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_4081009
_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            'C33 H51 I N4 Si2 Zr'
_chemical_formula_weight         778.08
_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     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_tg45
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.185(8)
_cell_angle_beta                 99.162(12)
_cell_angle_gamma                102.473(11)
_cell_formula_units_Z            2
_cell_length_a                   9.783(5)
_cell_length_b                   10.379(5)
_cell_length_c                   19.010(9)
_cell_measurement_reflns_used    8072
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.84
_cell_measurement_theta_min      2.34
_cell_volume                     1857.6(16)
_computing_cell_refinement
;
SAINT (Bruker AXS, 1997-2008). 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 (Bruker AXS, 1997-2008); SADABS (Bruker AXS, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al., 2004)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.922
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            45971
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         32.22
_diffrn_reflns_theta_min         2.01
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  0.9823
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.473
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.094
_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   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         12121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+1.1813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0713
_reflns_number_gt                10379
_reflns_number_total             12121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400337g_si_002.cif
_cod_data_source_block           complex_2
_cod_original_cell_volume        1857.5(16)
_cod_database_code               4081009
_audit_block_refno               1176