Synthesis of SiN/SiS-heterocycles <i>via</i> the reactions of a bis-silylene with isocyanate/isothiocyanate molecules.
Liu, Rui; Mondal, Kartik Chandra; Wang, Chenfeng; Suthar, Sonam; Fang, Zijie; Zuo, Darui; Li, Yan; Chemical communications (Cambridge, England) 60 (2024) 1148–1151; doi:10.1039/d3cc04950g

data_7132552
_publ_section_title
;
 Synthesis of SiN/SiS-heterocycles <i>via</i> the reactions of a
 bis-silylene with isocyanate/isothiocyanate molecules.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1148
_journal_page_last               1151
_journal_paper_doi               10.1039/d3cc04950g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C32 H56 B10 N4 S2 Si2, 2(C6 H6)'
_chemical_formula_sum            'C44 H68 B10 N4 S2 Si2'
_chemical_formula_weight         881.42
_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             2022-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-09-20 deposited with the CCDC.	2023-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                76.297(4)
_cell_angle_beta                 82.378(4)
_cell_angle_gamma                61.662(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3084(13)
_cell_length_b                   13.6054(13)
_cell_length_c                   16.2398(16)
_cell_measurement_reflns_used    8024
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.36
_cell_volume                     2513.7(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'zju Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32305
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.375
_diffrn_reflns_theta_min         1.981
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1621 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.8465.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0543P)^2^+1.9720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7107
_reflns_number_total             9919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04950g2.cif
_cod_data_source_block           mo_220426_ly_lr0425_2_0m
_cod_depositor_comments
'Adding full bibliography for 7132552--7132556.cif.'
_cod_database_code               7132552
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.983
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C24(H24), C25(H25), C26(H26),
 C27(H27), C28(H28), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44)
2.b Fitted hexagon refined as free rotating group:
 C39(C40,C41,C42,C43,C44)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C)
2.d Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4), B5(H5), B6(H6), B7(H7), B8(H8), B9(H9A),
 B10(H10A)
;
_shelx_res_checksum              95036
_shelx_hkl_checksum              58485
_olex2_submission_special_instructions 'No special instructions were received'