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_7134969
_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         'C Cl3 D, C38 H34 O4 Si'
_chemical_formula_sum            'C39 H34 Cl3 D O4 Si'
_chemical_formula_weight         703.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-07-15
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7308)
;
_audit_update_record
;
2025-07-15 deposited with the CCDC.	2025-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.6550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.05580(10)
_cell_length_b                   13.59260(10)
_cell_length_c                   23.50010(10)
_cell_measurement_reflns_used    58852
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9090
_cell_measurement_theta_min      3.2620
_cell_volume                     3445.73(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 42.58a 64-bit (release 31-05-2022))'
_computing_data_reduction        'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_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)'
_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 0.977
_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   -122.00 -29.00   0.50    0.05    --  -47.20  -9.00-152.00  186
  2  \w     25.00 120.00   0.50    0.05    --   47.20  77.00-180.00  190
  3  \w     25.00 120.00   0.50    0.05    --   47.20  77.00  30.00  190
  4  \w     25.00 120.00   0.50    0.05    --   47.20  77.00  60.00  190
  5  \w     25.00 120.00   0.50    0.05    --   47.20  77.00 -30.00  190
  6  \w     25.00 120.00   0.50    0.05    --   47.20  77.00-120.00  190
  7  \w     25.00  87.00   0.50    0.05    --   47.20  77.00 -90.00  124
  8  \w     29.00 122.00   0.50    0.05    --   47.20   9.00  21.00  186
  9  \w    -22.00  28.00   0.50    0.05    --  -47.20   9.00  21.00  100
 10  \w   -112.00 -26.00   0.50    0.05    --  -99.00 125.00  30.00  172
 11  \w     32.00 120.00   0.50    0.05    --   47.20  57.00 150.00  176
 12  \w     87.00 178.00   0.50    0.05    --  105.24   9.00  21.00  182
 13  \w     92.00 178.00   0.50    0.05    --  105.24  15.00 -30.00  172
 14  \w    -27.00  30.00   0.50    0.05    --   47.20 -19.00-120.00  114
 15  \w    -26.00  28.00   0.50    0.05    --   47.20  -9.00-152.00  108
 16  \w     33.00  75.00   0.50    0.05    --  105.24 -61.00-150.00   84
 17  \w     33.00  75.00   0.50    0.05    --  105.24 -61.00 -30.00   84
 18  \w     33.00  75.00   0.50    0.05    --  105.24 -61.00   0.00   84
 19  \w     33.00  75.00   0.50    0.05    --  105.24 -61.00  30.00   84
 20  \w     33.00  75.00   0.50    0.05    --  105.24 -61.00  60.00   84
 21  \w     19.00  95.00   0.50    0.05    --   47.20-125.00 120.00  152
 22  \w     33.00 112.00   0.50    0.05    --  105.24-125.00 150.00  158
 23  \w     33.00 105.00   0.50    0.05    --  105.24 -95.00 150.00  144
 24  \w     33.00 105.00   0.50    0.05    --  105.24 -95.00  60.00  144
 25  \w     33.00 105.00   0.50    0.05    --  105.24 -95.00 -60.00  144
 26  \w     33.00 105.00   0.50    0.05    --  105.24 -95.00-120.00  144
 27  \w     33.00 105.00   0.50    0.05    --  105.24 -95.00-180.00  144
 28  \w     19.00  95.00   0.50    0.05    --   47.20-125.00 -60.00  152
 29  \w   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00-180.00  192
 30  \w   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00 -90.00  192
 31  \w   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00  60.00  192
 32  \w   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00 150.00  192
 33  \w   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00  90.00  192
 34  \w   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00  30.00  192
 35  \w   -172.00 -82.00   0.50    0.05    --  -99.00 -61.00  90.00  180
 36  \w   -172.00 -82.00   0.50    0.05    --  -99.00 -61.00 120.00  180
 37  \w   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00   0.00  192
 38  \w   -174.00 -85.00   0.50    0.05    --  -99.00 -15.00 -60.00  178
 39  \w   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00-150.00  192
 40  \w   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00-120.00  192
 41  \w   -174.00 -81.00   0.50    0.05    --  -99.00  -9.00-152.00  186
 42  \w   -172.00 -82.00   0.50    0.05    --  -99.00 -61.00 -60.00  180
 43  \w   -174.00 -85.00   0.50    0.05    --  -99.00 -15.00 120.00  178
;
_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      -0.1071931000
_diffrn_orient_matrix_UB_12      -0.0055364000
_diffrn_orient_matrix_UB_13      -0.0542583000
_diffrn_orient_matrix_UB_21      -0.0942555000
_diffrn_orient_matrix_UB_22      0.0121366000
_diffrn_orient_matrix_UB_23      0.0390331000
_diffrn_orient_matrix_UB_31      0.0049789000
_diffrn_orient_matrix_UB_32      0.1125450000
_diffrn_orient_matrix_UB_33      -0.0068184000
_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  0.0410
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81206
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.440
_diffrn_reflns_theta_min         1.927
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.069
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.366
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.329
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 6320 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         13750
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0808P)^2^+0.7716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                13357
_reflns_number_total             13750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04234h3.cif
_cod_data_source_block           sb225kr2_auto
_cod_depositor_comments
'Adding full bibliography for 7134962--7134969.cif.'
_cod_database_code               7134969
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C38H34O4Si1
_cell_oxdiff_angle_alpha         90.0440(9)
_cell_oxdiff_angle_beta          102.6596(9)
_cell_oxdiff_angle_gamma         90.0244(9)
_cell_oxdiff_length_a            11.05505(12)
_cell_oxdiff_length_b            13.59327(16)
_cell_oxdiff_length_c            23.5009(2)
_cell_oxdiff_measurement_reflns_used 58852
_cell_oxdiff_volume              3445.73(7)
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.609(11)
 0.391(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 Cl5A-C78 \\sim Cl5B-C78
 with sigma of 0.02
 Cl4A-C78 \\sim Cl4B-C78
 with sigma of 0.02
 Cl3A-C77 \\sim Cl3B-C77
 with sigma of 0.02
 Cl1A-C77 \\sim Cl1B-C77
 with sigma of 0.02
4. Others
 Sof(D78A)=Sof(Cl4B)=Sof(Cl5B)=1-FVAR(1)
 Sof(D78)=Sof(Cl4A)=Sof(Cl5A)=FVAR(1)
 Sof(D77A)=Sof(Cl1B)=Sof(Cl3B)=1-FVAR(2)
 Sof(D77)=Sof(Cl1A)=Sof(Cl3A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C77(D77), C77(D77A), C78(D78), C78(D78A)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31),
  C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C44(H44),
 C50(H50), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61),
  C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68), C69(H69),
 C70(H70), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C52(H52A,H52B,
 H52C)
;
_shelx_res_checksum              99086
_ins_header
;
TITL SB225Kr2_auto in Pn 
REM Pn (#7 in standard setting)
CELL 1.54184  11.055795  13.592558  23.500131  90.0000 102.6548  90.0000
ZERR    5.00   0.000055   0.000077   0.000123   0.0000   0.0005   0.0000
LATT -1
SYMM  x+1/2,-y, z+1/2 
SFAC C H O Si
UNIT 190.00 170.00 20.00 5.00
REM  CrysAlisPro recorded range (K): Min=99.9; max=100.1; aver:100.0
TEMP -173
SIZE 0.20 0.33 0.35
TREF
HKLF 4
END
;
_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 1.868
_oxdiff_exptl_absorpt_empirical_full_min 0.566