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_7132556
_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 H71 B10 N6 O3 Si2, 2(C7 H8)'
_chemical_formula_sum            'C62 H87 B10 N6 O3 Si2'
_chemical_formula_weight         1128.65
_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             2022-04-27
_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                90
_cell_angle_beta                 90.955(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2822(7)
_cell_length_b                   20.2269(11)
_cell_length_c                   25.5456(13)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.49
_cell_volume                     6345.4(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0827
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            73787
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.940
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0788 before and 0.0579 after correction.
The Ratio of minimum to maximum transmission is 0.9139.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       block
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     944
_refine_ls_number_reflns         11616
_refine_ls_number_restraints     703
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+4.3364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8485
_reflns_number_total             11616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04950g2.cif
_cod_data_source_block           mo_220426_ly_lr0425_1_0m
_cod_depositor_comments
'Adding full bibliography for 7132552--7132556.cif.'
_cod_database_code               7132556
_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, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N6-C27 \\sim N6-C27A
 with sigma of 0.02
 O2-C32 \\sim O2A-C32A
 with sigma of 0.02
 O2-C33 \\sim O2A-C33A
 with sigma of 0.02
 C27-C32 \\sim C27A-C32A
 with sigma of 0.02
 C27-C28 \\sim C27A-C28A
 with sigma of 0.02
 C32-C31 \\sim C32A-C31A
 with sigma of 0.02
 C28-C29 \\sim C28A-C29A
 with sigma of 0.02
 C30-C29 \\sim C30A-C29A
 with sigma of 0.02
 C30-C31 \\sim C30A-C31A
 with sigma of 0.02
 N6-C32 \\sim N6-C32A
 with sigma of 0.04
 N6-C28 \\sim N6-C28A
 with sigma of 0.04
 O2-C27 \\sim O2A-C27A
 with sigma of 0.04
 O2-C31 \\sim O2A-C31A
 with sigma of 0.04
 C27-C29 \\sim C27A-C29A
 with sigma of 0.04
 C27-C31 \\sim C27A-C31A
 with sigma of 0.04
 C32-C28 \\sim C32A-C28A
 with sigma of 0.04
 C32-C30 \\sim C32A-C30A
 with sigma of 0.04
 C32-C33 \\sim C32A-C33A
 with sigma of 0.04
 C28-C30 \\sim C28A-C30A
 with sigma of 0.04
 C29-C31 \\sim C29A-C31A
 with sigma of 0.04
 C56-C57 \\sim C56A-C57A
 with sigma of 0.02
 C56-C61 \\sim C56A-C61A
 with sigma of 0.02
 C57-C58 \\sim C57A-C58A
 with sigma of 0.02
 C58-C59 \\sim C58A-C59A
 with sigma of 0.02
 C59-C60 \\sim C59A-C60A
 with sigma of 0.02
 C60-C61 \\sim C60A-C61A
 with sigma of 0.02
 C61-C62 \\sim C61A-C62A
 with sigma of 0.02
 C56-C58 \\sim C56A-C58A
 with sigma of 0.04
 C56-C60 \\sim C56A-C60A
 with sigma of 0.04
 C56-C62 \\sim C56A-C62A
 with sigma of 0.04
 C57-C59 \\sim C57A-C59A
 with sigma of 0.04
 C57-C61 \\sim C57A-C61A
 with sigma of 0.04
 C58-C60 \\sim C58A-C60A
 with sigma of 0.04
 C59-C61 \\sim C59A-C61A
 with sigma of 0.04
 C60-C62 \\sim C60A-C62A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C61A \\sim C57A \\sim C58A \\sim C59A \\sim C56A \\sim C60A \\sim C62A \\sim
C61 \\sim C56 \\sim C57 \\sim C58 \\sim C60 \\sim C62 \\sim C59: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C50A \\sim C49A \\sim C54A \\sim C53A \\sim C55A \\sim C51A \\sim H50A \\sim
C52A \\sim H51A \\sim H52A \\sim C54 \\sim C49 \\sim C53 \\sim C55 \\sim H49
\\sim C50 \\sim C52 \\sim H53 \\sim H55A \\sim H55B \\sim H55C \\sim H50 \\sim
C51 \\sim H52 \\sim H51: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C34 \\sim C39 \\sim C40 \\sim C44 \\sim C43 \\sim C41 \\sim C42: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C49A)=Sof(H49A)=Sof(C54A)=Sof(H54A)=Sof(C53A)=Sof(C52A)=Sof(H52A)=
 Sof(C51A)=Sof(H51A)=Sof(C50A)=Sof(H50A)=Sof(C55A)=Sof(H55D)=Sof(H55E)=
 Sof(H55F)=1-FVAR(1)
 Sof(C54)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=Sof(C52)=
 Sof(H52)=Sof(C53)=Sof(H53)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=FVAR(1)
 Sof(H6B)=Sof(O2A)=Sof(C27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=
 Sof(H30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(C33A)=Sof(H33D)=Sof(H33E)=
 Sof(H33F)=1-FVAR(2)
 Sof(H6A)=Sof(O2)=Sof(C27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=
 Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 FVAR(2)
 Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(H57A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=
 Sof(H59A)=Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(C62A)=Sof(H62D)=Sof(H62E)=
 Sof(H62F)=1-FVAR(3)
 Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=
 Sof(C60)=Sof(H60)=Sof(C61)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 N6(H6B), N6(H6A), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C20(H20),
 C21(H21), C22(H22), C23(H23), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
  C28(H28), C29(H29), C30(H30), C31(H31), C28A(H28A), C29A(H29A), C30A(H30A),
 C31A(H31A), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C56(H56),
 C57(H57), C58(H58), C59(H59), C60(H60), C49A(H49A), C54A(H54A), C52A(H52A),
 C51A(H51A), C50A(H50A), C56A(H56A), C57A(H57A), C58A(H58A), C59A(H59A),
 C60A(H60A)
5.b Fitted hexagon refined as free rotating group:
 C54(C49,C50,C51,C52,C53), C49A(C54A,C53A,C52A,C51A,C50A)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6C,H6D,H6E), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C33(H33A,H33B,H33C), C33A(H33D,H33E,H33F),
 C55(H55A,H55B,H55C), C62(H62A,H62B,H62C), C55A(H55D,H55E,H55F), C62A(H62D,H62E,
 H62F)
5.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              7525
_shelx_hkl_checksum              76132
_olex2_submission_special_instructions 'No special instructions were received'