A heteropolytungstate based 2D layered porous framework with high proton conductivity.
Yang, Mengnan; Zhang, Yao; Ji, Shiyan; Li, Huafeng; Ma, Xinyi; Jin, Yuzhen; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; Chemical communications (Cambridge, England)  (2023) –; doi:10.1039/d3cc04517j

data_7132281
_publ_section_title
;
 A heteropolytungstate based 2D layered porous framework with high proton
 conductivity.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc04517j
_journal_year                    2023
_chemical_formula_moiety         '0.5(C80 H64 Bi4 N16 Na12 O274 Ru8 W64), 8(O)'
_chemical_formula_sum            'C40 H32 Bi2 N8 Na6 O145 Ru4 W32'
_chemical_formula_weight         9788.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-10-11 deposited with the CCDC.	2023-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.4190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.9756(4)
_cell_length_b                   22.7835(7)
_cell_length_c                   23.5537(6)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.75
_cell_measurement_theta_min      2.26
_cell_volume                     9629.2(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            80083
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.262
_diffrn_source_type              Microfocus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.256
_exptl_absorpt_correction_T_max  0.0214
_exptl_absorpt_correction_T_min  0.0053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0950 before and 0.0728 after correction. The Ratio of minimum to maximum transmission is 0.2477. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.376
_exptl_crystal_description       block
_exptl_crystal_F_000             8528
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.685
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1132
_refine_ls_number_reflns         17126
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0513P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12315
_reflns_number_total             17126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04517j2.cif
_cod_data_source_block           2270810
_cod_database_code               7132281
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.318
_shelx_estimated_absorpt_t_min   0.225
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O9W) \\sim Ueq, Uanis(O20W) \\sim Ueq, Uanis(O22W) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: Na3(0.5) Na4(0.5) O5W(0.5) O8W(0.5) O9W(0.5) O10W(0.5) O11W(0.5)
 O14W(0.5) O16W(0.5) O22W(0.5) Na5(0.5) O21W(0.5) O19W(0.5) O20W(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              29122
_shelx_fab_checksum              41130
_olex2_submission_special_instructions 'No special instructions were received'