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_4122303
_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         '2(C19 H32 N5 O Ta), 0.5(C6 H14)'
_chemical_formula_sum            'C41 H71 N10 O2 Ta2'
_chemical_formula_weight         1097.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2012-05-25
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                68.087(5)
_cell_angle_beta                 75.004(8)
_cell_angle_gamma                64.226(5)
_cell_formula_units_Z            2
_cell_length_a                   12.3246(15)
_cell_length_b                   13.0655(15)
_cell_length_c                   17.410(3)
_cell_measurement_reflns_used    8133
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.137
_cell_measurement_theta_min      2.539
_cell_volume                     2326.5(6)
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29697
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         1.27
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.743
_exptl_absorpt_correction_T_max  0.3522
_exptl_absorpt_correction_T_min  0.2118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1373 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.6013.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'golden brown'
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1098
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.657
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         8208
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.256
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0006P)^2^+40.4005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1235
_reflns_number_gt                6754
_reflns_number_total             8208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja506187m_si_002.cif
_cod_data_source_block           ls324
_cod_depositor_comments
'Adding full bibliography for 4122302--4122304.cif.'
_cod_original_cell_volume        2326.5(5)
_cod_database_code               4122303