Synthesis of a Lewis Base Stabilized Dimer of N-Substituted Hydrosila Hydrazone and a Silaaziridine
Sarish, Sankaranarayana Pillai; Jana, Anukul; Roesky, Herbert W.; Samuel, Prinson P.; Andrade, Carlos E. Abad; Dittrich, Birger; Schulzke, Carola; Organometallics 30 (2011) 912–; doi:10.1021/om101066w

data_4063969
_publ_section_title
;
 Synthesis of a Lewis Base Stabilized Dimer of N-Substituted Hydrosila
 Hydrazone and a Silaaziridine
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              912
_journal_paper_doi               10.1021/om101066w
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C28 H34 Cl N3 Si'
_chemical_formula_weight         476.12
_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                89.93(3)
_cell_angle_beta                 83.27(3)
_cell_angle_gamma                71.19(3)
_cell_formula_units_Z            4
_cell_length_a                   11.161(2)
_cell_length_b                   15.987(3)
_cell_length_c                   16.576(3)
_cell_measurement_reflns_used    25187
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      54.2
_cell_measurement_theta_min      3.6
_cell_volume                     2778.3(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  IPDSII
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0922
_diffrn_reflns_av_sigmaI/netI    0.1561
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25187
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  0.9419
_exptl_absorpt_correction_T_min  0.8358
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.096
_platon_squeeze_details
;
The SQUEEZE routine of the PLATON software resulted in an electron
count of 12 e per unit cell. This equals 0.24 molecules of 
toluene or 0.29 molecules of pentane per unit cell, which are the 
solvents used during synthesis and crystallization.
;
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         11991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1656
_refine_ls_R_factor_gt           0.0873
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1633
_reflns_number_gt                6516
_reflns_number_total             11991
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om101066w_si_001.cif
_cod_data_source_block           pp
_cod_original_cell_volume        2778.3(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063969