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_7132555
_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         'C50 H73.544 B10 N6 O2 S2 Si2, C7 H8, 1(C7 H7)'
_chemical_formula_sum            'C64 H88.54 B10 N6 O2 S2 Si2'
_chemical_formula_weight         1202.35
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-07-29
_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                112.618(3)
_cell_angle_beta                 101.299(3)
_cell_angle_gamma                100.144(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7410(10)
_cell_length_b                   17.4714(16)
_cell_length_c                   18.7329(18)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      27.180
_cell_measurement_theta_min      2.231
_cell_volume                     3341.5(5)
_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      170.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_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  0.0734
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            72755
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.319
_diffrn_reflns_theta_min         2.231
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1075 before and 0.0800 after correction.
The Ratio of minimum to maximum transmission is 0.8168.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       plate
_exptl_crystal_F_000             1281
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.512
_refine_diff_density_min         -2.102
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         14869
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.1110
_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^)+(0.1399P)^2^+9.8323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2895
_refine_ls_wR_factor_ref         0.3058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11670
_reflns_number_total             14869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04950g2.cif
_cod_data_source_block           mo_220628_ly_lr0622_1_0m
_cod_depositor_comments
'Adding full bibliography for 7132552--7132556.cif.'
_cod_database_code               7132555
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, {H32A,H32B} of C32, {H65C,H65D} of C65A, {H65A,H65B} of
  C65, {H24A,H24B} of C24, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H13D,H13E} of C13A
2. Uiso/Uaniso restraints and constraints
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C13A \\sim C14A \\sim C15A: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C65 \\sim C64A \\sim C63A
\\sim C62A \\sim C61A \\sim C60A \\sim C59A \\sim C65A: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
3. Others
 Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
 Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(S4A)=Sof(C17A)=1-FVAR(2)
 Sof(S4)=Sof(C17)=FVAR(2)
 Sof(C64A)=Sof(C63A)=Sof(H63A)=Sof(C62A)=Sof(H62A)=Sof(C61A)=Sof(H61A)=
 Sof(C60A)=Sof(H60A)=Sof(C59A)=Sof(H59A)=Sof(C65A)=Sof(H65C)=Sof(H65D)=1-FVAR(3)
 Sof(C64)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60)=Sof(C61)=Sof(H61)=Sof(C62)=
 Sof(H62)=Sof(C63)=Sof(H63)=Sof(C65)=Sof(H65A)=Sof(H65B)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C32(H32A,H32B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C19(H19), C20(H20), C22(H22),
 C23(H23), C27(H27), C28(H28), C30(H30), C31(H31), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
 C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C63A(H63A), C62A(H62A),
 C61A(H61A), C60A(H60A), C59A(H59A)
4.c Fitted hexagon refined as free rotating group:
 C64(C59,C60,C61,C62,C63), C64A(C63A,C62A,C61A,C60A,C59A)
4.d X=CH2 refined with riding coordinates:
 C65(H65A,H65B), C65A(H65C,H65D)
4.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C25(H25A,H25B,H25C),
 C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C14A(H14D,H14E,H14F),
 C15A(H15D,H15E,H15F), C58(H58A,H58B,H58C)
4.f Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4), B5(H5), B6(H6), B7(H7A), B8(H8A), B9(H9A),
 B10(H10A)
;
_shelx_res_checksum              81565
_shelx_hkl_checksum              52434
_olex2_submission_special_instructions 'No special instructions were received'