Caesium-templated lanthanoid-containing polyoxotungstates
Hussain, Firasat; Spingler, Bernhard; Conrad, Franziska; Speldrich, Manfred; Kögerler, Paul; Boskovic, Colette; Patzke, Greta R.; Dalton Transactions  (2009) 4423–4425; doi:10.1039/b902077b

data_7001425
_publ_section_title
;
 Caesium-templated lanthanoid-containing polyoxotungstates
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              4423
_journal_page_last               4425
_journal_paper_doi               10.1039/b902077b
_journal_year                    2009
_chemical_formula_sum            'As6 Cs3.3 H154 Na7.6 O314 Tb6 W63'
_chemical_formula_weight         18778.15
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.894(2)
_cell_angle_beta                 105.820(2)
_cell_angle_gamma                92.029(2)
_cell_formula_units_Z            2
_cell_length_a                   23.4119(5)
_cell_length_b                   25.1489(6)
_cell_length_c                   28.3380(6)
_cell_measurement_reflns_used    18964
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.8480
_cell_measurement_theta_min      2.2127
_cell_volume                     14598.8(6)
_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, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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  0.2624
_diffrn_reflns_av_sigmaI/netI    0.3375
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            236046
_diffrn_reflns_theta_full        23.82
_diffrn_reflns_theta_max         23.82
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    27.348
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             16054
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.476
_refine_diff_density_min         -3.991
_refine_diff_density_rms         0.687
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2009
_refine_ls_number_reflns         44840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.2533
_refine_ls_R_factor_gt           0.0980
_refine_ls_shift/su_max          0.061
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2351
_refine_ls_wR_factor_ref         0.3105
_reflns_number_gt                15375
_reflns_number_total             44840
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902077b.txt
_cod_data_source_block           fh18
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'H154 As6 Cs3.30 Na7.60 O314 Tb6 W63'
_cod_database_code               7001425