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_4307196
_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            'Gd H27 K8.5 O91.5 Si2 W22'
_chemical_formula_weight         6081.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.586(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7494(10)
_cell_length_b                   20.0610(9)
_cell_length_c                   27.3796(14)
_cell_measurement_reflns_used    3490
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.45
_cell_measurement_theta_min      2.19
_cell_volume                     10208.2(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      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.2412
_diffrn_reflns_av_sigmaI/netI    0.1598
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            332104
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    25.785
_exptl_absorpt_correction_T_max  0.3899
_exptl_absorpt_correction_T_min  0.1107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.957
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             10562
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.882
_refine_diff_density_min         -6.882
_refine_diff_density_rms         0.737
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         24202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1853
_refine_ls_R_factor_gt           0.0879
_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^)+(0.1400P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2268
_refine_ls_wR_factor_ref         0.2846
_reflns_number_gt                11756
_reflns_number_total             24202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061737dsi20061219_051007_6.cif
_cod_data_source_block           p21c
_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 
;
_cod_original_formula_sum        'H27 Gd K8.50 O91.50 Si2 W22'
_cod_database_code               4307196