New Type of Heterometallic 3d-4f Rhomblike Core in Weakley-Like Polyoxometalates
Santiago Reinoso; José Ramón Galán-Mascarós; Luis Lezama; Inorganic Chemistry 50 (2011) 9587–9593; doi:10.1021/ic201331d

data_4326379
_publ_section_title
;
 New Type of Heterometallic 3d-4f Rhomblike Core in Weakley-Like
 Polyoxometalates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9587
_journal_page_last               9593
_journal_paper_doi               10.1021/ic201331d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C2 H45 Ce Cs3 Cu3 Ge2 K4 Na4 O91 W18'
_chemical_formula_weight         5957.69
_chemical_name_systematic
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 ?
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_formula_units_Z            2
_cell_length_a                   12.5496(2)
_cell_length_b                   17.4025(4)
_cell_length_c                   23.3170(5)
_cell_measurement_reflns_used    17160
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.9302
_cell_measurement_theta_min      2.3511
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_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX  (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla et al, 2005)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34532
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    25.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.202
_exptl_crystal_description       prism
_exptl_crystal_F_000             5222
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.598
_refine_diff_density_min         -3.335
_refine_diff_density_rms         0.397
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         14834
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0787P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                10679
_reflns_number_total             14834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201331d_si_002.cif
_cod_data_source_block           1a
_cod_original_cell_volume        4708.32(17)
_cod_database_code               4326379