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_7227281
_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 H11 O, 2(C6 H12 O)'
_chemical_formula_sum            'C38 H47 N6 O11 Zn3'
_chemical_formula_weight         959.92
_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                113.479(4)
_cell_angle_beta                 98.726(4)
_cell_angle_gamma                98.016(4)
_cell_formula_units_Z            1
_cell_length_a                   9.1743(4)
_cell_length_b                   10.8488(5)
_cell_length_c                   11.3458(5)
_cell_measurement_reflns_used    4265
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.4400
_cell_measurement_theta_min      7.5710
_cell_volume                     998.57(9)
_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)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.5148
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -113.00  -17.00   1.0000    1.9100
omega____ theta____ kappa____ phi______ frames
    -      -40.0194  -57.0000 -150.0000 96

  2 omega  -42.00   -8.00   1.0000    1.9100
omega____ theta____ kappa____ phi______ frames
    -      -40.0194   38.0000 -180.0000 34

  3 omega  -50.00   34.00   1.0000    1.9100
omega____ theta____ kappa____ phi______ frames
    -      -40.0194   38.0000    0.0000 84

  4 omega  -69.00   33.00   1.0000    1.9100
omega____ theta____ kappa____ phi______ frames
    -      -40.0194   57.0000   90.0000 102

  5 omega   25.00   97.00   1.0000    1.9100
omega____ theta____ kappa____ phi______ frames
    -       40.0194 -125.0000 -120.0000 72

  6 omega   35.00  122.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170 -125.0000  -60.0000 87

  7 omega   49.00  113.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170 -125.0000  150.0000 64

  8 omega  102.00  177.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170   30.0000  150.0000 75

  9 omega   37.00   90.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170  -30.0000 -120.0000 53

 10 omega   38.00   91.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170  -30.0000   30.0000 53

 11 omega   41.00   74.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170  -30.0000  120.0000 33

 12 omega  125.00  166.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170   61.0000    0.0000 41

 13 omega   87.00  176.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170   45.0000   60.0000 89

 14 omega   37.00   81.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170  -30.0000  -60.0000 44

 15 omega   35.00  123.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170  -61.0000  120.0000 88

 16 omega   34.00  141.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170  -77.0000  -60.0000 107

 17 omega -114.00  -10.00   1.0000    1.9100
omega____ theta____ kappa____ phi______ frames
    -      -40.0194  -57.0000   90.0000 104

 18 omega -119.00   -6.00   1.0000    1.9100
omega____ theta____ kappa____ phi______ frames
    -      -40.0194  -77.0000  -60.0000 113

 19 omega -114.00  -10.00   1.0000    1.9100
omega____ theta____ kappa____ phi______ frames
    -      -40.0194  -57.0000    0.0000 104

 20 omega   23.00   97.00   1.0000    1.9100
omega____ theta____ kappa____ phi______ frames
    -       40.0194 -125.0000 -180.0000 74

 21 omega   77.00  178.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170   30.0000   30.0000 101

 22 omega   74.00  178.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170   77.0000 -180.0000 104

 23 omega   46.00  178.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170   15.0000  -60.0000 132

 24 omega   74.00  129.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170   77.0000  -60.0000 55

 25 omega   74.00  178.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      107.4170   77.0000   90.0000 104
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0811031000
_diffrn_orient_matrix_UB_12      0.0173992000
_diffrn_orient_matrix_UB_13      0.1367374000
_diffrn_orient_matrix_UB_21      0.0232945000
_diffrn_orient_matrix_UB_22      0.1576313000
_diffrn_orient_matrix_UB_23      0.0522738000
_diffrn_orient_matrix_UB_31      -0.1523684000
_diffrn_orient_matrix_UB_32      -0.0066444000
_diffrn_orient_matrix_UB_33      0.0411098000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6536
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.993
_diffrn_reflns_theta_min         4.364
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75543
_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    1.596
_exptl_crystal_description       block
_exptl_crystal_F_000             495
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.905
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         6536
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0670
_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^)+(0.1342P)^2^+1.8220P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5766
_reflns_number_total             6536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ta10765b2.cif
_cod_data_source_block           FJU-31-Ch-lt
_cod_original_cell_volume        998.57(8)
_cod_database_code               7227281
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C1 H1 O1 N1 Zn1'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5282(19) 0.4718(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H6 of O6, All C(H,H) groups
 At 1.5 times of:
  H5 of O5
3. Restrained distances
 O6-C14
 1.4 with sigma of 0.02
 C14-C16
 1.5 with sigma of 0.02
 C16-C17
 1.5 with sigma of 0.02
 C17-C19
 1.5 with sigma of 0.02
 C19-C18
 1.5 with sigma of 0.02
 C18-C15
 1.5 with sigma of 0.02
 C15-C14
 1.5 with sigma of 0.02
 C16-C17
 1.5 with sigma of 0.02
 C14-C17
 2.5 with sigma of 0.04
 C14-C18
 2.5 with sigma of 0.04
 C16-C14 \\sim C16-C17 \\sim C17-C19 \\sim C18-C19 \\sim C18-C15 \\sim C15-C14
 with sigma of 0.02
 C15-C14 \\sim C16-C14 \\sim C16-C17 \\sim C17-C19 \\sim C18-C19 \\sim C18-C15
 with sigma of 0.02
 C18-C19 \\sim C18-C15 \\sim C15-C14 \\sim C16-C14 \\sim C16-C17 \\sim C17-C19
\\sim O6-C14
 with sigma of 0.02
 C16-C18 \\sim C14-C19 \\sim C15-C17
 with sigma of 0.02
4. Restrained planarity
 C16, O6, C14, C15, C17, C18, C19
 with sigma of 0.1
5. Rigid bond restraints
 O6, C14, C16, C15, H14, C17, H16A, H16B, H15A, H15B, C18, H17A, H17B, C19,
 H18A, H18B, H19A, H19B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
O6 \\sim C14 \\sim C16 \\sim C17 \\sim C19 \\sim C18 \\sim C15: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C17 \\sim O6 \\sim C14 \\sim C16 \\sim C15 \\sim H14 \\sim H16A \\sim H16B
\\sim H15A \\sim H15B \\sim C18 \\sim H17A \\sim H17B \\sim C19 \\sim H18A
\\sim H18B \\sim H19A \\sim H19B: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
7. Others
 Fixed Sof: O5(0.5) H5(0.5)
8.a Riding coordinates:
 O6(H6)
8.b Ternary CH refined with riding coordinates:
 C11(H11), C14(H14)
8.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C17(H17A,H17B), C16(H16A,H16B), C15(H15A,
 H15B), C18(H18A,H18B), C19(H19A,H19B)
8.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C4(H4), C10(H10), C3(H3), C9(H9)
8.e Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              48473
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'