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_1561589
_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         'Cs5 O62 P2 W18'
_chemical_formula_sum            'Cs5 O62 P2 W18'
_chemical_formula_weight         5027.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_Hall           '-P 2ab 2a'
_space_group_name_H-M_alt        'P m m n :2'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-27
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.1713(15)
_cell_length_b                   16.5887(9)
_cell_length_c                   12.6541(6)
_cell_measurement_reflns_used    3410
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      29.1340
_cell_measurement_theta_min      2.4650
_cell_volume                     5073.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      153.15
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'Rigaku HyPix-6000 area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -27.00   0.00   0.50   34.92    --    5.00  45.00  60.00   54
  2  \w      9.00  39.00   0.50   34.92    --  -14.80  45.00   0.00   60
  3  \w   -100.00 -73.00   0.50   34.92    --  -14.80  45.00   0.00   54
  4  \w    -98.00  45.00   0.50   34.92    --  -14.80  45.00 150.00  286
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0206256000
_diffrn_orient_matrix_UB_12      -0.0021662000
_diffrn_orient_matrix_UB_13      -0.0397342000
_diffrn_orient_matrix_UB_21      -0.0088788000
_diffrn_orient_matrix_UB_22      0.0376882000
_diffrn_orient_matrix_UB_23      -0.0203335000
_diffrn_orient_matrix_UB_31      0.0188718000
_diffrn_orient_matrix_UB_32      0.0200836000
_diffrn_orient_matrix_UB_33      0.0339404000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22778
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.193
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              'Ultrax 18'
_exptl_absorpt_coefficient_mu    22.174
_exptl_absorpt_correction_T_max  0.02812
_exptl_absorpt_correction_T_min  0.00877
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    3.291
_exptl_crystal_description       prism
_exptl_crystal_F_000             4266
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.015
_refine_diff_density_max         3.419
_refine_diff_density_min         -2.283
_refine_diff_density_rms         0.471
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5010
_refine_ls_number_restraints     1300
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0969
_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^)+(0.1237P)^2^+539.6894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2643
_refine_ls_wR_factor_ref         0.2956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3219
_reflns_number_total             5010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nr01220g2.cif
_cod_data_source_block           exp_25_sq
_cod_depositor_comments
'Adding full bibliography for 1561588--1561590.cif.'
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               1561589
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Cs5P2W18O62
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Restrained distances
 W8-O28 \\sim W7-O30 \\sim W7-O30
 with sigma of 0.02
 Cs2-O1 \\sim Cs2A-O1
 with sigma of 0.02
 Cs1-O7 \\sim Cs1A-O7
 with sigma of 0.02
 Cs1-O43 \\sim Cs1A-O43
 with sigma of 0.02
 Cs1-O66 \\sim Cs1A-O66
 with sigma of 0.02
 Cs3-O14 \\sim Cs3A-O14
 with sigma of 0.02
 Cs3-O28 \\sim Cs3A-O28
 with sigma of 0.02
 Cs3-O22 \\sim Cs3A-O22
 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(Cs3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cs2A) \\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(W7)=Sof(W6)=Sof(W9)=Sof(W10)=Sof(O15)=Sof(O30)=Sof(O84)=Sof(O66)=Sof(O21)=
 Sof(O45)=1-FVAR(1)
 Sof(W8)=Sof(O20)=Sof(O28)=Sof(O43)=Sof(O57)=Sof(O26)=Sof(O31)=Sof(O24)=0.5*(1-
 FVAR(2))
 Sof(W2)=Sof(O17)=Sof(O19)=Sof(O1)=Sof(O5)=Sof(O2)=Sof(O6)=Sof(O14)=0.5*FVAR(2)
 Sof(W4)=Sof(W5)=Sof(W3)=Sof(W1)=Sof(O22)=Sof(O12)=Sof(O7)=Sof(O9)=Sof(O3)=
 Sof(O4)=FVAR(1)
 Sof(Cs1A)=0.5*(1-FVAR(3))
 Sof(Cs1)=0.5*FVAR(3)
 Sof(Cs3A)=0.125*(1-FVAR(4))
 Sof(Cs3)=0.125*FVAR(4)
 Sof(Cs2A)=0.125*(1-FVAR(5))
 Sof(Cs2)=0.125*FVAR(5)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69390
_shelx_fab_checksum              22460
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.836
_oxdiff_exptl_absorpt_empirical_full_min 0.452