Solid-State and Solution Studies of {Lnn(SiW11O39)} Polyoxoanions: An Example of Building Block Condensation Dependent on the Nature of the Rare Earth
Pierre Mialane; Laurent Lisnard; Alain Mallard; Jérôme Marrot; Elisabeth Antic-Fidancev; Patrick Aschehoug; Daniel Vivien; Francis Sécheresse; Inorganic Chemistry 42 (2003) 2102–2108; doi:10.1021/ic020486f

data_4313341
_publ_contact_author
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        Pr. F. Secheresse
        Institut Lavoisier, IREM, UMR CNRS C 8637
        Universit\'e de Versailles Saint-Quentin-en-Yvelines
        45 Avenue des Etats Unis
        78035 Versailles cedex
        France
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_publ_contact_author_email       Secheres@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 1 39 25 43 81'
_publ_contact_author_phone       '(33) 1 39 25 43 83'
_publ_section_title
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 Solid-State and Solution Studies of {Lnn(SiW11O39)} Polyoxoanions: An
 Example of Building Block Condensation Dependent on the Nature of the
 Rare Earth
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2102
_journal_page_last               2108
_journal_paper_doi               10.1021/ic020486f
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'Cs4 K O44 Si W11 Yb'
_chemical_formula_weight         3498.22
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           31
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.4189(2)
_cell_length_b                   12.9208(2)
_cell_length_c                   11.29910(10)
_cell_measurement_reflns_used    15260
_cell_measurement_temperature    296(2)
_cell_volume                     2397.05(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Diamond Brandenburg'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_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  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16808
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    31.406
_exptl_absorpt_correction_T_max  0.2545
_exptl_absorpt_correction_T_min  0.0332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    4.847
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2978
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         5.521
_refine_diff_density_min         -2.988
_refine_diff_density_rms         0.640
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.00188(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6120
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0825P)^2^+25.5293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                5647
_reflns_number_total             6120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020486f_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4313341