New Approach for Size- and Shape-Controlled Preparation of Pd Nanoparticles with Organic Ligands. Synthesis and Application in Catalysis
Valentine P. Ananikov; Nikolay V. Orlov; Irina P. Beletskaya; Victor N. Khrustalev; Mikhail Yu. Antipin; Tatiana V. Timofeeva; Journal of the American Chemical Society 129 (2007) 7252–7253; doi:10.1021/ja071727r

data_4109521
_publ_section_title
;
 New Approach for Size- and Shape-Controlled Preparation of Pd
 Nanoparticles with Organic Ligands. Synthesis and Application in
 Catalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7252
_journal_page_last               7253
_journal_paper_doi               10.1021/ja071727r
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C11 H22 N S 1+, C2 H O4 1-'
_chemical_formula_sum            'C13 H23 N O4 S'
_chemical_formula_weight         289.38
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-03
_cell_angle_alpha                90.00
_cell_angle_beta                 93.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.42(7)
_cell_length_b                   5.567(12)
_cell_length_c                   16.32(3)
_cell_measurement_reflns_used    522
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.8
_cell_measurement_theta_min      2.5
_cell_volume                     2941(10)
_computing_cell_refinement       'SAINTPlus, v. 6.2 (Bruker, 2001)'
_computing_data_collection       'APEX2  (Bruker, 2005)'
_computing_data_reduction        'SAINTPlus, v. 6.2 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.12 (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL, v. 6.12 (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL, v. 6.12 (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL, v. 6.12 (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker SMART APEX II 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  0.0695
_diffrn_reflns_av_sigmaI/netI    0.3076
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12393
_diffrn_reflns_theta_full        26.15
_diffrn_reflns_theta_max         26.15
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       needle
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0109(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.2627
_refine_ls_R_factor_gt           0.0832
_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^)+(0.0100P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                966
_reflns_number_total             2838
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja071727rsi20070321_085608.cif
_cod_data_source_block           5d-salt
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4109521