Proton conduction in two Cu/Zn dimer-based hydrogen-bonded supramolecular frameworks from imidazole multi-carboxylate
Wang, Qingxu; Ye, Zhejun; Shi, Guoqing; Guo, Kaimeng; Li, Gang; New Journal of Chemistry 44 (2020) 8098–8105; doi:10.1039/D0NJ01189D

data_7059524
_publ_section_title
;
 Proton conduction in two Cu/Zn dimer-based hydrogen-bonded supramolecular
 frameworks from imidazole multi-carboxylate
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8098
_journal_page_last               8105
_journal_paper_doi               10.1039/D0NJ01189D
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         '2(C44 H28 N8 O12 Zn2), H2 O'
_chemical_formula_sum            'C88 H58 N16 O25 Zn4'
_chemical_formula_weight         2000.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-16
_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.	2020-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.427(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.2580(8)
_cell_length_b                   13.3387(5)
_cell_length_c                   18.2492(8)
_cell_measurement_reflns_used    4619
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.6910
_cell_measurement_theta_min      4.1340
_cell_volume                     4197.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -84.00 -39.00   0.50    4.50    --  -33.50-176.00 131.00   90
  2  \w      3.00  29.00   0.50    4.50    --  -33.50  77.00  30.00   52
  3  \w     -7.00  34.00   0.50    4.50    --  -33.50  57.00  60.00   82
  4  \w    -58.00 -21.00   0.50    4.50    --  -33.50  77.00  30.00   74
  5  \w    -48.00  -8.00   0.50    4.50    --  -33.50  37.00-120.00   80
  6  \w     22.00 106.00   0.50    4.50    --   36.47  77.00 150.00  168
  7  \w     64.00 108.00   0.50    4.50    --   36.47 178.00-180.00   88
  8  \w     66.00 104.00   0.50    4.50    --   36.47  77.00   0.00   76
  9  \w     18.00  44.00   0.50    4.50    --   36.47  77.00   0.00   52
 10  \w     48.00  77.00   0.50    4.50    --   36.47 -99.00 -60.00   58
 11  \w     68.00  94.00   0.50    4.50    --   36.47  77.00 -90.00   52
 12  \w     -4.00  37.00   0.50    4.50    --   36.47 -99.00 -60.00   82
 13  \w     76.00 109.00   0.50    4.50    --   36.47 178.00   0.00   66
 14  \w     29.00  62.00   0.50    4.50    --   36.47 -99.00 150.00   66
 15  \w     52.00  80.00   0.50   25.00    --  108.00 -30.00 -30.00   56
 16  \w     47.00 107.00   0.50   25.00    --  108.00 -94.00 -90.00  120
 17  \w     37.00  90.00   0.50   25.00    --  108.00 -30.00-120.00  106
 18  \w     39.00  85.00   0.50   25.00    --  108.00 -30.00  90.00   92
 19  \w     57.00  86.00   0.50   25.00    --  108.00 -45.00-180.00   58
 20  \w     37.00  80.00   0.50   25.00    --  108.00 -30.00 -60.00   86
 21  \w     39.00  80.00   0.50   25.00    --  108.00 -30.00  30.00   82
 22  \w     38.00 101.00   0.50   25.00    --  108.00-111.00  60.00  126
 23  \w    150.00 176.00   0.50   25.00    --  108.00  45.00 -90.00   52
 24  \w     99.00 129.00   0.50   25.00    --  108.00  45.00 -90.00   60
 25  \w     86.00 176.00   0.50   25.00    --  108.00  77.00   0.00  180
 26  \w     45.00 128.00   0.50   25.00    --  108.00 -61.00-120.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0239538000
_diffrn_orient_matrix_UB_12      -0.0795691000
_diffrn_orient_matrix_UB_13      0.0455611000
_diffrn_orient_matrix_UB_21      -0.0013869000
_diffrn_orient_matrix_UB_22      0.0809706000
_diffrn_orient_matrix_UB_23      0.0595022000
_diffrn_orient_matrix_UB_31      -0.0860958000
_diffrn_orient_matrix_UB_32      0.0208865000
_diffrn_orient_matrix_UB_33      -0.0572102000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7278
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.864
_diffrn_reflns_theta_min         4.190
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7b (Rigaku Oxford Diffraction, 2015)
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    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         7278
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0522
_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^)+(0.1006P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5681
_reflns_number_total             7278
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9771\% 
 around [0.77 0.00 0.63] (reciprocal) or [0.71 -0.00 0.71] (direct)
;
_cod_data_source_file            d0nj01189d2.cif
_cod_data_source_block           20180112a_twin1_hklf4
_cod_depositor_comments
;Adding full bibliography for 7059524--7059525.cif.

 Adding full bibliography for 7059524--7059525.cif.
;
_cod_database_code               7059524
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C33H37O4N2Zn1
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.746
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7385(10)
 0.2615(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O7(0.25) H7A(0.25) H7B(0.25)
5.a Riding coordinates:
 O7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15),
 C18(H18), C19(H19), C20(H20), C21(H21), N1(H1)
5.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.912
_oxdiff_exptl_absorpt_empirical_full_min 0.729
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2