Synthesis, characterization, and thermal properties of volatile 1,4-dialkyl-5-silatetrazolines: nitrogen-rich silicon heterocycles as possible CVD precursors for silicon nitride.
Flores, Vincent J.; Girolami, Gregory S.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9399–9404; doi:10.1039/d4dt03473b

data_7718303
_publ_section_title
;
 Synthesis, characterization, and thermal properties of volatile
 1,4-dialkyl-5-silatetrazolines: nitrogen-rich silicon heterocycles as
 possible CVD precursors for silicon nitride.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9399
_journal_page_last               9404
_journal_paper_doi               10.1039/d4dt03473b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C18 H38 N6 Si'
_chemical_formula_sum            'C18 H38 N6 Si'
_chemical_formula_weight         366.63
_chemical_name_common
1,4-Di(tert-butyl)-1,4-diazabut-2-ene-1,4-diyl][1,4-di(iso-propyl)tetraaz-2-ene-1,4-diyl]silane
_chemical_name_systematic
6,9-Di-tert-butyl-1,4-di(iso-propyl)-1,2,3,4,6,9-hexaaza-5-silaspiro[4.4]nona-2,7-diene
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-02-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-12 deposited with the CCDC.	2025-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8746(7)
_cell_length_b                   11.8697(7)
_cell_length_c                   13.0995(7)
_cell_measurement_reflns_used    7230
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.26
_cell_volume                     2157.3(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13096
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         2.258
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1505 before and 0.0522 after correction.
The Ratio of minimum to maximum transmission is 0.9156.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.624
_exptl_crystal_size_min          0.214
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0433P)^2^+1.6806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1328
_reflns_number_total             1459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03473b2.cif
_cod_data_source_block           practice_ditertbutyl_sila
_cod_depositor_comments
'Adding full bibliography for 7718302--7718304.cif.'
_cod_database_code               7718303
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H3A(0.5) H3B(0.5) H3C(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              43558
_shelx_hkl_checksum              74537
_olex2_submission_special_instructions 'No special instructions were received'