Cation-Directed Synthesis of Tungstosilicates. 2. Synthesis, Structure, and Characterization of the Open Wells-Dawson Anion α-[{K(H2O)2}(Si2W18O66)]15- and Its Transiton-Metal Derivatives [{M(H2O)}(μ-H2O)2K(Si2W18O66)]13- and [{M(H2O)}(μ-H2O)2K{M(H2O)4}(Si2W18O66)]11-
Nathalie Leclerc-Laronze; Jérôme Marrot; Gilbert Hervé; Inorganic Chemistry 44 (2005) 1275–1281; doi:10.1021/ic0486769

data_4308733
_publ_contact_author
;
Pr. G. Herv\'e
Institut Lavoisier, IREM, UMR 8637
Universit\'e de Versailles Saint-Quentin-en-Yvelines
45 Avenue des Etats Unis
78035 Versailles cedex
France
;
_publ_contact_author_email       herve@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 1 39 25 43 81'
_publ_contact_author_phone       '(33) 1 39 25 42 32'
_publ_section_title
;
Cation-Directed Synthesis of Tungstosilicates. 2. Synthesis, Structure, and
Characterization of the Open Wells-Dawson Anion
\a-[{K(H2O)2}(Si2W18O66)]15- and Its Transiton-Metal Derivatives
[{M(H2O)}(\m-H2O)2K(Si2W18O66)]13- and
[{M(H2O)}(\m-H2O)2K{M(H2O)4}(Si2W18O66)]11-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1275
_journal_page_last               1281
_journal_paper_doi               10.1021/ic0486769
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'K12 Mn2 O91 Si2 W18'
_chemical_formula_weight         5400.56
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.3780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.41420(10)
_cell_length_b                   23.5556(4)
_cell_length_c                   31.0844(5)
_cell_measurement_reflns_used    32228
_cell_measurement_temperature    296(2)
_cell_volume                     9033.6(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      296(2)
_diffrn_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_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  0.1588
_diffrn_reflns_av_sigmaI/netI    0.1718
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            62443
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         1.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.779
_exptl_absorpt_correction_T_max  0.0630
_exptl_absorpt_correction_T_min  0.0247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             9464
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.26
_refine_diff_density_max         3.975
_refine_diff_density_min         -3.727
_refine_diff_density_rms         0.582
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1180
_refine_ls_number_reflns         23577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0767
_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^)+(0.0649P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.1899
_reflns_number_gt                11592
_reflns_number_total             23577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0486769si20040929_110920_5.cif
_cod_data_source_block           1Mn2-K
_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 
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_cod_database_code               4308733