Facile synthesis of 1-silaacenaphthenes by transition metal-catalyzed intramolecular C(sp3)–H silylation
Mu, Delong; Zhu, Xinrui; Chen, Jiean; Chemical Communications 61 (2025) 7073–7076; doi:10.1039/D5CC00967G

data_7134382
_publ_section_title
;
 Facile synthesis of 1-silaacenaphthenes by transition metal-catalyzed
 intramolecular C(sp3)--H silylation
;
_journal_issue                   39
_journal_name_full               'Chemical Communications'
_journal_page_first              7073
_journal_page_last               7076
_journal_paper_doi               10.1039/D5CC00967G
_journal_volume                  61
_journal_year                    2025
_chemical_formula_sum            'C23 H18 Si'
_chemical_formula_weight         322.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-09-10 deposited with the CCDC.	2025-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.17670(10)
_cell_length_b                   12.3479(2)
_cell_length_c                   23.1083(3)
_cell_measurement_temperature    302(2)
_cell_volume                     1752.07(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      302(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.973
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20999
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.902
_diffrn_reflns_theta_min         3.848
_exptl_absorpt_coefficient_mu    1.153
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_F_000             680
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       0.0018(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0608P)^2^+0.4015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3360
_reflns_number_total             3597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00967g2.cif
_cod_data_source_block           yh253mdl0452_auto
_cod_depositor_comments          'Adding full bibliography for 7134382.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7134382
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              21267
_shelx_hkl_checksum              70541