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_4084282
_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 H16 F12 O P2'
_chemical_formula_weight         658.35
_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                 102.536(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.726(3)
_cell_length_b                   11.552(3)
_cell_length_c                   16.122(4)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.43
_cell_measurement_theta_min      2.19
_cell_volume                     2677.2(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_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  0.0796
_diffrn_reflns_av_sigmaI/netI    0.1051
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31861
_diffrn_reflns_theta_full        28.43
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_T_max  0.9788
_exptl_absorpt_correction_T_min  0.9188
_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    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1277
_reflns_number_gt                3719
_reflns_number_total             6627
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500699t_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        2677.1(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4084282