Integrating molecular design and crystal engineering approaches in non-humidified intermediate-temperature proton conductors based on a Dawson-type polyoxometalate and poly(ethylene glycol) derivatives.
Ogiwara, Naoki; Tomoda, Masahiro; Miyazaki, Shotaro; Weng, Zhewei; Takatsu, Hiroshi; Kageyama, Hiroshi; Misawa, Toshiyuki; Ito, Takeru; Uchida, Sayaka; Nanoscale 13 (2021) 8049–8057; doi:10.1039/d1nr01220g

data_1561590
_publ_section_title
;
 Integrating molecular design and crystal engineering approaches in
 non-humidified intermediate-temperature proton conductors based on a
 Dawson-type polyoxometalate and poly(ethylene glycol) derivatives.
;
_journal_issue                   17
_journal_name_full               Nanoscale
_journal_page_first              8049
_journal_page_last               8057
_journal_paper_doi               10.1039/d1nr01220g
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'Cs2 O62 P2 W18, 3(Cs)'
_chemical_formula_sum            'Cs5 O62 P2 W18'
_chemical_formula_weight         5027.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-12-29 deposited with the CCDC.	2021-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.688(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.261(5)
_cell_length_b                   30.571(8)
_cell_length_c                   28.331(8)
_cell_measurement_reflns_used    38340
_cell_measurement_temperature    153
_cell_measurement_theta_max      30.6670
_cell_measurement_theta_min      1.7313
_cell_volume                     14393(7)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      153
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Saturn70 RC'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1588
_diffrn_reflns_av_unetI/netI     0.1174
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            109230
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.656
_exptl_absorpt_coefficient_mu    15.633
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.2720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            'clear whitish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whitish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.320
_exptl_crystal_description       block
_exptl_crystal_F_000             8532
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         5.999
_refine_diff_density_min         -6.575
_refine_diff_density_rms         0.588
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.582
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         25084
_refine_ls_number_restraints     2263
_refine_ls_restrained_S_all      1.537
_refine_ls_R_factor_all          0.1981
_refine_ls_R_factor_gt           0.1740
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4477
_refine_ls_wR_factor_ref         0.4733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16627
_reflns_number_total             25084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nr01220g2.cif
_cod_data_source_block           shelxl_sq
_cod_depositor_comments
'Adding full bibliography for 1561588--1561590.cif.'
_cod_database_code               1561590
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.146
_shelx_estimated_absorpt_t_min   0.146
_olex2_refinement_description
;
1. Restrained distances
 W16-O42 \\sim W18-O42 \\sim W18-O3 \\sim W20-O3 \\sim W20-O27 \\sim W16-O27
 with sigma of 0.02
 W9-O11 \\sim O11-W19
 with sigma of 0.02
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O20) \\sim Ueq, Uanis(O42) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cs8)=1-FVAR(1)
 Sof(Cs1)=FVAR(1)
 Fixed Sof: Cs3(0.5) Cs5(0.5) Cs6(0.5) Cs7(0.5)
 Fixed X: O4(0.130509) O53(0.089609)
 Fixed Y: O4(0.69499) O53(0.46187)
 Fixed Z: O4(0.25023) O53(0.1741)
6.a Everything fixed:
 O4, O53
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1765
_shelx_fab_checksum              27332
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'