Rationally tuning host‒guest interactions to free hydroxide ions within intertrimerically cuprophilic metal‒organic frameworks for high OH− conductivity
Li, Ziyin; Zhang, Zhangjing; Ye, Yingxiang; Cai, Kaicong; Du, Fenfen; Zeng, Heng; Tao, Jin; Lin, Quanjie; Zheng, Ying; Xiang, Shengchang; Journal of Materials Chemistry A 5 (2017) 7816–; doi:10.1039/C6TA11242K

data_7236418
_publ_section_title
;
 Rationally tuning host--guest interactions to free hydroxide ions within
 intertrimerically cuprophilic metal--organic frameworks for high
 OH&#x2212; conductivity
;
_journal_issue                   17
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              7816
_journal_paper_doi               10.1039/C6TA11242K
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         'C36 H24 Cu3 N9 O6'
_chemical_formula_sum            'C36 H24 Cu3 N9 O6'
_chemical_formula_weight         869.26
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-11-12 deposited with the CCDC.
2017-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2079(3)
_cell_length_b                   17.2079(3)
_cell_length_c                   34.0361(10)
_cell_measurement_reflns_used    3208
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.5170
_cell_measurement_theta_min      4.4440
_cell_volume                     10078.5(4)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.1031
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            14517
_diffrn_reflns_point_group_measured_fraction_full 0.864
_diffrn_reflns_point_group_measured_fraction_max 0.818
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.089
_diffrn_reflns_theta_min         3.633
_exptl_absorpt_coefficient_mu    1.829
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45889
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1404 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.13(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8376
_refine_ls_number_restraints     323
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0400P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0.654
_reflns_Friedel_fraction_full    0.723
_reflns_Friedel_fraction_max     0.660
_reflns_number_gt                4320
_reflns_number_total             8376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ta11242k2.cif
_cod_data_source_block           FJU-66
_cod_database_code               7236418
_shelxl_version_number           2013-2
_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
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C8 \\sim C17 \\sim C16 \\sim C15 \\sim C10 \\sim C9 \\sim C11 \\sim C12 \\sim
C13 \\sim C14: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O1 \\sim N7 \\sim O2 \\sim C6 \\sim C7 \\sim C9 \\sim C10 \\sim C11 \\sim C12
\\sim C13 \\sim C14 \\sim C19 \\sim O4 \\sim N8 \\sim C15 \\sim C16 \\sim C17
\\sim C8 \\sim C18 \\sim O3: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C30) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C8) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
4.a Aromatic/amide H refined with riding coordinates:
 C34(H34), C13(H13), C30(H30), C12(H12), C17(H17), C8(H8)
4.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C1(H1A,H1B,H1C), C27(H27A,H27B,
 H27C), C36(H36A,H36B,H36C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              25130
_shelx_hkl_checksum              28387
_shelx_fab_checksum              18373
_olex2_submission_special_instructions 'No special instructions were received'