Zirconium Hydrazides as Metallanitrene Synthons: Release of Molecular N2from a Hydrazinediido Complex Induced by Oxidative N–N Bond Cleavage
Gehrmann, Thorsten; Lloret-Fillol, Julio; Herrmann, Heike; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 32 (2013) 3877–; doi:10.1021/om400337g

data_4081013
_publ_section_title
;
 Zirconium Hydrazides as Metallanitrene Synthons: Release of Molecular
 N2from a Hydrazinediido Complex Induced by Oxidative N--N Bond Cleavage
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3877
_journal_paper_doi               10.1021/om400337g
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C21 H41 N3 O Si2 Zr'
_chemical_formula_weight         498.97
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_block_code                ga_hh29
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.6510(10)
_cell_angle_beta                 82.5520(10)
_cell_angle_gamma                68.1170(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4274(7)
_cell_length_b                   10.7564(7)
_cell_length_c                   13.5613(9)
_cell_measurement_temperature    100(2)
_cell_volume                     1295.58(15)
_computing_cell_refinement       'SAINT (Bruker AXS, 1997-2006)'
_computing_data_collection       'SMART (Bruker AXS, 1997-2003)'
_computing_data_reduction        'SAINT (Bruker AXS, 1997-2006)'
_computing_molecular_graphics    'PLATON (Spek, 1980-2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens, 1999-2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'CCD area detector (Bruker AXS Smart 1000)'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27185
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         32.22
_diffrn_reflns_theta_min         2.11
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004-2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         8477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.5689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                7910
_reflns_number_total             8477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400337g_si_002.cif
_cod_data_source_block           complex_7
_cod_database_code               4081013
_audit_block_refno               676