Lanthanoid-Containing Open Wells-Dawson Silicotungstates: Synthesis, Crystal Structures, and Properties
Lubin Ni; Firasat Hussain; Bernhard Spingler; Stephen Weyeneth; Greta R. Patzke; Inorganic Chemistry 50 (2011) 4944–4955; doi:10.1021/ic2001943

data_4325196
_publ_contact_author_address
;
University of Zurich
Institute of Inorganic Chemistry
Winterthurerstrasse 190
CH-8057 Zurich
Switzerland
;
_publ_contact_author_email       greta.patzke@aci.uzh.ch
_publ_contact_author_name        'Dr Greta R. Patzke'
_publ_section_title
;
 Lanthanoid-Containing Open Wells-Dawson Silicotungstates: Synthesis,
 Crystal Structures, and Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4944
_journal_page_last               4955
_journal_paper_doi               10.1021/ic2001943
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'Ca Cl Cs0.5 Gd4 Na2 O111.5 Si2 W18'
_chemical_formula_weight         5966.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 94.021(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.1719(4)
_cell_length_b                   20.7408(4)
_cell_length_c                   39.3620(8)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.7399
_cell_measurement_theta_min      2.5021
_cell_volume                     21314.1(7)
_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\o oscillation scan'
_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  0.0946
_diffrn_reflns_av_sigmaI/netI    0.1418
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            98695
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    22.180
_exptl_absorpt_correction_T_max  0.4707
_exptl_absorpt_correction_T_min  0.0541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    3.719
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             20756
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.396
_refine_diff_density_min         -4.210
_refine_diff_density_rms         0.452
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         26434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0347P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                15564
_reflns_number_total             26434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2001943_si_002_Gd1.cif
_cod_data_source_block           Gd_1
_cod_original_formula_sum        'Ca Cl Cs0.50 Gd4 Na2 O111.50 Si2 W18'
_cod_database_code               4325196