Sandwich-Type Silicotungstates: Structure and Magnetic Properties of the Dimeric Polyoxoanions [{SiM2W9O34(H2O)}2]12- (M = Mn2+, Cu2+, Zn2+)
Ulrich Kortz; Samih Isber; Michael H. Dickman; Didier Ravot; Inorganic Chemistry 39 (2000) 2915–2922; doi:10.1021/ic000078g

data_4321067
_publ_contact_author_address
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Department of Chemistry
American University of Beirut
Bliss street, POB 11-0236
Beirut, LEBANON
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_publ_contact_author_email
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ulrich.kortz@aub.edu.lb
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_publ_contact_author_fax
;
+961 1 744 461
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_publ_contact_author_name
;
Ulrich KORTZ
;
_publ_contact_author_phone
;
+961 3 776 439
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_publ_section_title
;
 Sandwich-Type Silicotungstates: Structure and Magnetic Properties of the
 Dimeric Polyoxoanions [{SiM2W9O34(H2O)}2]12- (M = Mn2+, Cu2+, Zn2+)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2915
_journal_page_last               2922
_journal_paper_doi               10.1021/ic000078g
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'Cu4 K3 Na5 O96 Si2 W18'
_chemical_formula_weight         5387.9
_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                80.456(2)
_cell_angle_beta                 76.383(2)
_cell_angle_gamma                76.968(2)
_cell_formula_units_Z            1
_cell_length_a                   11.4271(12)
_cell_length_b                   12.5956(13)
_cell_length_c                   15.3223(16)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.46
_cell_measurement_theta_min      1.38
_cell_volume                     2073.3(4)
_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      203(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_sigmaI/netI    0.1071
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23973
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    26.189
_exptl_absorpt_correction_T_max  0.356
_exptl_absorpt_correction_T_min  0.164
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             2356
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.956
_refine_diff_density_min         -4.246
_refine_diff_density_rms         0.645
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         9942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0679P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                6982
_reflns_number_total             9942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000078g_3.cif
_cod_data_source_block           K3Na5[{SiCu2W9O34(H2O)}2]*26H2O
_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 
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_cod_database_code               4321067