Studies into the Mechanism of CO-Induced N2 Cleavage Promoted by an Ansa-Hafnocene Complex and C-C Bond Formation from an Observed Intermediate
Donald J. Knobloch; Scott P. Semproni; Emil Lobkovsky; Paul J. Chirik; Journal of the American Chemical Society 134 (2012) 3377–3386; doi:10.1021/ja208562d

data_4117501
_publ_section_title
;
 Studies into the Mechanism of CO-Induced N2 Cleavage Promoted by an
 Ansa-Hafnocene Complex and C-C Bond Formation from an Observed
 Intermediate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3377
_journal_page_last               3386
_journal_paper_doi               10.1021/ja208562d
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C52 H78 Hf2 N4 O4 Si2'
_chemical_formula_weight         1236.34
_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                83.601(2)
_cell_angle_beta                 77.383(2)
_cell_angle_gamma                87.862(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2354(4)
_cell_length_b                   13.7569(4)
_cell_length_c                   20.0187(10)
_cell_measurement_reflns_used    9068
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.36
_cell_measurement_theta_min      3.24
_cell_volume                     3000.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26925
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         66.61
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    6.971
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The unit cell contained two molecules of toluene which
were treated as a diffuse contribution to the overall scattering
through the use of PLATON/SQUEEZE.
;
_refine_diff_density_max         1.328
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         9819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+1.8259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                8677
_reflns_number_total             9819
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja208562d_si_002_4.cif
_cod_data_source_block           sps58
_cod_database_code               4117501