Asymmetric Catalytic Intramolecular Hydroamination of Aminoallenes by Tantalum Amidoalkoxide Complexes
Hansen, Michelle C.; Heusser, Carolyn A.; Narayan, Tarun C.; Fong, Kristine E.; Hara, Nagiko; Kohn, Alexander W.; Venning, Alexander R.; Rheingold, Arnold L.; Johnson, Adam R.; Organometallics 30 (2011) 4616–; doi:10.1021/om200446v

data_4064950
_publ_section_title
;
 Asymmetric Catalytic Intramolecular Hydroamination of Aminoallenes by
 Tantalum Amidoalkoxide Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4616
_journal_paper_doi               10.1021/om200446v
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C29 H47 N4 O Ta'
_chemical_formula_weight         648.66
_chemical_melting_point          384(1)
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2269(5)
_cell_length_b                   16.2635(8)
_cell_length_c                   19.5119(10)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      2.43
_cell_volume                     2928.0(3)
_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      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14424
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    3.781
_exptl_absorpt_correction_T_max  0.5378
_exptl_absorpt_correction_T_min  0.4565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0156
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0356
_refine_ls_wR_factor_ref         0.0358
_reflns_number_gt                5190
_reflns_number_total             5384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200446v_si_001.cif
_cod_data_source_block           hmc04
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4064950