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_7132553
_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         'C48 H64 B10 F6 N6 O3 Si2'
_chemical_formula_sum            'C48 H64 B10 F6 N6 O3 Si2'
_chemical_formula_weight         1051.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-06-27
_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                 99.975(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.118(3)
_cell_length_b                   18.777(4)
_cell_length_c                   20.911(4)
_cell_measurement_reflns_used    6294
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.316
_cell_measurement_theta_min      2.191
_cell_volume                     5460(2)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'zju Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.0989
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40756
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.574
_diffrn_reflns_theta_min         1.949
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1648 before and 0.0918 after correction.
The Ratio of minimum to maximum transmission is 0.7630.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear reddish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       needle
_exptl_crystal_F_000             2200
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         12458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1969
_refine_ls_R_factor_gt           0.1204
_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^)+25.0302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7577
_reflns_number_total             12458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04950g2.cif
_cod_data_source_block           220525li_lidz236494_zcs_0m
_cod_depositor_comments
'Adding full bibliography for 7132552--7132556.cif.'
_cod_database_code               7132553
_shelx_shelxl_version_number     2018/3
_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:
 C27(H27), C38(H38), C28(H28), C36(H36), C24(H24), C25(H25), C41(H41),
 C40(H40), C39(H39), C8(H8), C12(H12), C5(H5), C1(H1A), C4(H4A), C11(H11),
 C9(H9A), C2(H2A), C10(H10A)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C18(H18A,H18B,H18C), C42(H42A,H42B,H42C), C35(H35A,
 H35B,H35C), C21(H21A,H21B,H21C), C15(H15A,H15B,H15C), C43(H43A,H43B,H43C),
 C32(H32A,H32B,H32C)
2.c Boron cage BH refined with riding coordinates:
 B1(H1), B4(H4), B8(H8A), B7(H7), B2(H2), B9(H9), B10(H10), B3(H3), B5(H5A),
 B6(H6)
;
_shelx_res_checksum              48807
_shelx_hkl_checksum              76550
_olex2_submission_special_instructions 'No special instructions were received'