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_4130361
_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         'C36 H40 N4 O4 Pd S2, C H2 Cl2, H2 O'
_chemical_formula_sum            'C37 H44 Cl2 N4 O5 Pd S2'
_chemical_formula_weight         866.18
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                90.013(6)
_cell_angle_beta                 97.735(7)
_cell_angle_gamma                113.481(8)
_cell_formula_units_Z            2
_cell_length_a                   10.0440(2)
_cell_length_b                   12.3450(2)
_cell_length_c                   17.7048(12)
_cell_measurement_reflns_used    20661
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      2.50
_cell_volume                     1991.66(19)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      225(2)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0835
_diffrn_reflns_av_sigmaI/netI    0.0664
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31458
_diffrn_reflns_theta_full        68.21
_diffrn_reflns_theta_max         68.21
_diffrn_reflns_theta_min         4.53
_exptl_absorpt_coefficient_mu    6.345
_exptl_absorpt_correction_T_max  0.7854
_exptl_absorpt_correction_T_min  0.7020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.497
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         7116
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0726
_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^)+(0.1523P)^2^+1.6074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2149
_refine_ls_wR_factor_ref         0.2212
_reflns_number_gt                6433
_reflns_number_total             7116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b02714_si_003.cif
_cod_data_source_block           2TsNMe
_cod_original_cell_volume        1991.66(14)
_cod_database_code               4130361