Purely inorganic frameworks based on polyoxometalate clusters with abundant phosphate groups: single-crystal to single-crystal structural transformation and remarkable proton conduction.
Zhang, Shan; Lu, Ying; Sun, Xiu-Wei; Li, Zhuo; Dang, Tian-Yi; Zhang, Zhong; Tian, Hong-Rui; Liu, Shu-Xia; Chemical communications (Cambridge, England) 56 (2020) 391–394; doi:10.1039/c9cc08696j

data_7125641
_publ_section_title
;
 Purely inorganic frameworks based on polyoxometalate clusters with
 abundant phosphate groups: single-crystal to single-crystal structural
 transformation and remarkable proton conduction.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              391
_journal_page_last               394
_journal_paper_doi               10.1039/c9cc08696j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '0.5(Fe80 Mo192 Na64 O1156 P136), 54(O)'
_chemical_formula_sum            'Fe40 Mo96 Na32 O632 P68'
_chemical_formula_weight         24397.88
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-03-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-25 deposited with the CCDC.	2019-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.3329(12)
_cell_length_b                   27.3329(12)
_cell_length_c                   37.8621(14)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      2.59
_cell_volume                     28286(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            73586
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.065
_diffrn_reflns_theta_min         2.590
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.392
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.865
_exptl_crystal_description       block
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_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6960
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+461.1291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5905
_reflns_number_total             6960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08696j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7125640--7125641.cif.'
_cod_original_cell_volume        28286(3)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               7125641
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O10W) \\sim Ueq, Uanis(O12W) \\sim Ueq, Uanis(O9W) \\sim Ueq, Uanis(O8W)
\\sim Ueq, Uanis(O5W) \\sim Ueq, Uanis(O11W) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O4W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3WA) \\sim Ueq, Uanis(O3W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O6W) \\sim Ueq, Uanis(O13W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
2. Others
 Fixed Sof: O3W(0.5) O8W(0.5) O9W(0.5) O11W(0.5) O12W(0.25) O5W(0.5) O10W(0.5)
 O4W(0.125) O3WA(0.5) O7W(0.125) O13W(0.25) O6W(0.25)
;
_shelx_res_checksum              3312
_olex2_submission_special_instructions 'No special instructions were received'