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_7134965
_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      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     constr
_atom_sites_solution_secondary   constr
_audit_creation_date             2025-06-04
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-15 deposited with the CCDC.	2025-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.755(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8918(9)
_cell_length_b                   16.4124(7)
_cell_length_c                   11.5152(6)
_cell_measurement_reflns_used    58246
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      27.555
_cell_measurement_theta_min      3.07
_cell_volume                     3495.5(3)
_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    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      103.15
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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_unetI/netI     0.0755
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6334
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.070
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.994177
_exptl_absorpt_correction_T_min  0.983964
_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    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6334
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0840
_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^)+(0.1109P)^2^+7.0026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2148
_refine_ls_wR_factor_ref         0.2372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4695
_reflns_number_total             6334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04234h3.cif
_cod_data_source_block           sb110per3
_cod_depositor_comments
'Adding full bibliography for 7134962--7134969.cif.'
_cod_database_code               7134965
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.944
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.99106
 0.00894
2. Uiso/Uaniso restraints and constraints
Uanis(C27A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
3. Others
 Sof(C30B)=Sof(H30B)=Sof(C29B)=Sof(H29B)=Sof(H28A)=Sof(C27B)=Sof(H27B)=
 Sof(C26B)=Sof(H26B)=1-FVAR(1)
 Sof(H28)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C29A)=Sof(H29A)=
 Sof(C30A)=Sof(H30A)=FVAR(1)
 Sof(C36B)=Sof(H36B)=Sof(C35B)=Sof(H35B)=Sof(H34A)=Sof(C33B)=Sof(H33B)=
 Sof(C32B)=Sof(H32B)=1-FVAR(2)
 Sof(H34)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C35A)=Sof(H35A)=
 Sof(C36A)=Sof(H36A)=FVAR(2)
 Sof(C37B)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38B)=Sof(H38D)=Sof(H38E)=
 Sof(H38F)=Sof(C39B)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(3)
 Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38A)=Sof(H38A)=Sof(H38B)=
 Sof(H38C)=Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(3)
 Fixed Sof: C22A(0.65) H22A(0.65) H22B(0.65) H22C(0.65) C23A(0.65) H23A(0.65)
 H23B(0.65) H23C(0.65) C24A(0.65) H24A(0.65) H24B(0.65) H24C(0.65) C22B(0.35)
 H22D(0.35) H22E(0.35) H22F(0.35) C23B(0.35) H23D(0.35) H23E(0.35) H23F(0.35)
 C24B(0.35) H24D(0.35) H24E(0.35) H24F(0.35)
4.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), C30B(H30B), C29B(H29B), C28(H28), C28(H28A),
 C27B(H27B), C26B(H26B), C36B(H36B), C35B(H35B), C34(H34), C34(H34A),
 C33B(H33B), C32B(H32B), C26A(H26A), C27A(H27A), C29A(H29A), C30A(H30A),
 C32A(H32A), C33A(H33A), C35A(H35A), C36A(H36A)
4.b Fitted hexagon refined as free rotating group:
 C25(C30B,C29B,C28,C27B,C26B), C31(C36B,C35B,C34,C33B,C32B)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C22A(H22A,H22B,H22C), C23A(H23A,H23B,H23C), C24A(H24A,H24B,
 H24C), C37A(H37A,H37B,H37C), C38A(H38A,H38B,H38C), C39A(H39A,H39B,H39C),
 C22B(H22D,H22E,H22F), C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F), C37B(H37D,
 H37E,H37F), C38B(H38D,H38E,H38F), C39B(H39D,H39E,H39F)
;
_shelx_res_checksum              23811
_olex2_submission_special_instructions 'No special instructions were received'