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_4130360
_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         'C21 H20 F3 N3 O2 Pd S'
_chemical_formula_sum            'C21 H20 F3 N3 O2 Pd S'
_chemical_formula_weight         541.86
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.248(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.154(3)
_cell_length_b                   8.2340(2)
_cell_length_c                   31.472(2)
_cell_measurement_reflns_used    7933
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.1
_cell_measurement_theta_min      2.8
_cell_volume                     2096.1(8)
_computing_cell_refinement
;
Rigaku CrystalClear-SM Expert 2.0 r12
;
_computing_data_collection
;
Rigaku CrystalClear-SM Expert 2.0 r12
;
_computing_data_reduction
;
Rigaku CrystalClear-SM Expert 2.0 r12
;
_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      85(2)
_diffrn_detector_area_resol_mean 22.2222
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Rigaku CrystalClear-SM Expert 2.0 r12
;
_diffrn_measurement_method       'profile data from \w-scans'
_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  0.0902
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            26866
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         5.47
_exptl_absorpt_coefficient_mu    8.528
_exptl_absorpt_correction_T_max  0.4826
_exptl_absorpt_correction_T_min  0.3423
_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    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.650
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+3.4887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                3679
_reflns_number_total             3797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b02714_si_003.cif
_cod_data_source_block           2Tf
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2096.2(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4130360