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_7010774
_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         '[Pd16 (CO)13 (PMe3)9] 2(MeOH) 3(H2O)'
_chemical_formula_sum            'C42 H95 O18 P9 Pd16'
_chemical_formula_weight         2869.31
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_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            2
_cell_length_a                   15.6242(2)
_cell_length_b                   15.6242(2)
_cell_length_c                   20.2437(5)
_cell_measurement_reflns_used    7996
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     4279.73(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.906
_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  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8757
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0.3
_diffrn_standards_number         256
_exptl_absorpt_coefficient_mu    3.485
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2724
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(7)
_refine_ls_extinction_coef       0.00022(3)
_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   1.180
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3240
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+27.4739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                3189
_reflns_number_total             3240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103547a.txt
_cod_data_source_block           pd16f
_cod_depositor_comments
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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 
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_cod_database_code               7010774