Dinitrogen Functionalization with Terminal Alkynes, Amines, and Hydrazines Promoted by [(η5-C5Me4H)2Zr]2(μ2,η2,η2-N2): Observation of Side-On and End-On Diazenido Complexes in the Reduction of N2 to Hydrazine
Wesley H. Bernskoetter; Jaime A. Pool; Emil Lobkovsky; Paul J. Chirik; Journal of the American Chemical Society 127 (2005) 7901–7911; doi:10.1021/ja050387b

data_4111722
_publ_section_title
;
 Dinitrogen Functionalization with Terminal Alkynes, Amines, and
 Hydrazines Promoted by [(\h5-C5Me4H)2Zr]2(\m2,\h2,\h2-N2): Observation of
 Side-On and End-On Diazenido Complexes in the Reduction of N2 to
 Hydrazine
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7901
_journal_page_last               7911
_journal_paper_doi               10.1021/ja050387b
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C19 H27 F3 N O3 S Zr'
_chemical_formula_weight         497.70
_chemical_name_systematic
; 
 ? 
;
_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   mi
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.160(1)
_cell_angle_beta                 65.265(1)
_cell_angle_gamma                71.607(1)
_cell_formula_units_Z            2
_cell_length_a                   10.2470(4)
_cell_length_b                   10.4473(5)
_cell_length_c                   11.0073(5)
_cell_measurement_reflns_used    7332
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.69
_cell_measurement_theta_min      2.37
_cell_volume                     1014.96(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.661
_diffrn_measured_fraction_theta_max 0.661
_diffrn_measurement_device_type  'Bruker 1K CCD area detector'
_diffrn_measurement_method       '0.3 deg. omega 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  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9282
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.9796
_exptl_absorpt_correction_T_min  0.9662
_exptl_absorpt_correction_type   'semiempirical by SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             510
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.231
_refine_ls_shift/su_mean         0.014
_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          0.1047
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                3336
_reflns_number_total             4098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050387bsi20050325_083646.cif
_cod_data_source_block           wb7
_cod_database_code               4111722