Enhanced proton conductivity by guest molecules exchange in an acylamide-functionalized metal-organic framework
Feng, Zhen-Jie; Li, Jun-Jun; Sun, Jing; Wu, Xue-Song; Li, Ying; Wu, Di; Li, Shi-Hao; Wang, Xinlong; Su, Zhong-Min; Dalton Transactions  (2023) –; doi:10.1039/D3DT01028G

data_7712865
_publ_section_title
;
 Enhanced proton conductivity by guest molecules exchange in an
 acylamide-functionalized metal-organic framework
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01028G
_journal_year                    2023
_chemical_formula_moiety         'C64 H50 N12 Ni3 O24 S2, 2(C4 H9 N O), 32[H2O]'
_chemical_formula_sum            'C72 H132 N14 Ni3 O58 S2'
_chemical_formula_weight         2362.16
_chemical_name_systematic        CUST-736
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-11 deposited with the CCDC.	2023-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                104.388(7)
_cell_angle_beta                 96.648(8)
_cell_angle_gamma                106.752(9)
_cell_formula_units_Z            1
_cell_length_a                   11.273(2)
_cell_length_b                   16.660(3)
_cell_length_c                   16.747(3)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    173
_cell_measurement_theta_max      24.529
_cell_measurement_theta_min      2.329
_cell_volume                     2857.1(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1284
_diffrn_reflns_av_unetI/netI     0.0889
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            65915
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.551
_diffrn_reflns_theta_min         2.600
_diffrn_source_current           0.9
_diffrn_source_power             0.0405
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            'greenish green'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             1242
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         10197
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0642P)^2^+0.1731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1334
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6862
_reflns_number_total             10197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01028g2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2857.2(9)
_cod_database_code               7712865
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.825
_olex2_refinement_description
;
1. 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,H) groups
2. Restrained distances
 H00K-N00K
 0.741 with sigma of 0.001
 N8-C11
 1.421 with sigma of 0.001
 Ni02-H20A \\sim Ni02-H20B
 with sigma of 0.02
3.a Free rotating group:
 O20(H20A,H20B)
3.b Rotating group:
 O1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00M(H00M), C00R(H00R), C00S(H00S), C00X(H00X), C00Y(H00Y),
 C00Z(H00Z), C010(H010), C014(H014), C015(H015), C018(H018), C019(H019),
 C01B(H01B), C01C(H01C), C01D(H01D), C01I(H01I), C1(H1), C5(H5)
3.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3372
_shelx_fab_checksum              85398
_olex2_submission_special_instructions 'No special instructions were received'