Mechanistic Elucidation of Intramolecular Aminoalkene Hydroamination Catalyzed by a Tethered Bis(ureate) Complex: Evidence for Proton-Assisted C-N Bond Formation at Zirconium
David C. Leitch; Rachel H. Platel; Laurel L. Schafer; Journal of the American Chemical Society 133 (2011) 15453–15463; doi:10.1021/ja202448b

data_4106857
_publ_section_title
;
 Mechanistic Elucidation of Intramolecular Aminoalkene Hydroamination
 Catalyzed by a Tethered Bis(ureate) Complex: Evidence for Proton-Assisted
 C-N Bond Formation at Zirconium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15453
_journal_page_last               15463
_journal_paper_doi               10.1021/ja202448b
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C64 H104 N12 O4 Zr2'
_chemical_formula_sum            'C64 H104 N12 O4 Zr2'
_chemical_formula_weight         1288.03
_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                63.414(4)
_cell_angle_beta                 67.651(4)
_cell_angle_gamma                65.864(4)
_cell_formula_units_Z            1
_cell_length_a                   12.3906(12)
_cell_length_b                   12.5842(13)
_cell_length_c                   13.3974(14)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.635
_cell_measurement_theta_min      2.223
_cell_volume                     1654.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.781
_diffrn_measured_fraction_theta_max 0.781
_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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31286
_diffrn_reflns_theta_full        34.01
_diffrn_reflns_theta_max         34.01
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.9709
_exptl_absorpt_correction_T_min  0.8729
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       prism
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         10551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.5578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                9833
_reflns_number_total             10551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja202448b_si_002_2.cif
_cod_data_source_block           ls127_0m
_cod_database_code               4106857