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_7134968
_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         'C58 H42 O4 Si, C4 H8 O, C2 H4 O0.25'
_chemical_formula_sum            'C64 H54 O5.25 Si'
_chemical_formula_weight         935.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 117.338(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.7640(3)
_cell_length_b                   14.74850(10)
_cell_length_c                   25.3341(3)
_cell_measurement_reflns_used    40565
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4840
_cell_measurement_theta_min      3.0450
_cell_volume                     9878.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -68.00 -26.00   0.50    0.26    --  -99.00  61.00  30.00   84
  2  \w    -51.00  25.00   0.50    0.07    --  -47.20  48.00  16.00  152
  3  \w    -68.00 -26.00   0.50    0.26    --  -99.00  61.00-150.00   84
  4  \w    -23.00  28.00   0.50    0.07    --  -47.20  19.00-180.00  102
  5  \w     25.00 120.00   0.50    0.07    --   47.20  77.00-150.00  190
  6  \w     34.00 120.00   0.50    0.07    --   47.20  48.00  16.00  172
  7  \w     25.00 120.00   0.50    0.07    --   47.20  77.00 -90.00  190
  8  \w     25.00 120.00   0.50    0.07    --   47.20  77.00  30.00  190
  9  \w     25.00 120.00   0.50    0.07    --   47.20  77.00  90.00  190
 10  \w     25.00 120.00   0.50    0.07    --   47.20  77.00 150.00  190
 11  \w     91.00 178.00   0.50    0.26    --  105.24  48.00  16.00  174
 12  \w     93.00 177.00   0.50    0.26    --  105.24  45.00 -60.00  168
 13  \w     93.00 178.00   0.50    0.26    --  105.24  30.00  90.00  170
 14  \w     93.00 178.00   0.50    0.26    --  105.24  30.00 150.00  170
 15  \w     33.00 105.00   0.50    0.26    --  105.24 -95.00   0.00  144
 16  \w     33.00 105.00   0.50    0.26    --  105.24 -95.00-150.00  144
 17  \w     19.00  95.00   0.50    0.07    --   47.20-125.00  60.00  152
 18  \w     33.00  99.00   0.50    0.26    --  105.24-125.00 120.00  132
 19  \w     33.00 105.00   0.50    0.26    --  105.24 -95.00 150.00  144
 20  \w     33.00  75.00   0.50    0.26    --  105.24 -61.00 120.00   84
 21  \w     33.00  75.00   0.50    0.26    --  105.24 -61.00 150.00   84
 22  \w     33.00  75.00   0.50    0.26    --  105.24 -61.00  60.00   84
 23  \w     33.00  75.00   0.50    0.26    --  105.24 -61.00  90.00   84
 24  \w     33.00  75.00   0.50    0.26    --  105.24 -61.00   0.00   84
 25  \w    -24.00  58.00   0.50    0.07    --   47.20 -48.00-131.00  164
 26  \w     33.00  75.00   0.50    0.26    --  105.24 -61.00 -90.00   84
 27  \w     33.00  75.00   0.50    0.26    --  105.24 -61.00-150.00   84
 28  \w     33.00  75.00   0.50    0.26    --  105.24 -61.00-120.00   84
 29  \w   -120.00 -74.00   0.50    0.07    --  -47.20-125.00 -60.00   92
 30  \w   -172.00 -82.00   0.50    0.26    --  -99.00 -61.00 -30.00  180
 31  \w   -120.00 -33.00   0.50    0.07    --  -47.20 -48.00-131.00  174
 32  \w   -172.00 -82.00   0.50    0.26    --  -99.00 -61.00-180.00  180
 33  \w   -171.00 -85.00   0.50    0.26    --  -99.00 -48.00-131.00  172
 34  \w   -171.00 -86.00   0.50    0.26    --  -99.00 -45.00 -90.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0506580000
_diffrn_orient_matrix_UB_12      0.0333322000
_diffrn_orient_matrix_UB_13      -0.0503149000
_diffrn_orient_matrix_UB_21      0.0108692000
_diffrn_orient_matrix_UB_22      -0.0518361000
_diffrn_orient_matrix_UB_23      -0.0457198000
_diffrn_orient_matrix_UB_31      -0.0266585000
_diffrn_orient_matrix_UB_32      -0.0843378000
_diffrn_orient_matrix_UB_33      0.0081721000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            74073
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.343
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       plate
_exptl_crystal_F_000             3952
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.246
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.049
_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     636
_refine_ls_number_reflns         9009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+14.2237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8185
_reflns_number_total             9009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04234h3.cif
_cod_data_source_block           sb223kr1_auto
_cod_depositor_comments
'Adding full bibliography for 7134962--7134969.cif.'
_cod_database_code               7134968
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C58H42O4Si1
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.731
_diffrn_oxdiff_digest_hkl
;
015ac2ba42180cfa92fbb5c770b4ce774ba49b
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: O69(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C70(H70A,H70B), C71(H71A,H71B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,
 H67B), C68(H68A,H68B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C4(H4), C27(H27), C57(H57), C17(H17), C26(H26), C21(H21), C51(H51),
 C53(H53), C25(H25), C41(H41), C23(H23), C33(H33), C45(H45), C19(H19), C44(H44),
  C24(H24), C56(H56), C20(H20), C50(H50), C63(H63), C43(H43), C54(H54),
 C18(H18), C55(H55), C47(H47), C49(H49), C32(H32), C31(H31), C59(H59), C42(H42),
  C35(H35), C29(H29), C37(H37), C48(H48), C39(H39), C62(H62), C30(H30),
 C61(H61), C38(H38), C60(H60), C36(H36)
;
_shelx_res_checksum              93258
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.835
_oxdiff_exptl_absorpt_empirical_full_min 0.649