Broadening the Scope of Group 4 Hydroamination Catalysis Using a Tethered Ureate Ligand
David C. Leitch; Philippa R. Payne; Christine R. Dunbar; Laurel L. Schafer; Journal of the American Chemical Society 131 (2009) 18246–18247; doi:10.1021/ja906955b

data_4105498
_publ_section_title
;
 Broadening the Scope of Group 4 Hydroamination Catalysis Using a Tethered
 Ureate Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18246
_journal_page_last               18247
_journal_paper_doi               10.1021/ja906955b
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C25 H57 N7 O2 Zr'
_chemical_formula_sum            'C25 H57 N7 O2 Zr'
_chemical_formula_weight         579.00
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.248(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9870(12)
_cell_length_b                   16.1923(12)
_cell_length_c                   14.2982(11)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.48
_cell_volume                     3224.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34829
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.8944
_exptl_absorpt_correction_T_min  0.7583
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.327
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         9324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+1.6426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                7640
_reflns_number_total             9324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906955b_si_001.cif
_cod_data_source_block           ls156_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4105498