Mechanistic Insights in the Exchange of Arylthiolate Groups in Aryl(arylthiolato)palladium Complexes Supported by a Dippe Ligand
Munjanja, Lloyd; Brennessel, William W.; Jones, William D.; Organometallics 34 (2015) 4574–; doi:10.1021/acs.organomet.5b00662

data_4086266
_publ_section_title
;
 Mechanistic Insights in the Exchange of Arylthiolate Groups in
 Aryl(arylthiolato)palladium Complexes Supported by a Dippe Ligand
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4574
_journal_paper_doi               10.1021/acs.organomet.5b00662
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C26 H42 P2 Pd S'
_chemical_formula_sum            'C26 H42 P2 Pd S'
_chemical_formula_weight         554.99
_chemical_name_common            jonlm23
_chemical_name_systematic        Pd(dippe)(SPh)(Ph)
_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_method           SHELXL-2014/7
_cell_angle_alpha                90.138(6)
_cell_angle_beta                 90.198(7)
_cell_angle_gamma                99.772(6)
_cell_formula_units_Z            4
_cell_length_a                   8.434(3)
_cell_length_b                   11.375(4)
_cell_length_c                   27.611(9)
_cell_measurement_reflns_used    4072
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      24.25
_cell_measurement_theta_min      2.34
_cell_volume                     2610.4(16)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1508
_diffrn_reflns_av_unetI/netI     0.1327
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35873
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.482
_diffrn_reflns_theta_min         1.817
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.228
_refine_diff_density_min         -1.873
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         9526
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+24.4690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6835
_reflns_number_total             9526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00662_si_002.cif
_cod_data_source_block           3c
_cod_original_cell_volume        2610.6(15)
_cod_database_code               4086266
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.955
_exptl_absorpt_special_details
; 
The structure is a pseudomerohedral twin. Application of twin 
law [ -1 0 0 / 0 -1 0 / 0 0 1 ], a 180 degree rotation about direct 
and reciprocal axes [001] reduced the R1 value, from 0.229 to 0.083. 
The mass ratio of twin components refined to 0.6192(15):0.3808(15). 
  
The anistropic displacement parameters of three pairs of neighboring 
atoms were restrained to be similar. Additionally, anisotropic 
displacement parameters for pairs of opposing atoms of the various 
phenyl rings were constrained to be equivalent. 
;
_shelx_res_checksum              25500
_shelx_hkl_checksum              66926