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_7236419
_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, C2.02 H0.86 N0.58, 0.29(H O)'
_chemical_formula_sum            'C38.02 H25.15 Cu3 N9.58 O6.29'
_chemical_formula_weight         907.35
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-06
_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                   17.3245(3)
_cell_length_b                   17.3245(3)
_cell_length_c                   33.9396(6)
_cell_measurement_reflns_used    3208
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.5170
_cell_measurement_theta_min      4.4440
_cell_volume                     10186.6(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.977
_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  0.0400
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            14071
_diffrn_reflns_point_group_measured_fraction_full 0.850
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.065
_diffrn_reflns_theta_min         3.608
_exptl_absorpt_coefficient_mu    1.839
_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    1.183
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             3661
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Flack x determined using 2120 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8425
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0611
_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^)+(0.1125P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1790
_reflns_Friedel_coverage         0.632
_reflns_Friedel_fraction_full    0.696
_reflns_Friedel_fraction_max     0.642
_reflns_number_gt                6277
_reflns_number_total             8425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ta11242k2.cif
_cod_data_source_block           VOH
_cod_database_code               7236419
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C40-N11
 1.3 with sigma of 0.02
 C40-N11
 1.3 with sigma of 0.02
 N11-C40
 1.4 with sigma of 0.02
 C40-C37
 2.1 with sigma of 0.02
 C40-C41
 1.4 with sigma of 0.02
 C41-N11
 2.6 with sigma of 0.02
 N10-C39
 2 with sigma of 0.02
 C37-C39
 2 with sigma of 0.02
 C37-C39
 2.2 with sigma of 0.02
 C38-C37
 2.1 with sigma of 0.02
 N10_$1-N10
 1.5 with sigma of 0.02
 C37-C38
 2.2 with sigma of 0.02
3. Rigid bond restraints
 C41, C40, N11, C37, C39, C38, N10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C41 \\sim C40 \\sim N10 \\sim C37 \\sim N11 \\sim C39 \\sim C38: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(N10) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: C38(0.28829) H38(0.28829) N10(0.28829) C37(0.28829) H37(0.28829)
 N11(0.28829) C39(0.28829) H39(0.28829) C40(0.57658) C41(0.57658) O7(0.28829)
 H7(0.28829)
6.a :
 C38(N10,C37,N11,C39,C40,C41,O7,H7)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C8(H8), C34(H34), C17(H17), C30(H30), C38(H38), C37(H37),
 C39(H39)
6.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C1(H1A,H1B,H1C), C27(H27A,H27B,H27C), C5(H5A,H5B,H5C),
 C23(H23A,H23B,H23C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              91969
_shelx_hkl_checksum              94769
_olex2_submission_special_instructions 'No special instructions were received'