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_4313342
_publ_contact_author
;
        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
;
_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            'K0.5 Nd2.5 O59.5 Si W11'
_chemical_formula_weight         3382.59
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.8770(10)
_cell_angle_beta                 80.1520(10)
_cell_angle_gamma                82.9930(10)
_cell_formula_units_Z            2
_cell_length_a                   12.48240(10)
_cell_length_b                   12.7297(2)
_cell_length_c                   18.68150(10)
_cell_measurement_reflns_used    5096
_cell_measurement_temperature    296(2)
_cell_volume                     2901.14(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 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0724
_diffrn_reflns_av_sigmaI/netI    0.1432
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11202
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.068
_exptl_absorpt_correction_T_max  0.1970
_exptl_absorpt_correction_T_min  0.0652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            pale_pink
_exptl_crystal_density_diffrn    3.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2927
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.566
_refine_diff_density_min         -2.799
_refine_diff_density_rms         0.503
_refine_ls_extinction_coef       0.00020(2)
_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   0.908
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         8030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0052P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                5169
_reflns_number_total             8030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020486f_2.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_formula_sum        'K0.50 Nd2.50 O59.50 Si W11'
_cod_database_code               4313342