Double N-H bond activation of N,N'-bis-substituted hydrazines with stable N-heterocyclic silylene.
Azhakar, Ramachandran; Ghadwal, Rajendra S.; Roesky, Herbert W.; Hey, Jakob; Stalke, Dietmar; Dalton transactions (Cambridge, England : 2003) 41 (2012) 1529–1533; doi:10.1039/c1dt11708d

data_7017944
_publ_section_title
;
 Double N-H bond activation of N,N'-bis-substituted hydrazines with stable
 N-heterocyclic silylene.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1529
_journal_page_last               1533
_journal_paper_doi               10.1039/c1dt11708d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C33 H48 N4 O2 Si'
_chemical_formula_sum            'C33 H48 N4 O2 Si'
_chemical_formula_weight         560.84
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   13.816(2)
_cell_length_b                   14.387(2)
_cell_length_c                   15.751(3)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.082
_cell_measurement_theta_min      2.419
_cell_volume                     3130.8(9)
_computing_cell_refinement       'SAINT V7.60A'
_computing_data_collection       'APEX2 v2010.11-3'
_computing_data_reduction        'SAINT V7.60A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II with D8'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'INCOATEC I\mS microfocus source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26322
_diffrn_reflns_theta_full        27.13
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.9956
_exptl_absorpt_correction_T_min  0.9891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6906
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0521P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                6198
_reflns_number_total             6906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11708d.txt
_cod_data_source_block           p212121
_cod_original_sg_symbol_H-M      'P21 21 21'
_cod_database_code               7017944