An unprecedented Zr-containing polyoxometalate tetramer with mixed trilacunary/dilacunary Keggin-type polyoxotungstate units
Zhang, Zhong; Wang, Yue-Lin; Yang, Guo-Yu; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618006538

data_2021256
_publ_section_title
;
 An unprecedented Zr-containing polyoxometalate tetramer with mixed
 trilacunary/dilacunary Keggin-type polyoxotungstate units
;
_journal_coeditor_code           JR3002
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618006538
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
'H6 K4 Na16 [Zr4 (Ge W10 O38)2 (P W9 O34)2], 37H2 O'
_chemical_formula_sum            'Ge2 H80 K4 Na16 O181 P2 W38 Zr4'
_chemical_formula_weight         11059.18
_chemical_name_systematic
;
Hexahydride tetrapotassium hexadecasodium
(germanodecatungstato)(phosphononatungstato)tetrazirconate
heptatriacontahydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 95.172(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.5605(13)
_cell_length_b                   11.4578(6)
_cell_length_c                   32.7134(13)
_cell_measurement_reflns_used    11245
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6118
_cell_measurement_theta_min      2.9478
_cell_volume                     8421.8(7)
_computing_cell_refinement
;
FRAMBO (Bruker, 2009)
;
_computing_data_collection
;
FRAMBO (Bruker, 2009)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2009)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4170
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_av_unetI/netI     0.1011
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            43361
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.058
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    26.699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09788
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.361
_exptl_crystal_description       block
_exptl_crystal_F_000             9692
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
;
_refine_diff_density_max         5.848
_refine_diff_density_min         -3.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         14781
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0829
_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^)+(0.0731P)^2^+1085.8478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.2054
_reflns_number_gt                10800
_reflns_number_total             14781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3002sup1.cif
_cod_data_source_block           I
_cod_database_code               2021256
_shelx_estimated_absorpt_t_min   0.050
_shelx_estimated_absorpt_t_max   0.175
_shelx_hkl_checksum              68960
_shelx_res_checksum              59462
_cod_database_fobs_code 2021256