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_7236417
_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             2016-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-22 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                   17.4696(5)
_cell_length_b                   17.4696(5)
_cell_length_c                   33.7023(9)
_cell_measurement_reflns_used    3272
_cell_measurement_temperature    100(10)
_cell_measurement_theta_max      71.8300
_cell_measurement_theta_min      4.4000
_cell_volume                     10285.5(5)
_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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
  1 omega  -96.00   -2.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.0749  125.0000  150.0000 94

  2 omega  -35.00   74.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.0749  -77.0000   30.0000 109

  3 omega   30.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -30.0000  -60.0000 61

  4 omega   33.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -45.0000   60.0000 66

  5 omega   30.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -30.0000 -120.0000 61

  6 omega   94.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  125.0000    0.0000 84

  7 omega   33.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3615  -45.0000  120.0000 66

  8 omega -117.00  -87.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.0749  -77.0000  120.0000 30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0413737000
_diffrn_orient_matrix_UB_12      0.0695432000
_diffrn_orient_matrix_UB_13      0.0181567000
_diffrn_orient_matrix_UB_21      0.0543545000
_diffrn_orient_matrix_UB_22      0.0543274000
_diffrn_orient_matrix_UB_23      -0.0224229000
_diffrn_orient_matrix_UB_31      -0.0556606000
_diffrn_orient_matrix_UB_32      0.0013312000
_diffrn_orient_matrix_UB_33      -0.0354530000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_unetI/netI     0.1166
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            15360
_diffrn_reflns_point_group_measured_fraction_full 0.889
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.330
_diffrn_reflns_theta_min         4.438
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.792
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22312
_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            red
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.688
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 1536 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.08(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.0813
_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^)+(0.1221P)^2^+16.0714P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2131
_refine_ls_wR_factor_ref         0.3106
_reflns_Friedel_coverage         0.719
_reflns_Friedel_fraction_full    0.780
_reflns_Friedel_fraction_max     0.719
_reflns_number_gt                4818
_reflns_number_total             8840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ta11242k2.cif
_cod_data_source_block           FJU-66a
_cod_original_cell_volume        10285.5(7)
_cod_database_code               7236417
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C1 H1 O1 N1 Cu1'
_reflns_odcompleteness_completeness 99.40
_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 C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C12(H12), C32(H32), C10(H10), C34(H34), C13(H13)
2.b Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C5(H5a,H5b,H5c), C23(H23a,H23b,H23c), C27(H27a,H27b,
 H27c), C1(H1a,H1b,H1c), C36(H36a,H36b,H36c)
;
_shelx_res_checksum              79263
_shelx_hkl_checksum              46045
_olex2_submission_special_instructions 'No special instructions were received'