Cation-Directed Synthesis of Tungstosilicates. 1. Syntheses and Structures of K10A-α-[SiW9O34].24H2O, of the Sandwich-Type Complex K10.75[Co(H2O)6]0.5[Co(H2O)4Cl]0.25A-α-[K2{Co(H2O)2}3(SiW9O34)2].32H2O and of Cs15[K(SiW11O39)2].39H2O
Nathalie Laronze; Jérôme Marrot; Gilbert Hervé; Inorganic Chemistry 42 (2003) 5857–5862; doi:10.1021/ic0342752

data_4314227
_publ_contact_author
;
     Pr. G. Herv\'e
     Institut Lavoisier, IREM, UMR CNRS C 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. 1. Syntheses and
 Structures of K10A-\a-[SiW9O34].24H2O, of the Sandwich-Type Complex
 K10.75[Co(H2O)6]0.5[Co(H2O)4Cl]0.25A-\a-[K2{Co(H2O)2}3(SiW9O34)2].32H2O
 and of Cs15[K(SiW11O39)2].39H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5857
_journal_page_last               5862
_journal_paper_doi               10.1021/ic0342752
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'Cs14 K O96 Si2 W22'
_chemical_formula_weight         7536.72
_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                96.6330(10)
_cell_angle_beta                 101.6260(10)
_cell_angle_gamma                117.731(10)
_cell_formula_units_Z            1
_cell_length_a                   12.07930(10)
_cell_length_b                   12.7145(2)
_cell_length_c                   19.3029(3)
_cell_measurement_reflns_used    6941
_cell_measurement_temperature    296(2)
_cell_volume                     2494.2(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_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    0.1756
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17585
_diffrn_reflns_theta_full        29.76
_diffrn_reflns_theta_max         29.76
_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    30.459
_exptl_absorpt_correction_T_max  0.2623
_exptl_absorpt_correction_T_min  0.0848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3213
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         4.903
_refine_diff_density_min         -7.677
_refine_diff_density_rms         0.832
_refine_ls_extinction_coef       0.000155(5)
_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   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         12386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1802
_reflns_number_gt                6702
_reflns_number_total             12386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0342752si20030318_055959_3.cif
_cod_data_source_block           3
_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_cell_volume        2494.23(6)
_cod_database_code               4314227