First Structurally Characterized Palladium(II)-Substituted Polyoxoanion: [Cs~2~Na(H~2~O)~10~Pd~3~(α-Sb^III^W~9~O~33~)~2~]^9-^
Li-Hua Bi; Markus Reicke; Ulrich Kortz; Bineta Keita; Louis Nadjo; Ronald J. Clark; Inorganic Chemistry 43 (2004) 3915–3920; doi:10.1021/ic049736d

data_4311181
_publ_contact_author_address
; 
International University Bremen
School of Engineering and Science
P.O. Box 750 561
28725 Bremen
Germany
;
_publ_contact_author_email
;
u.kortz@iu-bremen.de
;
_publ_contact_author_fax
;
+49-421-200 3229
;
_publ_contact_author_name
;
Ulrich KORTZ
;
_publ_contact_author_phone
;
+49-421-200 3235
;
_publ_section_title
;
 First Structurally Characterized Palladium(II)-Substituted Polyoxoanion:
 [Cs~2~Na(H~2~O)~10~Pd~3~(\a-Sb^III^W~9~O~33~)~2~]^9-^
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3915
_journal_page_last               3920
_journal_paper_doi               10.1021/ic049736d
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'Cs5 H59 K Na6 O92.5 Pd3 Sb2 W18'
_chemical_formula_weight         6253.2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 100.416(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3963(13)
_cell_length_b                   19.5970(19)
_cell_length_c                   18.1723(17)
_cell_measurement_reflns_used    9275
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      1.85
_cell_volume                     4692.1(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65274
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    25.171
_exptl_absorpt_correction_T_max  0.1526
_exptl_absorpt_correction_T_min  0.0466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5326
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         4.120
_refine_diff_density_min         -3.198
_refine_diff_density_rms         0.446
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         12053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+248.7946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1243
_reflns_number_gt                11387
_reflns_number_total             12053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049736dsi20040416_014826.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_formula_sum        'Cs5 H59 K Na6 O92.50 Pd3 Sb2 W18'
_cod_database_code               4311181