A water-stable open-framework zirconium(iv) phosphate and its water-assisted high proton conductivity
Yu, Jing-Wei; Yu, Hai-Jiao; Yao, Zhi-Yuan; Li, Zi-Han; Ren, Qiu; Luo, Hong-Bin; Zou, Yang; Wang, Lifeng; Ren, Xiao-Ming; CrystEngComm 23 (2021) 6093–6097; doi:10.1039/D1CE00852H

data_7243261
_publ_section_title
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 A water-stable open-framework zirconium(iv) phosphate and its
 water-assisted high proton conductivity
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              6093
_journal_page_last               6097
_journal_paper_doi               10.1039/D1CE00852H
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         '0.5(F24 H16 O60 P12 Zr12), 10(H4 N)'
_chemical_formula_sum            'F12 H48 N10 O30 P6 Zr6'
_chemical_formula_weight         1629.62
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-02
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-26 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.593(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.502(2)
_cell_length_b                   7.5316(11)
_cell_length_c                   19.141(3)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.69
_cell_volume                     2181.0(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21056
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.643
_diffrn_reflns_theta_min         1.536
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.751
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4009
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1195 before and 0.0466 after correction.
The Ratio of minimum to maximum transmission is 0.5377.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.481
_exptl_crystal_description       needle
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.811
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.0098(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+5.0405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4666
_reflns_number_total             5031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00852h3.cif
_cod_data_source_block           t2
_cod_depositor_comments          'Adding full bibliography for 7243261.cif.'
_cod_original_cell_volume        2181.0(6)
_cod_database_code               7243261
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.710
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups, H2W of O2W, H2 of O8, H1W of O1W
 At 1.5 times of:
  H3W of O3W
2.a Riding coordinates:
 O8(H2), O3W(H3W), O2W(H2W), O1W(H1W), N2(H2A,H2B,H2C,H2D), N1(H1A,H1B,H1C,
 H1D), N4(H4A,H4B,H4C,H4D), N5(H5A,H5B,H5C,H5D), N3(H3A,H3B,H3C,H3D)
;
_shelx_res_checksum              31786
_shelx_hkl_checksum              83053
_olex2_submission_special_instructions 'No special instructions were received'