Experimental and Computational Assessment of Reactivity and Mechanism in C(sp(3))-N Bond-Forming Reductive Elimination from Palladium(IV).
Pendleton, Ian M.; Pérez-Temprano, Mónica H; Sanford, Melanie S.; Zimmerman, Paul M.; Journal of the American Chemical Society 138 (2016) 6049–6060; doi:10.1021/jacs.6b02714

data_4130358
_publ_section_title
;
 Experimental and Computational Assessment of Reactivity and Mechanism in
 C(sp(3))-N Bond-Forming Reductive Elimination from Palladium(IV).
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6049
_journal_page_last               6060
_journal_paper_doi               10.1021/jacs.6b02714
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C28 H30 F N3 O2 Pd S'
_chemical_formula_sum            'C28 H30 F N3 O2 Pd S'
_chemical_formula_weight         598.01
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c a 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                   16.2633(6)
_cell_length_b                   9.9482(3)
_cell_length_c                   15.9423(11)
_cell_measurement_reflns_used    17960
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      69.50
_cell_measurement_theta_min      9.00
_cell_volume                     2579.3(2)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12'
_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      85(2)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'micro-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1305
_diffrn_reflns_av_sigmaI/netI    0.1015
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            68910
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         4.44
_exptl_absorpt_coefficient_mu    6.875
_exptl_absorpt_correction_T_max  0.8747
_exptl_absorpt_correction_T_min  0.4461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.112
_refine_diff_density_min         -1.786
_refine_diff_density_rms         0.189
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.040(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4708
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0714
_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^)+(0.0374P)^2^+43.8717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.1895
_reflns_number_gt                4536
_reflns_number_total             4708
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b02714_si_003.cif
_cod_data_source_block           1TsNMe-b
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               4130358