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_4084281
_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            'C33 H40 F6 Na O10 P S'
_chemical_formula_weight         796.67
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_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                84.68(3)
_cell_angle_beta                 89.20(3)
_cell_angle_gamma                74.64(3)
_cell_formula_units_Z            2
_cell_length_a                   10.110(2)
_cell_length_b                   10.205(2)
_cell_length_c                   18.067(4)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.08
_cell_volume                     1789.6(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1026
_diffrn_reflns_av_sigmaI/netI    0.2058
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17431
_diffrn_reflns_theta_full        25.16
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  0.9815
_exptl_absorpt_correction_T_min  0.9121
_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    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.738
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         6352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.738
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                2732
_reflns_number_total             6352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500699t_si_002.cif
_cod_data_source_block           '[Na(18-crown-6)(H2O)][1]'
_cod_original_cell_volume        1789.6(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084281