Reduction Pathway of End-On Terminally Coordinated Dinitrogen. IV. Geometric, Electronic, and Vibrational Structure of a W(IV) Dialkylhydrazido Complex and Its Two-Electron-Reduced Derivative Undergoing N-N Cleavage upon Protonation
Kay H. Horn; Natascha Böres; Nicolai Lehnert; Klaus Mersmann; Christian Näther; Gerhard Peters; Felix Tuczek; Inorganic Chemistry 44 (2005) 3016–3030; doi:10.1021/ic048675g

data_1100715
_publ_contact_author_name        'Felix Tuczek'
_publ_section_title
;

Reduction Pathway of End-On Terminally Coordinated Dinitrogen. IV.

Geometric, Electronic, and Vibrational Structure of a W(IV)

Dialkylhydrazido Complex and Its Two-Electron-Reduced Derivative Undergoing

N-N Cleavage upon Protonation

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3016
_journal_page_last               3030
_journal_paper_doi               10.1021/ic048675g
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C57 H58 N2 P4 W'
_chemical_formula_weight         1078.79
_chemical_name_systematic
;

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;
_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                84.980(11)
_cell_angle_beta                 76.410(10)
_cell_angle_gamma                67.177(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6448(11)
_cell_length_b                   12.9364(12)
_cell_length_c                   16.7806(16)
_cell_measurement_reflns_used    7998
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      11.5
_cell_volume                     2459.2(4)
_computing_data_collection       'IPDS program package'
_computing_data_reduction        'IPDS program package'
_computing_molecular_graphics    'XP in SHELXTL-PC'
_computing_publication_material  'CIFTAB in SHELXL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       Phi-Scans
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16042
_diffrn_reflns_theta_full        24.94
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         2.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.519
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.944
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.0027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         8020
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                6467
_reflns_number_total             8020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048675gsi20040929_105115.cif
_cod_data_source_block           ja029735p
_cod_database_code               1100715