N-C Bond Formation Promoted by a Hafnocene Dinitrogen Complex: Comparison of Zirconium and Hafnium Congeners
Wesley H. Bernskoetter; Andrea V. Olmos; Jaime A. Pool; Emil Lobkovsky; Paul J. Chirik; Journal of the American Chemical Society 128 (2006) 10696–10697; doi:10.1021/ja064163k

data_4110829
_publ_section_title
;
 N-C Bond Formation Promoted by a Hafnocene Dinitrogen Complex: Comparison
 of Zirconium and Hafnium Congeners
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10696
_journal_page_last               10697
_journal_paper_doi               10.1021/ja064163k
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C50 H62 Hf2 N4 O2'
_chemical_formula_sum            'C50 H62 Hf2 N4 O2'
_chemical_formula_weight         1108.02
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.742(4)
_cell_angle_beta                 92.033(4)
_cell_angle_gamma                115.880(3)
_cell_formula_units_Z            2
_cell_length_a                   12.4523(8)
_cell_length_b                   14.1355(9)
_cell_length_c                   15.1817(16)
_cell_measurement_reflns_used    7372
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.82
_cell_measurement_theta_min      2.45
_cell_volume                     2330.4(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 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker 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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            82780
_diffrn_reflns_theta_full        33.95
_diffrn_reflns_theta_max         33.95
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    4.493
_exptl_absorpt_correction_T_max  0.8065
_exptl_absorpt_correction_T_min  0.3458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       plate
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.843
_refine_diff_density_min         -1.650
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         18441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.275
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                14021
_reflns_number_total             18441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064163ksi20060613_100146.cif
_cod_data_source_block           wb42
_cod_database_code               4110829