Water-assisted proton conductivity of two highly stable imidazole multi-carboxylate-based MOFs
Qin, Yin; Li, Yilin; Guo, Kaimeng; Tang, Huabiao; Hou, Lifen; Li, Gang; New Journal of Chemistry 43 (2019) 4859–; doi:10.1039/C9NJ00400A

data_7058215
_publ_section_title
;
 Water-assisted proton conductivity of two highly stable imidazole
 multi-carboxylate-based MOFs
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4859
_journal_paper_doi               10.1039/C9NJ00400A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         '0.5(C196 H124 N36 O48 Zn10), 5(H2 O)'
_chemical_formula_sum            'C98 H72 N18 O29 Zn5'
_chemical_formula_weight         2292.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-21 deposited with the CCDC.    2019-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1821(3)
_cell_length_b                   35.3003(4)
_cell_length_c                   13.25738(19)
_cell_measurement_reflns_used    9342
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.4900
_cell_measurement_theta_min      4.1630
_cell_volume                     9445.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega -100.00  -40.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000    0.0000 120

  2 omega  -76.00  -15.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000   60.0000 122

  3 omega  -22.00   34.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -19.0000 -150.0000 112

  4 omega   57.00   82.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000  -90.0000 50

  5 omega   59.00  107.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000   60.0000 96

  6 omega  -32.00    2.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -57.0000  150.0000 68

  7 omega   45.00   71.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -19.0000 -150.0000 52

  8 omega   71.00  102.00   0.5000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000  150.0000 62

  9 omega   56.00   86.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 60

 10 omega   45.00   90.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 90

 11 omega   43.00   90.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   90.0000 94

 12 omega   47.00   78.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   60.0000 62

 13 omega   39.00   90.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 102

 14 omega   43.00  104.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 122

 15 omega   91.00  156.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  150.0000 130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0601276000
_diffrn_orient_matrix_UB_12      0.0097431000
_diffrn_orient_matrix_UB_13      -0.0667503000
_diffrn_orient_matrix_UB_21      -0.0460226000
_diffrn_orient_matrix_UB_22      0.0205886000
_diffrn_orient_matrix_UB_23      -0.0747682000
_diffrn_orient_matrix_UB_31      0.0097551000
_diffrn_orient_matrix_UB_32      0.0372055000
_diffrn_orient_matrix_UB_33      0.0588561000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24558
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.561
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.612
_exptl_crystal_description       prism
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         8415
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0753P)^2^+4.9480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6788
_reflns_number_total             8415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj00400a1.cif
_cod_data_source_block           20180113
_cod_depositor_comments
'Adding full bibliography for 7058215--7058216.cif.'
_cod_database_code               7058215
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C33H37O4N2Zn1
_shelx_estimated_absorpt_t_max   0.777
_shelx_estimated_absorpt_t_min   0.692
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H,H) groups
2. Restrained distances
 H3-O3
 0.86 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N9) = Uanis(N9A)
Uanis(C45) = Uanis(C45A)
Uanis(C46) = Uanis(C46A)
Uanis(C47) = Uanis(C47A)
Uanis(C48) = Uanis(C48A)
4. Others
 Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47A)=Sof(N9A)=1-FVAR(1)
 Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=Sof(N9)=FVAR(1)
 Fixed Sof: C48(0.5) H48(0.5) C48A(0.5) C49(0.5)
5.a Riding coordinates:
 O12(H12), O13(H13A), O15(H15A,H15B)
5.b Free rotating group:
 O14(H14A,H14B)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16),
 C19(H19), C20(H20), C21(H21), C22(H22), C30(H30), C31(H31), C32(H32), C33(H33),
  C35(H35), C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43),
 C44(H44), C45(H45), C45A(H45A), C46(H46), C46A(H46A), C47(H47), C47A(H47A),
 C48(H48)
;
_olex2_submission_special_instructions 'No special instructions were received'