CsCl-type inorganic cluster-based high-symmetry crystal built from {Mo4.55V7.45PO40}10.45− with high ratio of vanadium to molybdenum and {H2O0.3@K6(H2O)12}6+ clusters exhibiting proton conduction below the freezing point of water
Yao, Zhi-Yuan; Zhang, Guo-Qin; Zhang, Jin; Liu, Jian-Lan; Liu, Longwen; Ren, XiaoMing; Dalton Transactions  (2019) –; doi:10.1039/C9DT03960K

data_7701496
_publ_section_title
;
 CsCl-type inorganic cluster-based high-symmetry crystal built from
 {Mo4.55V7.45PO40}10.45&#x2212; with high ratio of vanadium to molybdenum
 and {H2O0.3@K6(H2O)12}6+ clusters exhibiting proton conduction below the
 freezing point of water
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03960K
_journal_year                    2019
_chemical_formula_moiety
' H12 Mo4.55 O42 V7.45, O4 P, 12(H2 O), 0.3(O), 6(K) [+ solvent]'
_chemical_formula_sum            'H36 K6 Mo4.55 O58.28 P V7.45'
_chemical_formula_weight         2050.37
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-10-27 deposited with the CCDC.	2019-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   10.6513(5)
_cell_length_b                   10.6513(5)
_cell_length_c                   10.6513(5)
_cell_measurement_reflns_used    6692
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.1460
_cell_measurement_theta_min      3.3130
_cell_volume                     1208.39(10)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0078
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16220
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.536
_diffrn_reflns_theta_min         3.313
_exptl_absorpt_coefficient_mu    3.200
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.818
_exptl_crystal_description       block
_exptl_crystal_F_000             994
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.884
_refine_diff_density_min         -2.013
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1095P)^2^+45.8405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2399
_refine_ls_wR_factor_ref         0.2424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                302
_reflns_number_total             328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03960k2.cif
_cod_data_source_block           1_sq
_cod_original_cell_volume        1208.39(17)
_cod_database_code               7701496
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.856
_shelx_estimated_absorpt_t_max   0.883
_shelx_res_checksum              93317
_shelx_fab_checksum              66627