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_4111721
_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            'C36 H54 Cl2 N2 Zr2'
_chemical_formula_weight         768.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.766(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.7229(13)
_cell_length_b                   9.4395(5)
_cell_length_c                   17.1227(10)
_cell_measurement_reflns_used    9447
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.75
_cell_measurement_theta_min      2.35
_cell_volume                     3497.5(3)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker Apex2'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and 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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60955
_diffrn_reflns_theta_full        33.20
_diffrn_reflns_theta_max         33.20
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.9265
_exptl_absorpt_correction_T_min  0.7466
_exptl_absorpt_correction_type   'semiempirical by SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.278
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         13300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.243
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                10402
_reflns_number_total             13300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050387bsi20050325_083631.cif
_cod_data_source_block           wb15
_cod_database_code               4111721