Synthesis, structure, and characterization of a novel heterocyclic organosilicon-quinone adduct
Ni, Congjian; Ma, Xiaoli; Yang, Zhi; New Journal of Chemistry 49 (2025) 13352–13356; doi:10.1039/D5NJ00982K

data_7063873
_publ_section_title
;
 Synthesis, structure, and characterization of a novel heterocyclic
 organosilicon-quinone adduct
;
_journal_issue                   31
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13352
_journal_page_last               13356
_journal_paper_doi               10.1039/D5NJ00982K
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C46 H46 Cl6 N8 O4 Si2'
_chemical_formula_sum            'C46 H46 Cl6 N8 O4 Si2'
_chemical_formula_weight         1043.79
_chemical_properties_physical    Air-sensitive
_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     dual
_audit_creation_date             2024-11-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-27 deposited with the CCDC.	2025-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                61.931(3)
_cell_angle_beta                 78.366(4)
_cell_angle_gamma                67.495(4)
_cell_formula_units_Z            1
_cell_length_a                   11.7808(15)
_cell_length_b                   14.0813(17)
_cell_length_c                   14.5520(18)
_cell_measurement_reflns_used    3548
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      21.801
_cell_measurement_theta_min      2.818
_cell_volume                     1967.2(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      150.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1144
_diffrn_reflns_av_unetI/netI     0.1317
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30921
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.586
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1216 before and 0.0646 after correction.
The Ratio of minimum to maximum transmission is 0.8897.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.881
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6920
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1623
_refine_ls_R_factor_gt           0.1011
_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^)+(0.1000P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2552
_refine_ls_wR_factor_ref         0.2926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3386
_reflns_number_total             6920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00982k2.cif
_cod_data_source_block           134
_cod_depositor_comments          'Adding full bibliography for 7063873.cif.'
_cod_database_code               7063873
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.964
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-C16 \\sim C18-C16
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C16, C18, C19, C21, C23, C25, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C24, C26, C20, C17, C28, C22, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C17)=Sof(C20)=Sof(H20)=Sof(C22)=Sof(H22)=Sof(C24)=Sof(H24)=Sof(C26)=
 Sof(H26)=Sof(C28)=Sof(H28)=1-FVAR(1)
 Sof(C18)=Sof(C19)=Sof(H19)=Sof(C21)=Sof(H21)=Sof(C23)=Sof(H23)=Sof(C25)=
 Sof(H25)=Sof(C27)=Sof(H27)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C21(H21), C23(H23), C25(H25), C27(H27), C20(H20), C22(H22),
 C24(H24), C26(H26), C28(H28)
5.b Fitted hexagon refined as free rotating group:
 C7(C6,C5,C4,C3,C8), C18(C19,C21,C23,C25,C27), C17(C20,C22,C24,C26,C28)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C10(H10A,H10B,H10C), C65(H65A,H65B,H65C), C15(H15A,H15B,
 H15C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              70471
_shelx_fab_checksum              26990
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'