Ligand- and Base-Free Pd(II)-Catalyzed Controlled Switching between Oxidative Heck and Conjugate Addition Reactions.
Walker, Sarah E.; Boehnke, Julian; Glen, Pauline E.; Levey, Steven; Patrick, Lisa; Jordan-Hore, James A; Lee, Ai-Lan; Organic letters 15 (2013) 1886–1889; doi:10.1021/ol400539h

data_1511914
_publ_section_title
;
 Ligand- and Base-Free Pd(II)-Catalyzed Controlled Switching between
 Oxidative Heck and Conjugate Addition Reactions.
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              1886
_journal_page_last               1889
_journal_paper_doi               10.1021/ol400539h
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C8 H24 O4 Pd S4, 2(C F3 O3 S)'
_chemical_formula_sum            'C10 H24 F6 O10 Pd S6'
_chemical_formula_weight         717.05
_chemical_name_systematic
;
 ? 
;
_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             2013-01-29
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                100.351(3)
_cell_angle_beta                 95.827(3)
_cell_angle_gamma                102.234(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6136(4)
_cell_length_b                   8.6555(4)
_cell_length_c                   17.1980(8)
_cell_measurement_reflns_used    7218
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.10
_cell_measurement_theta_min      2.45
_cell_volume                     1219.62(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31422
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.22
_diffrn_reflns_theta_min         1.22
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.364
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0656 before and 0.0482 after correction.
The Ratio of minimum to maximum transmission is 0.8940.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.633
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         8445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0173P)^2^+0.9279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                6936
_reflns_number_total             8445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol400539h_si_001.cif
_cod_data_source_block           4561
_cod_database_code               1511914