Nanosized Pd37(CO)28{P(p-Tolyl)3}12 Containing Geometrically Unprecedented Central 23-Atom Interpenetrating Tri-icosahedral Palladium Kernel of Double Icosahedral Units: Its Postulated Metal-Core Evolution and Resulting Stereochemical Implications
Evgueni G. Mednikov; Lawrence F. Dahl; Journal of the American Chemical Society 130 (2008) 14813–14821; doi:10.1021/ja805679j

data_4108606
_publ_section_title
;
 Nanosized Pd37(CO)28{P(p-Tolyl)3}12 Containing Geometrically
 Unprecedented Central 23-Atom Interpenetrating Tri-icosahedral Palladium
 Kernel of Double Icosahedral Units: Its Postulated Metal-Core Evolution
 and Resulting Stereochemical Implications
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14813
_journal_page_last               14821
_journal_paper_doi               10.1021/ja805679j
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C302 H302 O29 P12 Pd37.05'
_chemical_formula_weight         8709.20
_chemical_name_common            'Palladium Carbonyl Phosphine cluster'
_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                96.80
_cell_angle_beta                 90.34
_cell_angle_gamma                114.67
_cell_formula_units_Z            2
_cell_length_a                   20.6439(5)
_cell_length_b                   22.0806(5)
_cell_length_c                   36.0579(8)
_cell_measurement_temperature    100(2)
_cell_volume                     14803.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'SMART CCD 1000 area detector difractometer'
_diffrn_measurement_method       'w 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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            118532
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    2.311
_exptl_absorpt_correction_T_max  0.5638
_exptl_absorpt_correction_T_min  0.4161
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_description       'block crystal'
_exptl_crystal_F_000             8461
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         2.419
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3260
_refine_ls_number_reflns         68887
_refine_ls_number_restraints     359
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+134.6392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1289
_reflns_number_gt                53156
_reflns_number_total             68887
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja805679j_si_001.cif
_cod_data_source_block           dahl330
_cod_original_cell_volume        14802.4(6)
_cod_database_code               4108606