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_4063971
_publ_contact_author
;
Dittrich, Birger, Institute for Inorganic Chemistry,
Georg-August-University Goettingen, Tammannstr. 4,
D-37077 Goettingen, Germany.
;
_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_compound_source        ' Synthesis '
_chemical_formula_moiety         'C56 H68 N8 Si2, 2(C4 H8 O)'
_chemical_formula_sum            'C64 H84 N8 O2 Si2'
_chemical_formula_weight         1053.57
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 113.1287(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.7543(3)
_cell_length_b                   18.2098(4)
_cell_length_c                   13.9106(3)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.0
_cell_measurement_theta_min      3.75
_cell_volume                     2971.11(12)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2008)'
_computing_data_collection       'Apex2 (Bruker AXS, 2008)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_UB_11      2.8607631e-02
_diffrn_orient_matrix_UB_12      3.5793826e-02
_diffrn_orient_matrix_UB_13      5.9195384e-02
_diffrn_orient_matrix_UB_21      -7.8925155e-02
_diffrn_orient_matrix_UB_22      1.9871533e-02
_diffrn_orient_matrix_UB_23      -2.0521937e-02
_diffrn_orient_matrix_UB_31      -1.4873491e-02
_diffrn_orient_matrix_UB_32      -3.6601171e-02
_diffrn_orient_matrix_UB_33      4.6747878e-02
_diffrn_radiation_monochromator  'incoatec mirror optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5349
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.99
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.4698
_exptl_absorpt_correction_T_min  0.3964
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2008/2, multi-scan. (G. M. Sheldrick, 2008)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1136.0
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0484P)^2^+1.4174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                5319
_reflns_number_total             5349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101066w_si_001.cif
_cod_data_source_block           vana1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4063971