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_4324792
_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         'C37 H54 N4 O4 Si'
_chemical_formula_sum            'C37 H54 N4 O4 Si'
_chemical_formula_weight         646.93
_space_group_IT_number           29
_symmetry_cell_setting           Pca21
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6931(14)
_cell_length_b                   12.1192(10)
_cell_length_c                   17.9703(15)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      24.866
_cell_measurement_theta_min      2.262
_cell_volume                     3635.5(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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      99(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Quazar mirror optics'
_diffrn_radiation_source         'INCOATEC Mo Microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            66985
_diffrn_reflns_theta_full        27.13
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.9648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         8037
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0384P)^2^+0.7268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                7612
_reflns_number_total             8037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102566c_si_003.cif
_cod_data_source_block           pca21
_cod_database_code               4324792