The Monolanthanide-Containing Silicotungstates [Ln(β2-SiW11O39)2]13- (Ln = La, Ce, Sm, Eu, Gd, Tb, Yb, Lu): A Synthetic and Structural Investigation
Bassem S. Bassil; Michael H. Dickman; Bernd von der Kammer; Ulrich Kortz; Inorganic Chemistry 46 (2007) 2452–2458; doi:10.1021/ic061737d

data_4307198
_publ_contact_author_address
; 
International University Bremen
School of Engineering and Science
P.O. Box 750 561
28725 Bremen
Germany
;
_publ_contact_author_email
;
u.kortz@iu-bremen.de
;
_publ_contact_author_fax
;
+49-421-200 3229
;
_publ_contact_author_name
;
Ulrich KORTZ
;
_publ_contact_author_phone
;
+49-421-200 3235
;
_publ_section_title
;
The Monolanthanide-Containing Silicotungstates [Ln(\b2-SiW11O39)2]13- (Ln =
La, Ce, Sm, Eu, Gd, Tb, Yb, Lu): A Synthetic and Structural Investigation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2452
_journal_page_last               2458
_journal_paper_doi               10.1021/ic061737d
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'H46 K10.5 O101 Si2 W22 Yb'
_chemical_formula_weight         6346.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   21.3738(5)
_cell_length_b                   38.3275(10)
_cell_length_c                   25.3172(7)
_cell_measurement_reflns_used    5089
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      22.55
_cell_measurement_theta_min      3.22
_cell_volume                     20740.0(9)
_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      163(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2062
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            288147
_diffrn_reflns_theta_full        24.62
_diffrn_reflns_theta_max         24.62
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    25.738
_exptl_absorpt_correction_T_max  0.6544
_exptl_absorpt_correction_T_min  0.2949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.065
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             22236
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.998
_refine_diff_density_min         -2.523
_refine_diff_density_rms         0.500
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         17459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0730P)^2^+2000.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1745
_reflns_number_gt                12618
_reflns_number_total             17459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061737dsi20061219_051007_8.cif
_cod_data_source_block           pbca
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 
;
_cod_original_formula_sum        'H46 K10.50 O101 Si2 W22 Yb'
_cod_database_code               4307198