2-pyridonate tantalum complexes for the intermolecular hydroaminoalkylation of sterically demanding alkenes.
Chong, Eugene; Brandt, Jason W.; Schafer, Laurel L.; Journal of the American Chemical Society 136 (2014) 10898–10901; doi:10.1021/ja506187m

data_4122302
_publ_section_title
;
 2-pyridonate tantalum complexes for the intermolecular
 hydroaminoalkylation of sterically demanding alkenes.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10898
_journal_page_last               10901
_journal_paper_doi               10.1021/ja506187m
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C17 H26 Cl N O Ta'
_chemical_formula_sum            'C17 H26 Cl N O Ta'
_chemical_formula_weight         518.82
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                83.546(5)
_cell_angle_beta                 76.684(5)
_cell_angle_gamma                68.516(5)
_cell_formula_units_Z            6
_cell_length_a                   10.8175(19)
_cell_length_b                   13.761(2)
_cell_length_c                   21.924(4)
_cell_measurement_reflns_used    9527
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.2995
_cell_measurement_theta_min      2.8655
_cell_volume                     2953.8(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            64307
_diffrn_reflns_theta_full        30.25
_diffrn_reflns_theta_max         30.25
_diffrn_reflns_theta_min         1.59
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.728
_exptl_absorpt_correction_T_max  0.1201
_exptl_absorpt_correction_T_min  0.0948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1524
_exptl_crystal_recrystallization_method hexanes
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.592
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         17439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0202P)^2^+1.6537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0599
_reflns_number_gt                15262
_reflns_number_total             17439
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja506187m_si_002.cif
_cod_data_source_block           ls501_0m
_cod_depositor_comments
'Adding full bibliography for 4122302--4122304.cif.'
_cod_original_cell_volume        2953.8(15)
_cod_database_code               4122302