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_7010775
_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         '[Pd29 Ni3 (CO)22 (PMe3)13] 0.3(C4 H8 O)'
_chemical_formula_sum            'C62.2 H119.4 Ni3 O22.3 P13 Pd29'
_chemical_formula_weight         4888.52
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.4877(2)
_cell_length_b                   16.4877(2)
_cell_length_c                   38.2484(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     9004.59(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.917
_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            10756
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        1.08
_diffrn_standards_number         389
_exptl_absorpt_coefficient_mu    4.897
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.570
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6852
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.082
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.174
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         6122
_refine_ls_number_restraints     441
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+234.0554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                5898
_reflns_number_total             6122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103547a.txt
_cod_data_source_block           dahl59a
_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_sg_symbol_H-M      R3
_cod_original_formula_sum        'C62.20 H119.40 Ni3 O22.30 P13 Pd29'
_cod_database_code               7010775