Yttrium Polyoxometalates. Synthesis and Characterization of a Carbonate-Encapsulated Sandwich-Type Complex
Xikui Fang; Travis M. Anderson; Wade A. Neiwert; Craig L. Hill; Inorganic Chemistry 42 (2003) 8600–8602; doi:10.1021/ic0350842

data_4312839
_publ_section_title
;
 Yttrium Polyoxometalates. Synthesis and Characterization of a
 Carbonate-Encapsulated Sandwich-Type Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8600
_journal_page_last               8602
_journal_paper_doi               10.1021/ic0350842
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C H4 K6.5 Na4.5 O72 P2 W18 Y3'
_chemical_formula_weight         5163.62
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.8860(10)
_cell_angle_beta                 70.9690(10)
_cell_angle_gamma                65.5040(10)
_cell_formula_units_Z            4
_cell_length_a                   19.3845(13)
_cell_length_b                   22.8445(15)
_cell_length_c                   23.6383(15)
_cell_measurement_temperature    100(2)
_cell_volume                     8970.9(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_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  0.0814
_diffrn_reflns_av_sigmaI/netI    0.1190
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            160063
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    25.336
_exptl_crystal_density_diffrn    3.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8952
_refine_diff_density_max         8.063
_refine_diff_density_min         -5.135
_refine_diff_density_rms         0.681
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1353
_refine_ls_number_reflns         63490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+263.6471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1630
_reflns_number_gt                48973
_reflns_number_total             63490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0350842si20030912_115940.cif
_cod_data_source_block           xf731ns
_cod_original_formula_sum        'C H4 K6.50 Na4.50 O72 P2 W18 Y3'
_cod_database_code               4312839