Synthesis and redox behavior of Si-Si dimeric 9-methylsilafluorene.
Wentz, Kelsie E.; Molino, Andrew; Jiang, George Q.; Siegler, Maxime A.; Wilson, David J. D.; Thoi, V. Sara; Klausen, Rebekka S.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6167–6173; doi:10.1039/d5dt00097a

data_7718324
_publ_section_title
;
 Synthesis and redox behavior of Si-Si dimeric 9-methylsilafluorene.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6167
_journal_page_last               6173
_journal_paper_doi               10.1039/d5dt00097a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C26 H22 Si2'
_chemical_formula_sum            'C26 H22 Si2'
_chemical_formula_weight         390.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-06-24 deposited with the CCDC.	2025-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.872(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.4395(8)
_cell_length_b                   14.6169(5)
_cell_length_c                   17.3824(7)
_cell_measurement_reflns_used    6031
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      70.0620
_cell_measurement_theta_min      5.1970
_cell_volume                     4316.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33758
_diffrn_reflns_point_group_measured_fraction_full 0.794
_diffrn_reflns_point_group_measured_fraction_max 0.787
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.880
_diffrn_reflns_theta_min         3.989
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.537
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.95a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       'small irregular plate'
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.058
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.013
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         6670
_refine_ls_number_restraints     1996
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0585P)^2^+0.8913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.573
_reflns_Friedel_fraction_full    0.588
_reflns_Friedel_fraction_max     0.574
_reflns_number_gt                5529
_reflns_number_total             6670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00097a3.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7718324.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7718324
_shelx_shelxl_version_number     2019/3
_oxdiff_exptl_absorpt_empirical_full_min 0.812
_oxdiff_exptl_absorpt_empirical_full_max 1.599
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_shelx_res_checksum              4622
_shelx_hkl_checksum              23288