Palladium(II)-Substituted Tungstosilicate [Cs2K(H2O)7Pd2WO(H2O)(A-α-SiW9O34)2]9-
Li-Hua Bi; Ulrich Kortz; Bineta Keita; Louis Nadjo; Horst Borrmann; Inorganic Chemistry 43 (2004) 8367–8372; doi:10.1021/ic048864z

data_4312218
_publ_section_title
;
 Palladium(II)-Substituted Tungstosilicate
 [Cs2K(H2O)7Pd2WO(H2O)(A-\a-SiW9O34)2]9-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8367
_journal_page_last               8372
_journal_paper_doi               10.1021/ic048864z
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'Cs5 H26 K3 Na4 O82 Pd2 Si2 W19'
_chemical_formula_weight         5974.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 95.4596(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6549(2)
_cell_length_b                   19.7290(2)
_cell_length_c                   25.9950(5)
_cell_measurement_reflns_used    35424
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.09
_cell_volume                     8502.8(2)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2003)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2003)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2003)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.819
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measurement_device_type  'Rigaku AFC7 and Mercury CCD'
_diffrn_measurement_method       'phi and omega 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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            63415
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    28.374
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    4.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10158
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         6.092
_refine_diff_density_min         -4.494
_refine_diff_density_rms         0.469
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         19961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0424P)^2^+359.0999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                17305
_reflns_number_total             19961
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048864zsi20041004_013750.cif
_cod_data_source_block           test
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        8502.8(3)
_cod_database_code               4312218