Synthesis and characterization of the first neutral hexacoordinated silole complexes.
Szathmári, Balázs; Holczbauer, Tamás; Balterer, Bence; Domján, Attila; Volk, Balázs; Kovács, Ilona; Kelemen, Zsolt; Chemical communications (Cambridge, England) 61 (2025) 16042–16045; doi:10.1039/d5cc04234h

data_7134967
_publ_section_title
;
 Synthesis and characterization of the first neutral hexacoordinated
 silole complexes.
;
_journal_issue                   82
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              16042
_journal_page_last               16045
_journal_paper_doi               10.1039/d5cc04234h
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C38 H42 O2 Si3'
_chemical_formula_sum            'C38 H42 O2 Si3'
_chemical_formula_weight         614.98
_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     direct
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-07-15 deposited with the CCDC.	2025-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                78.610(5)
_cell_angle_beta                 82.780(6)
_cell_angle_gamma                76.832(5)
_cell_formula_units_Z            2
_cell_length_a                   9.5424(8)
_cell_length_b                   10.5382(8)
_cell_length_c                   18.3347(11)
_cell_measurement_reflns_used    88702
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      27.495
_cell_measurement_theta_min      3.025
_cell_volume                     1753.6(2)
_computing_cell_refinement       'Crystal Clear V.1.4.1 (Rigaku/MSC, 2007)'
_computing_data_collection       'Crystal Clear V.1.4.1 (Rigaku/MSC, 2007)'
_computing_data_reduction        'Crystal Clear V.1.4.1 (Rigaku/MSC, 2007)'
_computing_molecular_graphics
;
PLATON (Spek, 2009)
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_publication_material
;
PLATON (Spek, 2009)
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID II'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       RX
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            103452
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.542
_diffrn_reflns_theta_min         3.028
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.959400
_exptl_absorpt_correction_T_min  0.946428
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
T.Higashi, Numerical Absorption Correction, NUMABS, 2002
T.Higashi, Empirical Absorption Correction, 2001
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       chunk
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.550
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         8093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0411P)^2^+0.7586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7601
_reflns_number_total             8093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04234h3.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7134962--7134969.cif.'
_cod_database_code               7134967
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.914
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
1.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              88486