High-nuclearity palladium carbonyl trimethylphosphine clusters containing unprecedented face-condensed icosahedral-based transition-metal core geometries: proposed growth patterns from a centered Pd13 icosahedron†
Tran, Nguyet T.; Kawano, Masaki; Dahl, Lawrence F.; Journal of the Chemical Society, Dalton Transactions  (2001) 2731–; doi:10.1039/b103547a

data_7010776
_publ_section_title
;
 High-nuclearity palladium carbonyl trimethylphosphine clusters
 containing unprecedented face-condensed icosahedral-based
 transition-metal core geometries: proposed growth patterns from a
 centered Pd13 icosahedron&#x2020;
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2731
_journal_paper_doi               10.1039/b103547a
_journal_year                    2001
_chemical_formula_moiety         '[Pd35 (CO)23 (PMe3)15]'
_chemical_formula_sum            'C68 H135 O23 P15 Pd35'
_chemical_formula_weight         5509.31
_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                75.353(2)
_cell_angle_beta                 89.019(2)
_cell_angle_gamma                83.392(2)
_cell_formula_units_Z            2
_cell_length_a                   16.6290(2)
_cell_length_b                   17.5060(2)
_cell_length_c                   25.0118(3)
_cell_measurement_reflns_used    5704
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     6997.15(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device       'Siemens P4/ccd'
_diffrn_measurement_method       'phi scan frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1371
_diffrn_reflns_av_sigmaI/netI    0.2821
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45307
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.23
_diffrn_standards_decay_%        0.3
_diffrn_standards_number         217
_exptl_absorpt_coefficient_mu    4.584
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.425
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5124
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.844
_refine_diff_density_min         -3.398
_refine_diff_density_rms         0.533
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1270
_refine_ls_number_reflns         23072
_refine_ls_number_restraints     684
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.2234
_refine_ls_R_factor_gt           0.1006
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2254
_refine_ls_wR_factor_ref         0.2873
_reflns_number_gt                9948
_reflns_number_total             23072
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103547a.txt
_cod_data_source_block           pd35f
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        6997.16(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010776