Self-assembled monolayers based on Pd-containing organometallic thiols: preparation and structural characterization.
Vitaliano, Rosa; Fratoddi, Ilaria; Venditti, Iole; Roviello, Giuseppina; Battocchio, Chiara; Polzonetti, Giovanni; Russo, Maria Vittoria; The journal of physical chemistry. A 113 (2009) 14730–14740; doi:10.1021/jp904865k

data_1516351
_publ_section_title
;
 Self-assembled monolayers based on Pd-containing organometallic thiols:
 preparation and structural characterization.
;
_journal_issue                   52
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              14730
_journal_page_last               14740
_journal_paper_doi               10.1021/jp904865k
_journal_volume                  113
_journal_year                    2009
_chemical_formula_moiety         'C28 H60 O2 P2 Pd S2'
_chemical_formula_sum            'C28 H60 O2 P2 Pd S2'
_chemical_formula_weight         661.22
_chemical_name_systematic
;
 trans-Palladium(II)-bis(tributylphosphine)-bis(kS-thioacetate)
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_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                67.8280(10)
_cell_angle_beta                 81.864(5)
_cell_angle_gamma                85.0560(10)
_cell_formula_units_Z            1
_cell_length_a                   8.538(5)
_cell_length_b                   10.605(4)
_cell_length_c                   11.064(6)
_cell_measurement_reflns_used    99
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.453
_cell_measurement_theta_min      3.865
_cell_volume                     917.8(8)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0786
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14254
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.24
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.8683
_exptl_absorpt_correction_T_min  0.8115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS(Bruker 2000)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.30(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6745
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.938
_refine_ls_shift/su_mean         0.104
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1536
_reflns_number_gt                4666
_reflns_number_total             6745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp904865k_si_002.cif
_cod_data_source_block           rv80
_cod_original_sg_symbol_H-M      P1
_cod_database_code               1516351