Synthesis and characterization of carbonate-encapsulated ytterbium- and yttrium-containing polyoxotungstates
Kaushik, Reetam; Khan, Imran; Saini, Mukesh Kumar; Hussain, Firasat; Sadakane, Masahiro; Acta Crystallographica Section C 74 (2018) 1355–1361; doi:10.1107/S2053229618011841

data_2021401
_publ_section_title
;
 Synthesis and characterization of carbonate-encapsulated ytterbium- and
 yttrium-containing polyoxotungstates
;
_journal_coeditor_code           JR3017
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1355
_journal_page_last               1361
_journal_paper_doi               10.1107/S2053229618011841
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
'Na12 [Na (C2 H3 O2) {Y2 (As W9 O33)2 (W2 O5) (C O3) (H2 O)3}], 22H2 O'
_chemical_formula_moiety         'As2 C3 Na12 O110 W20 Y2, 3(O)'
_chemical_formula_sum            'C3 As2 Na12 O113 W20 Y2'
_chemical_formula_weight         6124.57
_chemical_name_systematic
;
Dodecasodium
acetato(arsenotungstato)triaquacarbonato(ditungstato)sodiumdiyttrium
dodecahyrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                91.090(2)
_cell_angle_beta                 92.169(2)
_cell_angle_gamma                108.155(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3054(4)
_cell_length_b                   18.0281(6)
_cell_length_c                   22.4544(5)
_cell_measurement_reflns_used    10464
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9860
_cell_measurement_theta_min      3.0020
_cell_volume                     5111.7(3)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1031
_diffrn_reflns_av_unetI/netI     0.1264
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            69959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.847
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.979
_exptl_crystal_description       block
_exptl_crystal_F_000             5356
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.452
_refine_diff_density_min         -2.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         20134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+39.5926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                13492
_reflns_number_total             20134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3017sup1.cif
_cod_data_source_block           1a
_cod_depositor_comments
;

2019-09-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C6 As4 Na24 O226 W40 Y4'
_cod_original_formula_weight         12249.14
_cod_original_formula_moiety         'As4 C6 Na24 O220 W40 Y4, 6(O)'
_cod_original_formula_units_Z            1
_cod_database_code               2021401
_shelx_hkl_checksum              84615
_shelx_res_checksum              57283