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_4110830
_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         'C57 H67 Hf2 N5 O3'
_chemical_formula_sum            'C57 H67 Hf2 N5 O3'
_chemical_formula_weight         1227.14
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.829(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.6159(16)
_cell_length_b                   22.4276(15)
_cell_length_c                   10.8063(7)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.33
_cell_measurement_theta_min      2.38
_cell_volume                     5442.3(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            61103
_diffrn_reflns_theta_full        25.48
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    3.858
_exptl_absorpt_correction_T_max  0.8305
_exptl_absorpt_correction_T_min  0.5125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.406
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         10074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.088
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+14.3274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                7588
_reflns_number_total             10074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064163ksi20060613_100204.cif
_cod_data_source_block           wb40
_cod_database_code               4110830