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_7058216
_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         'C17 H14 Mn N3 O8, 3(H2 O)'
_chemical_formula_sum            'C17 H20 Mn N3 O11'
_chemical_formula_weight         497.30
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-15 deposited with the CCDC.    2019-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                91.380(2)
_cell_angle_beta                 111.018(2)
_cell_angle_gamma                117.458(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2225(3)
_cell_length_b                   11.0737(3)
_cell_length_c                   11.3556(2)
_cell_measurement_reflns_used    3504
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.8580
_cell_measurement_theta_min      4.6040
_cell_volume                     1036.54(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega -103.00   -5.00   0.5000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -77.0000 -180.0000 196

  2 omega   -4.00   77.00   0.5000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  150.0000 162

  3 omega   18.00  105.00   0.5000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000   90.0000 174

  4 omega   18.00  105.00   0.5000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000  -60.0000 174

  5 omega   -4.00   77.00   0.5000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000   30.0000 162

  6 omega   -1.00  109.00   0.5000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   19.0000 -120.0000 220

  7 omega   57.00  110.00   0.5000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000 -120.0000 106

  8 omega   -4.00   77.00   0.5000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000 -120.0000 162

  9 omega   57.00  110.00   0.5000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000   90.0000 106

 10 omega   -1.00  109.00   0.5000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   19.0000  120.0000 220

 11 omega   88.00  176.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000   90.0000 176

 12 omega   41.00   98.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -180.0000 114

 13 omega   51.00   99.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 96

 14 omega   44.00   87.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 86

 15 omega   53.00   89.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 72

 16 omega   79.00  107.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  120.0000 56

 17 omega   63.00  173.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000   60.0000 220

 18 omega   47.00  109.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   60.0000 124

 19 omega   40.00  102.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -30.0000 124

 20 omega   37.00   87.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 100

 21 omega  111.00  137.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 52

 22 omega  135.00  178.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -60.0000 86

 23 omega   40.00   72.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  120.0000 64

 24 omega   37.00   68.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 62

 25 omega   37.00   77.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 80

 26 omega  100.00  126.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -60.0000 52

 27 omega   72.00  125.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000   30.0000 106

 28 omega   69.00  114.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0370003000
_diffrn_orient_matrix_UB_12      0.1296657000
_diffrn_orient_matrix_UB_13      -0.0585998000
_diffrn_orient_matrix_UB_21      -0.1736877000
_diffrn_orient_matrix_UB_22      -0.0291703000
_diffrn_orient_matrix_UB_23      -0.0350329000
_diffrn_orient_matrix_UB_31      0.0580716000
_diffrn_orient_matrix_UB_32      0.0909537000
_diffrn_orient_matrix_UB_33      0.1327656000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7503
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         4.623
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.789
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71650
_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    1.593
_exptl_crystal_description       prism
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         3703
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0748P)^2^+0.3179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3316
_reflns_number_total             3703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj00400a1.cif
_cod_data_source_block           gkm8
_cod_depositor_comments
'Adding full bibliography for 7058215--7058216.cif.'
_cod_original_cell_volume        1036.55(6)
_cod_database_code               7058216
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C15H15O3N2Mn1
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.687
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups, All O(H,H,H,H) groups
2. Restrained distances
 O11-H11B
 0.9 with sigma of 0.02
3.a Riding coordinates:
 O7(H7A,H7B), O9(H9A,H9B,H10A,H10B), O10(H11A,H11B)
3.b Rotating group:
 O8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C16(H16), C17(H17),
 N2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'