Differentiation between Chelate Ring Inversion and Aryl Rotation in a CF3-Substituted Phosphine-Sulfonate Palladium Methyl Complex
Feng, Ge; Conley, Matthew P.; Jordan, Richard F.; Organometallics 33 (2014) 4486–; doi:10.1021/om500699t

data_4084284
_publ_section_title
;
 Differentiation between Chelate Ring Inversion and Aryl Rotation in a
 CF3-Substituted Phosphine-Sulfonate Palladium Methyl Complex
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4486
_journal_paper_doi               10.1021/om500699t
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C28 H24 Cl2 F6 N O3 P Pd S'
_chemical_formula_weight         776.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_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                 125.490(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.412(3)
_cell_length_b                   16.226(5)
_cell_length_c                   19.195(4)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      1.81
_cell_volume                     2894.0(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32657
_diffrn_reflns_theta_full        27.31
_diffrn_reflns_theta_max         27.31
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  0.8211
_exptl_absorpt_correction_T_min  0.7349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
absorption corrections were made based on correspondance of
equivalent intensities usingprogram SADABS (G. Sheldrick, Bruker 
Analytical X-ray Systems, Madison, WI)
;
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.262
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0894P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1642
_reflns_number_gt                4944
_reflns_number_total             6408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500699t_si_002.cif
_cod_data_source_block           4
_cod_original_cell_volume        2894.0(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4084284