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_7125640
_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 O1170.86 P136), 40(O)'
_chemical_formula_sum            'Fe40 Mo96 Na32 O625.43 P68'
_chemical_formula_weight         24292.76
_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             2019-04-01
_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                   27.3577(9)
_cell_length_b                   27.3577(9)
_cell_length_c                   38.0332(12)
_cell_measurement_reflns_used    9819
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.31
_cell_volume                     28465.7(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0683
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            79867
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.061
_diffrn_reflns_theta_max         25.061
_diffrn_reflns_theta_min         2.609
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.369
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.834
_exptl_crystal_description       block
_exptl_crystal_F_000             22895
_refine_diff_density_max         1.171
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         6311
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0422P)^2^+762.9777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5100
_reflns_number_total             6311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08696j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7125640--7125641.cif.'
_cod_original_cell_volume        28466(2)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               7125640
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O8W) \\sim Ueq, Uanis(O4W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O5W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2W) \\sim Ueq, Uanis(O6W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O3W) \\sim Ueq, Uanis(O3WA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O9WA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2. Others
 Fixed Sof: O6W(0.5) O7W(0.5) O5W(0.125) O4W(0.125) O8W(0.125) Na3(0.5)
 O10W(0.25) O9W(0.5) O3W(0.25) O3WA(0.25) O9WA(0.5)
;
_shelx_res_checksum              78220
_olex2_submission_special_instructions 'No special instructions were received'