Addition of Methyl Triflate to a Hafnocene Dinitrogen Complex: Stepwise N2 Methylation and Conversion to a Hafnocene Hydrazonato Compound
Donald J. Knobloch; David Benito-Garagorri; Wesley H. Bernskoetter; Ivan Keresztes; Emil Lobkovsky; Hannah Toomey; Paul J. Chirik; Journal of the American Chemical Society 131 (2009) 14903–14912; doi:10.1021/ja904436a

data_4105143
_publ_section_title
;
 Addition of Methyl Triflate to a Hafnocene Dinitrogen Complex: Stepwise
 N2 Methylation and Conversion to a Hafnocene Hydrazonato Compound
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14903
_journal_page_last               14912
_journal_paper_doi               10.1021/ja904436a
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C37 H55 Hf2 I N2'
_chemical_formula_sum            'C37 H55 Hf2 I N2'
_chemical_formula_weight         1011.71
_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                76.576(7)
_cell_angle_beta                 67.489(7)
_cell_angle_gamma                76.621(7)
_cell_formula_units_Z            1
_cell_length_a                   8.6689(13)
_cell_length_b                   10.3474(14)
_cell_length_c                   10.8645(16)
_cell_measurement_reflns_used    2457
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     864.6(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0636
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14322
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    6.920
_exptl_absorpt_correction_T_max  0.9033
_exptl_absorpt_correction_T_min  0.5445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3509
_refine_ls_number_restraints     263
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.598
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+9.7429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                2861
_reflns_number_total             3509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja904436a_si_001.cif
_cod_data_source_block           wb46
_cod_database_code               4105143