Metal–organic frameworks with a large breathing effect to host hydroxyl compounds for high anhydrous proton conductivity over a wide temperature range from subzero to 125 Â°C
Ye, Yingxiang; Wu, Xiuzhen; Yao, Zizhu; Wu, Ling; Cai, Zetao; Wang, Lihua; Ma, Xiuling; Chen, Qian-Huo; Zhang, Zhangjing; Xiang, Shengchang; J. Mater. Chem. A 4 (2016) 4062–4070; doi:10.1039/c5ta10765b

data_7227277
_publ_section_title
;
 Metal--organic frameworks with a large breathing effect to host hydroxyl
 compounds for high anhydrous proton conductivity over a wide temperature
 range from subzero to 125 \^A\%C
;
_journal_issue                   11
_journal_name_full               'J. Mater. Chem. A'
_journal_page_first              4062
_journal_page_last               4070
_journal_paper_doi               10.1039/c5ta10765b
_journal_volume                  4
_journal_year                    2016
_chemical_formula_moiety         'C12 H12 N22 O12 Zn5'
_chemical_formula_sum            'C12 H12 N22 O12 Zn5'
_chemical_formula_weight         983.29
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-12 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5031(4)
_cell_length_b                   15.5031(4)
_cell_length_c                   12.0934(4)
_cell_measurement_reflns_used    2133
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.8510
_cell_measurement_theta_min      4.6050
_cell_volume                     2906.60(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.2574
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega -113.00  -87.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0194 -153.0000    2.0000 26

  2 omega -115.00  -31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0194  -77.0000 -150.0000 84

  3 omega   36.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4170  -30.0000  150.0000 30

  4 omega   49.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4170  -30.0000 -150.0000 42

  5 omega  106.00  166.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4170  121.0000 -115.0000 60

  6 omega   34.00   76.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4170  -30.0000 -180.0000 42

  7 omega   32.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4170  -30.0000   90.0000 59

  8 omega -114.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0194  -57.0000   60.0000 104

  9 omega -114.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0194  -57.0000  -60.0000 104
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0292792000
_diffrn_orient_matrix_UB_12      -0.0908913000
_diffrn_orient_matrix_UB_13      -0.0352804000
_diffrn_orient_matrix_UB_21      0.0814027000
_diffrn_orient_matrix_UB_22      -0.0390217000
_diffrn_orient_matrix_UB_23      0.0532804000
_diffrn_orient_matrix_UB_31      -0.0487263000
_diffrn_orient_matrix_UB_32      -0.0104024000
_diffrn_orient_matrix_UB_33      0.1101936000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4140
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.959
_diffrn_reflns_theta_min         4.637
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.247
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         1434
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0412P)^2^+3.7347P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1210
_reflns_number_total             1434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ta10765b2.cif
_cod_data_source_block           FJU-30
_cod_original_cell_volume        2906.58(17)
_cod_database_code               7227277
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C1 H1 Zn1 N1'
_shelx_estimated_absorpt_t_max   0.734
_shelx_estimated_absorpt_t_min   0.558
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(N6)=Sof(O3)=Sof(O2)=Sof(O1)=1-FVAR(1)
 Sof(N6A)=Sof(O3A)=Sof(O2A)=Sof(O1A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C1(H1)
;
_shelx_res_checksum              44420
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'