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_4081010
_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            'C39 H56 N4 S Si2 Zr'
_chemical_formula_weight         760.34
_chemical_properties_physical    air-sensitive
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_tg14
_audit_creation_method           SHELXL-97
_audit_update_record             'Mon Nov 12 18:16:57 CET 2012'
_cell_angle_alpha                86.117(6)
_cell_angle_beta                 87.819(6)
_cell_angle_gamma                77.450(13)
_cell_formula_units_Z            2
_cell_length_a                   9.582(5)
_cell_length_b                   10.413(5)
_cell_length_c                   20.309(10)
_cell_measurement_temperature    100(2)
_cell_volume                     1972.9(17)
_computing_cell_refinement
;
SAINT 8.x (Bruker AXS, 1997-2011). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT 8.x (Bruker AXS, 1997-2011)'
_computing_publication_material
'encif (Wadepohl, 2012); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF (Beurskens et al., 1999-2008)'
_diffrn_ambient_environment      'perfluoro polyether oil'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_av_sigmaI/netI    0.0744
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            58995
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         2.01
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  0.745686
_exptl_absorpt_correction_T_min  0.615643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         17175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+12.8084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1580
_reflns_number_gt                13483
_reflns_number_total             17175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400337g_si_002.cif
_cod_data_source_block           complex_4a
_cod_database_code               4081010
_audit_block_refno               847