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_7132554
_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         'C40 H63 B10 N5 O3 Si2'
_chemical_formula_sum            'C40 H63 B10 N5 O3 Si2'
_chemical_formula_weight         826.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-07
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-09-20 deposited with the CCDC.	2023-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.210(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.922(5)
_cell_length_b                   17.399(8)
_cell_length_c                   21.674(8)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      27.093
_cell_measurement_theta_min      2.269
_cell_volume                     4724(3)
_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      170.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            52696
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.078
_diffrn_reflns_theta_min         2.087
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0820 before and 0.0609 after correction.
The Ratio of minimum to maximum transmission is 0.9482.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'whiteish colourless'
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         10383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0435P)^2^+2.1968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7851
_reflns_number_total             10383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04950g2.cif
_cod_data_source_block           mo_220506_ly_lr0505_1_0m
_cod_depositor_comments
'Adding full bibliography for 7132552--7132556.cif.'
_cod_database_code               7132554
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.991
_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:
 C20(H20), C16(H16), C33(H33), C29(H29), C19(H19), C18(H18), C6(H6), C3(H3),
 C17(H17), C2(H2), C30(H30), C1(H1), C32(H32), C31(H31)
2.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C39(H39A,H39B,
 H39C), C28(H28A,H28B,H28C), C36(H36A,H36B,H36C), C26(H26A,H26B,H26C), C22(H22A,
 H22B,H22C), C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C7(H7A,H7B,H7C), C13(H13A,H13B,H13C)
2.c Boron cage BH refined with riding coordinates:
 B8(H8), B5(H5), B1(H1A), B9(H9), B10(H10), B4(H4), B7(H7), B6(H6A), B3(H3A),
 B2(H2A)
;
_shelx_res_checksum              79009
_shelx_hkl_checksum              38601
_olex2_submission_special_instructions 'No special instructions were received'