-C36 \\sim C38A-C36A
 with sigma of 0.04
 Si1-C30 \\sim Si1A-C30A
 with sigma of 0.04
 Si1-C40 \\sim Si1A-C40A
 with sigma of 0.04
 F1-N3 \\sim F1A-N3A
 with sigma of 0.04
 F1-N4 \\sim F1A-N4A
 with sigma of 0.04
 F1-C28 \\sim F1A-C28
 with sigma of 0.04
 F1-C29 \\sim F1A-C29A
 with sigma of 0.04
 F1-C44 \\sim F1A-C44
 with sigma of 0.04
 C42-C43 \\sim C42A-C43A
 with sigma of 0.04
 N3-N4 \\sim N3A-N4A
 with sigma of 0.04
 N3-C28 \\sim N3A-C28
 with sigma of 0.04
 N3-C29 \\sim N3A-C29A
 with sigma of 0.04
 N3-C44 \\sim N3A-C44
 with sigma of 0.04
 N3-C34 \\sim N3A-C34A
 with sigma of 0.04
 N3-C32 \\sim N3A-C32A
 with sigma of 0.04
 N3-C31 \\sim N3A-C31A
 with sigma of 0.04
 N3-C33 \\sim N3A-C33A
 with sigma of 0.04
 C32-C31 \\sim C32A-C31A
 with sigma of 0.04
 C31-C33 \\sim C31A-C33A
 with sigma of 0.04
 N4-C28 \\sim N4A-C28
 with sigma of 0.04
 N4-C29 \\sim N4A-C29A
 with sigma of 0.04
 N4-C44 \\sim N4A-C44
 with sigma of 0.04
 N4-C34 \\sim N4A-C34A
 with sigma of 0.04
 F5-C48 \\sim F5A-C48A
 with sigma of 0.02
 N4-C42 \\sim N4A-C42A
 with sigma of 0.04
 F4-C47 \\sim F4A-C47A
 with sigma of 0.02
 N4-C41 \\sim N4A-C41A
 with sigma of 0.04
 N4-C43 \\sim N4A-C43A
 with sigma of 0.04
 N5-C47 \\sim N5-C47A
 with sigma of 0.02
 C44-C45 \\sim C44-C45A
 with sigma of 0.02
 C45-C46 \\sim C45A-C46A
 with sigma of 0.02
 C48-C47 \\sim C48A-C47A
 with sigma of 0.02
 C28-C29 \\sim C28-C29A
 with sigma of 0.04
 F2-C46 \\sim F2A-C46A
 with sigma of 0.04
 C29-C44 \\sim C29A-C44
 with sigma of 0.04
 C29-C39 \\sim C29A-C39A
 with sigma of 0.04
 F5-C44 \\sim F5A-C44
 with sigma of 0.04
 C29-C30 \\sim C29A-C30A
 with sigma of 0.04
 C29-C35 \\sim C29A-C35A
 with sigma of 0.04
 F4-N5 \\sim F4A-N5
 with sigma of 0.04
 C29-C40 \\sim C29A-C40A
 with sigma of 0.04
 F3-C45 \\sim F3A-C45A
 with sigma of 0.04
 N5-C45 \\sim N5-C45A
 with sigma of 0.04
 C44-C47 \\sim C44-C47A
 with sigma of 0.04
 C34-C38 \\sim C34A-C38A
 with sigma of 0.04
 C34-C36 \\sim C34A-C36A
 with sigma of 0.04
 C39-C35 \\sim C39A-C35A
 with sigma of 0.04
 C39-C37 \\sim C39A-C37A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C28 \\sim Si1 \\sim F1 \\sim F2 \\sim F5 \\sim F4 \\sim N3 \\sim N4 \\sim F3
\\sim N5 \\sim C29 \\sim C44 \\sim C45 \\sim C34 \\sim C48 \\sim C47 \\sim C39
\\sim C30 \\sim C35 \\sim C46 \\sim C38 \\sim C36 \\sim C37 \\sim C40 \\sim C42
\\sim C41 \\sim C43 \\sim C32 \\sim C31 \\sim C33 \\sim Si1A \\sim F1A \\sim
N3A \\sim N4A \\sim C29A \\sim C34A \\sim C39A \\sim C30A \\sim C35A \\sim C38A
\\sim C36A \\sim C37A \\sim C40A \\sim C42A \\sim C41A \\sim C43A \\sim C32A
\\sim C31A \\sim C33A \\sim F2A \\sim F5A \\sim F4A \\sim F3A \\sim C45A \\sim
C48A \\sim C47A \\sim C46A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
4. Others
 Sof(Si1A)=Sof(F1A)=Sof(N3A)=Sof(N4A)=Sof(C29A)=Sof(C34A)=Sof(C39A)=Sof(H39A)=
 Sof(C38A)=Sof(H38A)=Sof(C37A)=Sof(H37A)=Sof(C36A)=Sof(H36A)=Sof(C35A)=
 Sof(H35A)=Sof(C30A)=Sof(C40A)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=
 Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C43A)=Sof(H43D)=Sof(H43E)=
 Sof(H43F)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C31A)=Sof(H31D)=
 Sof(H31E)=Sof(H31F)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(F2A)=Sof(F5A)=
 Sof(F4A)=Sof(F3A)=Sof(C45A)=Sof(C48A)=Sof(C47A)=Sof(C46A)=1-FVAR(1)
 Sof(Si1)=Sof(F1)=Sof(F2)=Sof(F5)=Sof(F4)=Sof(N3)=Sof(N4)=Sof(F3)=Sof(C29)=
 Sof(C45)=Sof(C34)=Sof(C48)=Sof(C47)=Sof(C39)=Sof(H39)=Sof(C30)=Sof(C35)=
 Sof(H35)=Sof(C38)=Sof(H38)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=Sof(C40)=
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C21(H21), C24(H24)
5.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C5(H5), C35(H35), C7(H7), C6(H6), C2(H2), C38(H38), C36(H36),
 C37(H37), C18(H18), C17(H17), C1(H1), C19(H19), C39A(H39A), C38A(H38A),
 C37A(H37A), C36A(H36A), C35A(H35A)
5.c Fitted hexagon refined as free rotating group:
 C34A(C39A,C38A,C37A,C36A,C35A)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C42(H42A,H42B,H42C), C41(H41A,H41B,H41C), C43(H43A,H43B,
 H43C), C14(H14A,H14B,H14C), C32(H32A,H32B,H32C), C11(H11A,H11B,H11C), C31(H31A,
 H31B,H31C), C33(H33A,H33B,H33C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C),
 C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C42A(H42D,H42E,
 H42F), C41A(H41D,H41E,H41F), C43A(H43D,H43E,H43F), C32A(H32D,H32E,H32F),
 C31A(H31D,H31E,H31F), C33A(H33D,H33E,H33F)
;
_olex2_submission_special_instructions 'No special instructions were received'