Origin of Fast Catalysis in Allylic Amination Reactions Catalyzed by Pd-Ti Heterobimetallic Complexes.
Walker, Whitney K.; Kay, Benjamin M.; Michaelis, Scott A.; Anderson, Diana L.; Smith, Stacey J.; Ess, Daniel H.; Michaelis, David J.; Journal of the American Chemical Society 137 (2015) 7371–7378; doi:10.1021/jacs.5b02428

data_4123761
_publ_section_title
;
 Origin of Fast Catalysis in Allylic Amination Reactions Catalyzed by
 Pd-Ti Heterobimetallic Complexes.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7371
_journal_page_last               7378
_journal_paper_doi               10.1021/jacs.5b02428
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C38 H49 N2 P2 Pd, S O3 C F3'
_chemical_formula_sum            'C39 H49 F3 N2 O3 P2 Pd S'
_chemical_formula_weight         851.20
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 108.3560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3888(4)
_cell_length_b                   34.9174(14)
_cell_length_c                   11.0842(4)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.05
_cell_measurement_theta_min      2.61
_cell_volume                     3816.2(3)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            328261
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.032
_diffrn_reflns_theta_min         1.936
_diffrn_source                   'I\mS micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.493(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         26571
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+1.2513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0450
_reflns_Friedel_coverage         0.972
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     1.000
_reflns_number_gt                26431
_reflns_number_total             26571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b02428_si_002.cif
_cod_data_source_block           14002
_cod_depositor_comments          'Adding full bibliography for 4123761.cif.'
_cod_database_code               4123761
_shelx_estimated_absorpt_t_min   0.807
_shelx_estimated_absorpt_t_max   0.920
_shelxl_version_number           2013-4
_shelx_res_checksum              69423
_shelx_hkl_checksum              268