Large Cluster Formation through Multiple Substitution with Lanthanide Cations (La, Ce, Nd, Sm, Eu, and Gd) of the Polyoxoanion [(B-α-AsO3W9O30)4(WO2)4]28-. Synthesis and Structural Characterization
Knut Wassermann; Michael T. Pope; Inorganic Chemistry 40 (2001) 2763–2768; doi:10.1021/ic001233u

data_4319748
_publ_section_title
;
 Large Cluster Formation through Multiple Substitution with Lanthanide
 Cations (La, Ce, Nd, Sm, Eu, and Gd) of the Polyoxoanion
 [(B-\a-AsO3W9O30)4(WO2)4]28-. Synthesis and Structural Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2763
_journal_page_last               2768
_journal_paper_doi               10.1021/ic001233u
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'As4 Ce4 H156 K N15 Na2 O190 W40'
_chemical_formula_weight         11706.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.861(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.335(2)
_cell_length_b                   19.618(2)
_cell_length_c                   33.380(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      0.89
_cell_volume                     17580(3)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.3223
_diffrn_reflns_av_sigmaI/netI    0.2937
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            199755
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         0.89
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    27.966
_exptl_absorpt_correction_T_max  0.4604
_exptl_absorpt_correction_T_min  0.2123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             20584
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.18
_refine_diff_density_max         4.774
_refine_diff_density_min         -6.057
_refine_diff_density_rms         0.844
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1262
_refine_ls_number_reflns         42949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.2467
_refine_ls_R_factor_gt           0.1005
_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^)+(0.0989P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.2533
_reflns_number_gt                18295
_reflns_number_total             42949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001233u_6.cif
_cod_data_source_block           KCe4As4W40
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        17580(2)
_cod_original_formula_sum        'H156 As4 Ce4 K N15 Na2 O190 W40'
_cod_database_code               4319748