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_7227279
_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         'C20 H12 N6 O8 Zn3, C6 H6 O2, 2(C4 H9 N O)'
_chemical_formula_sum            'C34 H36 N8 O12 Zn3'
_chemical_formula_weight         944.82
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                117.938(8)
_cell_angle_beta                 100.535(5)
_cell_angle_gamma                98.517(5)
_cell_formula_units_Z            1
_cell_length_a                   9.1768(5)
_cell_length_b                   10.9017(8)
_cell_length_c                   11.3961(9)
_cell_measurement_reflns_used    3873
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.9860
_cell_measurement_theta_min      4.5610
_cell_volume                     953.71(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      nitrogen
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -50.00   34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5749   38.0000  120.0000 84

  2 omega  -96.00   -2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5749  125.0000 -120.0000 94

  3 omega  -82.00   39.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5749   19.0000 -120.0000 121

  4 omega   23.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5749 -125.0000  -90.0000 74

  5 omega   23.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5749 -125.0000   60.0000 74

  6 omega   78.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   30.0000 -120.0000 100

  7 omega   30.00  139.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -77.0000 -150.0000 109

  8 omega   30.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -30.0000 -180.0000 61

  9 omega   24.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -94.0000    0.0000 85

 10 omega   33.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -45.0000   90.0000 66

 11 omega   30.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -30.0000  -60.0000 61

 12 omega   33.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -45.0000   30.0000 66

 13 omega   33.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615 -125.0000 -120.0000 88

 14 omega   33.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615 -125.0000   60.0000 88

 15 omega   30.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -30.0000  -30.0000 61

 16 omega   33.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -45.0000  -30.0000 66

 17 omega   30.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -30.0000   30.0000 61

 18 omega   24.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -94.0000  120.0000 85

 19 omega   78.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   30.0000  -30.0000 100

 20 omega    8.00  117.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5749   77.0000   30.0000 109

 21 omega   12.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5749   57.0000  -90.0000 102

 22 omega    8.00   87.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5749   77.0000 -180.0000 79

 23 omega   12.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5749   57.0000  150.0000 102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0697656000
_diffrn_orient_matrix_UB_12      0.0368720000
_diffrn_orient_matrix_UB_13      0.1500008000
_diffrn_orient_matrix_UB_21      -0.1574469000
_diffrn_orient_matrix_UB_22      0.0092905000
_diffrn_orient_matrix_UB_23      0.0273397000
_diffrn_orient_matrix_UB_31      -0.0421545000
_diffrn_orient_matrix_UB_32      -0.1616715000
_diffrn_orient_matrix_UB_33      -0.0479028000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6234
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         4.587
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.829
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       block
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.950
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         6234
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0810
_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^)+(0.1632P)^2^+2.8077P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2161
_refine_ls_wR_factor_ref         0.2326
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5139
_reflns_number_total             6234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ta10765b2.cif
_cod_data_source_block           FJU-31-Hq-lt
_cod_original_cell_volume        953.72(13)
_cod_database_code               7227279
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C1 H1 O1 N1 Zn1'
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.557(2) 0.443(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 C14-O6
 1.3 with sigma of 0.02
 O6-C14
 1.2 with sigma of 0.02
 O6_$1-C14_$1
 1.3 with sigma of 0.02
 O6_$1-C14_$1
 1.4 with sigma of 0.02
 C14_$1-O6_$1
 1.4 with sigma of 0.02
 C11-C12
 1.5 with sigma of 0.02
 C11-C12
 1.5 with sigma of 0.02
 N4-C10
 1.3 with sigma of 0.02
 N4-C9
 1.3 with sigma of 0.02
 C15-C13
 1.35 with sigma of 0.02
 C15-C13
 1.4 with sigma of 0.02
4. Rigid bond restraints
 C14, O6, C15, C13, C13, C15, C14, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, N2, N3, C17, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, C9, N4, C10, C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, N4, C10, C11, O5, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C13 \\sim O6 \\sim C14 \\sim C15 \\sim C13 \\sim C15 \\sim C14 \\sim O6: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
N1 \\sim N2 \\sim N3 \\sim C17 \\sim C16: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C9 \\sim N4 \\sim C10 \\sim C11 \\sim O5 \\sim C12: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
6.a Riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C8(H8), C3(H3), C16(H16), C17(H17), C15(H15), C13(H13)
6.c Tetrahedral OH refined with riding coordinates:
 O6(H6)
;
_shelx_res_checksum              64567
_olex2_submission_special_instructions 'No special instructions were received'