Carbon Monoxide-Induced Dinitrogen Cleavage with Group 4 Metallocenes: Reaction Scope and Coupling to N-H Bond Formation and CO Deoxygenation
Donald J. Knobloch; Emil Lobkovsky; Paul J. Chirik; Journal of the American Chemical Society 132 (2010) 10553–10564; doi:10.1021/ja104025v

data_4102749
_publ_section_title
;
 Carbon Monoxide-Induced Dinitrogen Cleavage with Group 4 Metallocenes:
 Reaction Scope and Coupling to N-H Bond Formation and CO Deoxygenation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10553
_journal_page_last               10564
_journal_paper_doi               10.1021/ja104025v
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         '2(C41 H62 Hf2 N2 O Si2), C7 H7'
_chemical_formula_sum            'C89 H131 Hf4 N4 O2 Si4'
_chemical_formula_weight         2115.30
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.975(2)
_cell_angle_beta                 79.535(2)
_cell_angle_gamma                68.141(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9609(6)
_cell_length_b                   13.9203(7)
_cell_length_c                   16.4943(9)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.36
_cell_volume                     2147.8(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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36239
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.921
_exptl_absorpt_correction_T_max  0.9080
_exptl_absorpt_correction_T_min  0.6389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1053
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.676
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         10582
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+1.2183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0502
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                7762
_reflns_number_total             10582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja104025v_si_001_4.cif
_cod_data_source_block           djk24
_cod_database_code               4102749