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_1561588
_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         'C3 Cs2 K0.5 O68 P2 W18'
_chemical_formula_sum            'C3 Cs2 K0.5 O68 P2 W18'
_chemical_formula_weight         4780.60
_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_Hall           'P 6c 2c'
_space_group_name_H-M_alt        'P 63 2 2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2020-12-14 deposited with the CCDC.	2021-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            2
_cell_length_a                   17.2090(3)
_cell_length_b                   17.2090(6)
_cell_length_c                   28.5570(5)
_cell_measurement_reflns_used    67347
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.316
_cell_measurement_theta_min      1.695
_cell_volume                     7324.1(3)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL rayonix-MX225-HS ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'rayonix-MX225-HS CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.61000
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            24097
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         26.316
_diffrn_reflns_theta_min         1.695
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.286
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. z. otwinowski et al. acta cryst. (2003), a59, 228-234 ]
;
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    2.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4087.00
_exptl_crystal_size_max          0.036
_exptl_crystal_size_mid          0.024
_exptl_crystal_size_min          0.018
_refine_diff_density_max         6.32
_refine_diff_density_min         -2.44
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2700 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.48(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_number_parameters     92
_refine_ls_number_reflns         6601
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1532
_refine_ls_R_factor_gt           0.1008
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1842P)^2^+132.9796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3464
_refine_ls_wR_factor_ref         0.3674
_reflns_Friedel_coverage         0.692
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.814
_reflns_number_gt                3530
_reflns_number_total             6601
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1nr01220g2.cif
_cod_data_source_block           test
_cod_depositor_comments
'Adding full bibliography for 1561588--1561590.cif.'
_cod_database_code               1561588
_shelx_res_checksum              26607