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_4105866
_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         '9(Na +), (H7 O50 P10 Pd17 9-), 40(H2 O)'
_chemical_formula_sum            'H87 Na9 O90 P10 Pd17'
_chemical_formula_weight         3853.11
_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                87.270(2)
_cell_angle_beta                 82.755(2)
_cell_angle_gamma                73.821(2)
_cell_formula_units_Z            2
_cell_length_a                   14.9100(2)
_cell_length_b                   14.9327(3)
_cell_length_c                   23.0483(4)
_cell_measurement_reflns_used    50004
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.4
_cell_measurement_theta_min      3.08
_cell_volume                     4888.62(15)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Gemini CCD'
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            84920
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    27.610
_exptl_absorpt_correction_T_max  0.569
_exptl_absorpt_correction_T_min  0.069
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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            red
_exptl_crystal_density_diffrn    2.618
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3676
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.59
_refine_diff_density_min         -0.86
_refine_diff_density_rms         0.20
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1218
_refine_ls_number_reflns         17546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+29.0202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                15695
_reflns_number_total             17546
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja1105514_si_002_2.cif
_cod_data_source_block           Pd17
_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               4105866