Monolacunary Keggin polyoxometalates connected to ten 4d or 4f metal atoms.
Pang, Haijun; Gómez-García, Carlos J; Peng, Jun; Ma, Huiyuan; Zhang, Chunjing; Wu, Qingyin; Dalton transactions (Cambridge, England : 2003) 42 (2013) 16596–16601; doi:10.1039/c3dt51899j

data_7023918
_publ_section_title
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 Monolacunary Keggin polyoxometalates connected to ten 4d or 4f metal
 atoms.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16596
_journal_page_last               16601
_journal_paper_doi               10.1039/c3dt51899j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'Ag3 Ce4 H63 O109 Si2 W22'
_chemical_formula_weight         6792.15
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.617(3)
_cell_angle_beta                 92.259(3)
_cell_angle_gamma                105.104(4)
_cell_formula_units_Z            1
_cell_length_a                   12.3582(6)
_cell_length_b                   13.2410(6)
_cell_length_c                   18.0640(5)
_cell_measurement_temperature    571(2)
_cell_volume                     2838.9(2)
_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      571(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.838
_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  0.0704
_diffrn_reflns_av_sigmaI/netI    0.1962
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22384
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    24.390
_exptl_absorpt_correction_T_max  0.005
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.870
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2845.0
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
The free water molecules were highly disordered and could not be modeled properly, thus the SQUEEZE routine of PLATON was applied to remove the contributions to the scattering from the solvent molecules. The reported refinements are of the guest-free structures using the *.hkp files produced via the SQUEEZE routine. 
;
_refine_diff_density_max         8.065
_refine_diff_density_min         -6.373
_refine_diff_density_rms         0.547
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         12886
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0179P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                6252
_reflns_number_total             15377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51899j.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7023918