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_4111720
_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 I2 N2 Zr2'
_chemical_formula_weight         951.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.166(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.638(2)
_cell_length_b                   21.033(5)
_cell_length_c                   18.755(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3702.0(14)
_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 0.884
_diffrn_measured_fraction_theta_max 0.884
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51943
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    2.257
_exptl_absorpt_correction_T_max  0.6023
_exptl_absorpt_correction_T_min  0.3982
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.867
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         12478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.165
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+1.2214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                9591
_reflns_number_total             12478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050387bsi20050325_083617.cif
_cod_data_source_block           jd29
_cod_original_cell_volume        3701.8(14)
_cod_database_code               4111720