A Supramolecular Heteropolyoxopalladate {Pd15} Cluster Host Encapsulating a {Pd2} Dinuclear Guest: [PdII2@{H7PdII15O10(PO4)10}]9-
Feng Xu; Rachel A. Scullion; Jun Yan; Haralampos N. Miras; Christoph Busche; Antonino Scandurra; Bruno Pignataro; De-Liang Long; Leroy Cronin; Journal of the American Chemical Society 133 (2011) 4684–4686; doi:10.1021/ja1105514

data_4105865
_publ_section_title
;
 A Supramolecular Heteropolyoxopalladate {Pd15} Cluster Host Encapsulating
 a {Pd2} Dinuclear Guest: [PdII2@{H7PdII15O10(PO4)10}]9-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4684
_journal_page_last               4686
_journal_paper_doi               10.1021/ja1105514
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         '13(Na +), (H7 O50 P10 Pd15 13-), 40(H2 O)'
_chemical_formula_sum            'H87 Na13 O90 P10 Pd15'
_chemical_formula_weight         3732.27
_chemical_name_systematic
;
 ?
;
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.083(3)
_cell_angle_beta                 81.990(3)
_cell_angle_gamma                72.782(3)
_cell_formula_units_Z            2
_cell_length_a                   13.5833(5)
_cell_length_b                   15.9930(5)
_cell_length_c                   21.7485(8)
_cell_measurement_reflns_used    18564
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.5
_cell_measurement_theta_min      2.89
_cell_volume                     4468.7(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w & \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47938
_diffrn_reflns_theta_full        62.60
_diffrn_reflns_theta_max         62.60
_diffrn_reflns_theta_min         2.89
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    27.258
_exptl_absorpt_correction_T_max  0.525
_exptl_absorpt_correction_T_min  0.151
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.774
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3580
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.51
_refine_diff_density_min         -1.28
_refine_diff_density_rms         0.22
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1217
_refine_ls_number_reflns         14041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0759P)^2^+27.4181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1389
_reflns_number_gt                10223
_reflns_number_total             14041
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja1105514_si_002_1.cif
_cod_data_source_block           Pd15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4105865