Synthesis and Characterization of a New Tiara Pd(II) Thiolate Complex, [Pd(SC12H25)2]6, and Its Solution-Phase Thermolysis to Prepare Nearly Monodisperse Palladium Sulfide Nanoparticles
Zhiqiang Yang; Alexander B. Smetana; Christopher M. Sorensen; Kenneth J. Klabunde; Inorganic Chemistry 46 (2007) 2427–2431; doi:10.1021/ic061242o

data_4306934
_publ_section_title
;
Synthesis and Characterization of a New Tiara Pd(II) Thiolate Complex,
[Pd(SC12H25)2]6, and Its Solution-Phase Thermolysis to Prepare Nearly
Monodisperse Palladium Sulfide Nanoparticles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2427
_journal_page_last               2431
_journal_paper_doi               10.1021/ic061242o
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety
;
(C12 H25 S)2 Pd
;
_chemical_formula_sum            'C24 H50 Pd S2'
_chemical_formula_weight         509.16
_chemical_name_systematic
;
bis(dodecanethiolato)palladium(II)
;
_space_group_IT_number           2
_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                66.529(5)
_cell_angle_beta                 70.892(8)
_cell_angle_gamma                77.054(7)
_cell_formula_units_Z            6
_cell_length_a                   13.2189(14)
_cell_length_b                   18.2919(18)
_cell_length_c                   19.1575(19)
_cell_measurement_reflns_used    2069
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.55
_cell_measurement_theta_min      2.25
_cell_volume                     3991.4(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1073
_diffrn_reflns_av_sigmaI/netI    0.2124
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28432
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.336
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         17309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1616
_reflns_number_gt                8089
_reflns_number_total             17309
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061242osi20061121_094803.cif
_cod_data_source_block           kk0105m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C24 H50 Pd1 S2'
_cod_database_code               4306934