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_4084283
_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            'C29 H26 F6 N O3 P Pd S'
_chemical_formula_weight         719.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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_method           SHELXL-97
_cell_angle_alpha                81.697(9)
_cell_angle_beta                 82.962(9)
_cell_angle_gamma                87.266(9)
_cell_formula_units_Z            2
_cell_length_a                   9.025(5)
_cell_length_b                   9.143(5)
_cell_length_c                   17.445(9)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      2.25
_cell_volume                     1413.0(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0980
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13618
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.9344
_exptl_absorpt_correction_T_min  0.7947
_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    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                3612
_reflns_number_total             5031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500699t_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        1413.1(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084283