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_4070314
_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            'C42 H52 N4 Si'
_chemical_formula_weight         640.97
_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                78.93(3)
_cell_angle_beta                 84.21(3)
_cell_angle_gamma                77.19(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2397(18)
_cell_length_b                   12.543(3)
_cell_length_c                   16.134(3)
_cell_measurement_reflns_used    15866
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      53.9
_cell_measurement_theta_min      3.4
_cell_volume                     1786.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15866
_diffrn_reflns_theta_full        26.96
_diffrn_reflns_theta_max         26.96
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.8938
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         7665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0608P)^2^+0.5195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                6863
_reflns_number_total             7665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9007086_si_001.cif
_cod_data_source_block           ja58
_cod_original_cell_volume        1786.1(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070314