Insertion Reaction of a Silylene into a N−H Bond of Hydrazine and a [1+4] Cycloaddition with Diphenyl Hydrazone§
Jana, Anukul; Roesky, Herbert W.; Schulzke, Carola; Samuel, Prinson P.; Organometallics 28 (2009) 6574–; doi:10.1021/om9007086

data_4070313
_publ_section_title
;
 Insertion Reaction of a Silylene into a N&#x2212;H Bond of Hydrazine and
 a [1+4] Cycloaddition with Diphenyl Hydrazone&#x00A7;
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6574
_journal_paper_doi               10.1021/om9007086
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C29 H44 N4 Si'
_chemical_formula_weight         476.77
_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                 97.53(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.574(2)
_cell_length_b                   20.188(4)
_cell_length_c                   12.598(3)
_cell_measurement_reflns_used    25210
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      51.9
_cell_measurement_theta_min      3.3
_cell_volume                     2918.2(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0704
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24687
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.9732
_exptl_absorpt_correction_T_min  0.9428
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0696P)^2^+0.4403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                3837
_reflns_number_total             5679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9007086_si_001.cif
_cod_data_source_block           ja55
_cod_original_cell_volume        2918.3(10)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4070313