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_7718304
_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         'C16 H34 N6 Si'
_chemical_formula_sum            'C16 H34 N6 Si'
_chemical_formula_weight         338.58
_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      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                93.0697(15)
_cell_angle_beta                 97.2334(17)
_cell_angle_gamma                90.9204(16)
_cell_formula_units_Z            2
_cell_length_a                   8.9917(4)
_cell_length_b                   10.0564(4)
_cell_length_c                   11.0337(4)
_cell_measurement_reflns_used    12553
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.68
_cell_volume                     988.09(7)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24544
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.435
_diffrn_reflns_theta_min         2.284
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       plate
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         8049
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0393P)^2^+0.2668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.981
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                7539
_reflns_number_total             8049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03473b2.cif
_cod_data_source_block           isopropylsilatetrazene
_cod_depositor_comments
'Adding full bibliography for 7718302--7718304.cif.'
_cod_database_code               7718304
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.981
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(12)
 0.48(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C27(H27), C30(H30)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C17(H17), C18(H18)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C)
;
_shelx_res_checksum              29088
_shelx_hkl_checksum              73600
_olex2_submission_special_instructions 'No special instructions were received'