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_2021403
_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
'Yb K8 Na2 [Yb (Ge W9 O34)2 (C O3) (H2 O1)3], 16H2 O1'
_chemical_formula_moiety         '0.25(C4 Ge8 K32 Na4 O372 W72 Yb16)'
_chemical_formula_sum            'C Ge2 K8 Na O93 W18 Yb4'
_chemical_formula_weight         5982.44
_chemical_name_systematic
;
Ytterbium octapotassiumdisodium
triaquacarbonato(germanotungstato)triyttrium hexadecahydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.037(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.2367(6)
_cell_length_b                   22.6726(5)
_cell_length_c                   20.1786(5)
_cell_measurement_reflns_used    13245
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0370
_cell_measurement_theta_min      3.5710
_cell_volume                     9495.3(4)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Xcalibur Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64358
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         3.374
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    26.687
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.185
_exptl_crystal_description       needle
_exptl_crystal_F_000             10356
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.748
_refine_diff_density_min         -2.935
_refine_ls_extinction_coef       0.0000051(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2017 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         9007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0420P)^2^+738.7803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                7562
_reflns_number_total             9007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3017sup1.cif
_cod_data_source_block           3a
_cod_database_code               2021403
_shelx_hkl_checksum              38227
_shelx_res_checksum              38540