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_4117500
_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_moiety         'C42 H60 Hf2 N2 O3 Si2, 0.5(C6 H6)'
_chemical_formula_sum            'C45 H63 Hf2 N2 O3 Si2'
_chemical_formula_weight         1093.13
_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                85.677(3)
_cell_angle_beta                 87.437(3)
_cell_angle_gamma                68.155(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3309(7)
_cell_length_b                   10.2407(8)
_cell_length_c                   24.575(2)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      36.49
_cell_measurement_theta_min      2.48
_cell_volume                     2173.1(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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            37372
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.870
_exptl_absorpt_correction_T_max  0.6416
_exptl_absorpt_correction_T_min  0.3228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       block
_exptl_crystal_F_000             1086
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         13133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0169P)^2^+1.1450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0414
_refine_ls_wR_factor_ref         0.0440
_reflns_number_gt                11318
_reflns_number_total             13133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja208562d_si_002_3.cif
_cod_data_source_block           djk33
_cod_database_code               4117500