Formation of Silicon Centered Spirocyclic Compounds: Reaction of N-Heterocyclic Stable Silylene with Benzoylpyridine, Diisopropyl Azodicarboxylate, and 1,2-Diphenylhydrazine
Ramachandran Azhakar; Sankaranarayana Pillai Sarish; Gašper Tavčar; Herbert W. Roesky; Jakob Hey; Dietmar Stalke; Debasis Koley; Inorganic Chemistry 50 (2011) 3028–3036; doi:10.1021/ic102566c

data_4324793
_publ_section_title
;
 Formation of Silicon Centered Spirocyclic Compounds: Reaction of
 N-Heterocyclic Stable Silylene with Benzoylpyridine, Diisopropyl
 Azodicarboxylate, and 1,2-Diphenylhydrazine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3028
_journal_page_last               3036
_journal_paper_doi               10.1021/ic102566c
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C41 H50 N4 Si'
_chemical_formula_sum            'C41 H50 N4 Si'
_chemical_formula_weight         626.94
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.357(3)
_cell_angle_beta                 93.727(3)
_cell_angle_gamma                90.731(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9890(17)
_cell_length_b                   12.566(2)
_cell_length_c                   12.909(2)
_cell_measurement_reflns_used    2031
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      21.217
_cell_measurement_theta_min      2.218
_cell_volume                     1777.1(5)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2008.11'
_computing_data_reduction        'SAINT V7.46A'
_computing_molecular_graphics    'XP in SHELXTL Version 2008/3'
_computing_publication_material  'XP in SHELXTL Version 2008/3'
_computing_structure_refinement  'SHELXL in SHELXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/3'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II Ultra'
_diffrn_measurement_method       'omega scans and phi scans'
_diffrn_radiation_monochromator  'INCOATEC Helios mirror optics'
_diffrn_radiation_source         'Bruker TXS-Mo rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29684
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.9276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6480
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.5671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                4992
_reflns_number_total             6480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102566c_si_004.cif
_cod_data_source_block           p-1
_cod_database_code               4324793