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_4102750
_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 N2 O Si2 Zr2), C7 H7'
_chemical_formula_sum            'C89 H131 N4 O2 Si4 Zr4'
_chemical_formula_weight         1766.22
_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                68.060(4)
_cell_angle_beta                 80.456(6)
_cell_angle_gamma                69.609(5)
_cell_formula_units_Z            1
_cell_length_a                   10.9031(12)
_cell_length_b                   13.7960(16)
_cell_length_c                   16.365(2)
_cell_measurement_reflns_used    1630
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.38
_cell_measurement_theta_min      2.36
_cell_volume                     2138.5(4)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1409
_diffrn_reflns_av_sigmaI/netI    0.1703
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19489
_diffrn_reflns_theta_full        21.96
_diffrn_reflns_theta_max         21.96
_diffrn_reflns_theta_min         1.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  0.9857
_exptl_absorpt_correction_T_min  0.9444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             925
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         5146
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1629
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.2008
_reflns_number_gt                2643
_reflns_number_total             5146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja104025v_si_001_5.cif
_cod_data_source_block           djk23
_cod_database_code               4102750