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_4117498
_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 O2 Si2'
_chemical_formula_sum            'C42 H60 Hf2 N2 O2 Si2'
_chemical_formula_weight         1038.08
_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                95.947(3)
_cell_angle_beta                 107.780(3)
_cell_angle_gamma                97.433(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2531(6)
_cell_length_b                   13.9891(9)
_cell_length_c                   15.2353(9)
_cell_measurement_reflns_used    9288
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.37
_cell_volume                     2039.5(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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41113
_diffrn_reflns_theta_full        28.52
_diffrn_reflns_theta_max         28.52
_diffrn_reflns_theta_min         1.89
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.182
_exptl_absorpt_correction_T_max  0.7817
_exptl_absorpt_correction_T_min  0.2642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       block
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         10092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0111P)^2^+4.0632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0539
_reflns_number_gt                8574
_reflns_number_total             10092
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja208562d_si_002_1.cif
_cod_data_source_block           djk29
_cod_database_code               4117498