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_4319746
_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            'As8 Gd6 H266 Na40 O414 W80'
_chemical_formula_weight         24062.58
_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_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.606(1)
_cell_angle_beta                 74.030(1)
_cell_angle_gamma                62.996(1)
_cell_formula_units_Z            1
_cell_length_a                   19.448(1)
_cell_length_b                   19.630(1)
_cell_length_c                   29.277(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      1.16
_cell_volume                     9571.1(10)
_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 0.954
_diffrn_measured_fraction_theta_max 0.954
_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  0.0799
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            109265
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.16
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    25.804
_exptl_absorpt_correction_T_max  0.0479
_exptl_absorpt_correction_T_min  0.0120
_exptl_absorpt_correction_type   muli-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelogram
_exptl_crystal_F_000             10586
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.35
_refine_diff_density_max         4.688
_refine_diff_density_min         -5.652
_refine_diff_density_rms         0.623
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1376
_refine_ls_number_reflns         45662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+85.9831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1680
_reflns_number_gt                33484
_reflns_number_total             45662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001233u_4.cif
_cod_data_source_block           Gd3As4W40
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

2024-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         12031.29
_cod_original_formula_units_Z            2
_cod_original_cell_volume        9571.6(9)
_cod_original_formula_sum        'H133 As4 Gd3 Na20 O207 W40'
_cod_database_code               4319746