Effect of Imidazole Arrangements on Proton-Conductivity in Metal-Organic Frameworks.
Zhang, Feng-Ming; Dong, Long-Zhang; Qin, Jun-Sheng; Guan, Wei; Liu, Jiang; Li, Shun-Li; Lu, Meng; Lan, Ya-Qian; Su, Zhong-Min; Zhou, Hong-Cai; Journal of the American Chemical Society 139 (2017) 6183–6189; doi:10.1021/jacs.7b01559

data_4126096
_publ_section_title
;
 Effect of Imidazole Arrangements on Proton-Conductivity in Metal-Organic
 Frameworks.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6183
_journal_page_last               6189
_journal_paper_doi               10.1021/jacs.7b01559
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         '0.06(C918 H612 Fe54 N108 O234)'
_chemical_formula_sum            'C51 H34 Fe3 N6 O13'
_chemical_formula_weight         1106.39
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   27.696(5)
_cell_length_b                   27.696
_cell_length_c                   72.829(13)
_cell_measurement_reflns_used    7523
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.034
_cell_measurement_theta_min      2.231
_cell_volume                     48380(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.45
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       80
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            49893
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        23.162
_diffrn_reflns_theta_max         23.162
_diffrn_reflns_theta_min         1.693
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6556
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.684
_exptl_crystal_description       block
_exptl_crystal_F_000             10152
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
TITL 1         R -3 c       R = 0.17
CELL   27.6960   27.6960   72.8290     90.00     90.00    120.00
SPGR R-3c
C101 0.680 0.572 0.464 !       2.70 eA-3
C102 0.658 0.603 0.522 !       1.83 eA-3
C103 0.787 0.407 0.224 !       1.75 eA-3
C104 0.548 0.292 0.940 !       1.72 eA-3
C105 0.154 0.366 0.168 !       1.71 eA-3
C106 0.549 0.132 0.374 !       1.69 eA-3
C107 0.798 0.122-0.001 !       1.67 eA-3
C108 0.202 0.878 0.001 !       1.67 eA-3
C109 0.522 0.105 0.031 !       1.66 eA-3
C110 0.336 0.673 0.202 !       1.65 eA-3
C111 0.493 0.992 0.383 !       1.62 eA-3
C112 0.900 0.444 0.874 !       1.59 eA-3
C113 0.452 0.506 0.168 !       1.55 eA-3
C114 0.616 0.678 0.605 !       1.54 eA-3
C115 0.370 0.603 0.284 !       1.54 eA-3
C116 0.242 0.979 0.317 !       1.53 eA-3
C117 0.299 0.312 0.070 !       1.52 eA-3
C118 0.484 0.985 0.500 !       1.51 eA-3
C119 0.907 0.805 0.202 !       1.49 eA-3
C120 0.094 0.898 0.296 !       1.49 eA-3
C121 1.000 1.002 0.313 !       1.47 eA-3
C122 0.172 0.072 0.652 !       1.47 eA-3
C123 0.101 0.928 0.848 !       1.46 eA-3
C124 0.256 0.803 0.379 !       1.46 eA-3
C125 0.773 0.508 0.489 !       1.45 eA-3
C126 0.851 0.406 0.482 !       1.45 eA-3
C127 0.813 0.924 0.852 !       1.43 eA-3
C128 0.101 0.404 0.863 !       1.40 eA-3
Q129 0.054 0.595 0.223 !       1.39 eA-3
C130 0.999 1.001 0.051 !       1.36 eA-3
C131 0.280 0.024 0.243 !       1.35 eA-3
C132 0.492 0.021 0.508 !       1.34 eA-3
C133 0.744 0.885 0.293 !       1.34 eA-3
C134 0.523 0.047 0.382 !       1.33 eA-3
C135 0.337 0.702 0.855 !       1.33 eA-3
C136 0.569 0.145 0.378 !       1.32 eA-3
C137 0.978 0.234 0.945 !       1.31 eA-3
C138 0.663 0.664 0.249 !       1.30 eA-3
C139 0.743 0.553 0.610 !       1.28 eA-3
Q140 0.915 0.786 0.449 !       1.27 eA-3
C141 0.397 0.276 0.969 !       1.26 eA-3
C142 0.259 0.775 0.495 !       1.26 eA-3
Q143 0.642 0.541 0.074 !       1.25 eA-3
C144 1.000 0.976 0.164 !       1.24 eA-3
C145 0.329 0.707 0.976 !       1.24 eA-3
C146 0.446 0.116 0.277 !       1.22 eA-3
C147 0.814 0.400 0.975 !       1.22 eA-3
C148 0.508 0.232 0.691 !       1.21 eA-3
C149 0.867 0.421 0.992 !       1.21 eA-3
C150 0.992 0.312 0.238 !       1.20 eA-3
C151 0.008 0.091 0.257 !       1.20 eA-3
C152 0.151 0.336 0.222 !       1.19 eA-3
C153 0.721 0.844 0.965 !       1.19 eA-3
Q154 0.992 0.655 0.598 !       1.19 eA-3
C155 0.673 0.835 0.848 !       1.18 eA-3
C156 0.087 0.552 0.468 !       1.18 eA-3
C157 0.593 0.318 0.212 !       1.18 eA-3
C158 0.743 0.945 0.758 !       1.17 eA-3
Q159 0.828 0.968 0.546 !       1.17 eA-3
C160 0.758 0.522 0.995 !       1.17 eA-3
Q161 0.719 0.214 0.371 !       1.16 eA-3
C162 0.336 0.674 0.937 !       1.15 eA-3
Q163 0.010 0.673 0.929 !       1.15 eA-3
C164 0.063 0.681 0.394 !       1.14 eA-3
C165 0.632 0.633 0.250 !       1.14 eA-3
C166 0.922 0.767 0.727 !       1.14 eA-3
C167 0.769 0.073 0.836 !       1.13 eA-3
C168 0.386 0.921 0.926 !       1.13 eA-3
C169 0.588 0.168 0.194 !       1.12 eA-3
C170 0.806 0.943 0.304 !       1.11 eA-3
Q171 0.344 0.642 0.118 !       1.11 eA-3
C172 0.255 0.508 0.527 !       1.10 eA-3
C173 0.150 0.085 0.847 !       1.09 eA-3
C174 0.314 0.395 0.340 !       1.09 eA-3
C175 0.089 0.590 0.952 !       1.08 eA-3
C176 0.938 0.863 0.656 !       1.08 eA-3
C177 0.149 0.054 0.157 !       1.08 eA-3
C178 0.515 0.436 0.015 !       1.07 eA-3
C179 0.603 0.823 0.210 !       1.07 eA-3
Q180 0.398 0.811 0.216 !       1.06 eA-3
C181 0.164 0.585 0.981 !       1.06 eA-3
Q182 0.406 0.268 0.578 !       1.05 eA-3
Q183 0.539 0.827 0.919 !       1.05 eA-3
C184 0.632 0.139 0.202 !       1.04 eA-3
C185 0.376 0.313 0.071 !       1.04 eA-3
C186 0.242 0.490 0.832 !       1.04 eA-3
C187 0.768 0.313 0.976 !       1.04 eA-3
C188 0.774 0.310 0.457 !       1.04 eA-3
Q189 1.001 0.727 0.922 !       1.03 eA-3
Q190 0.750 0.263 0.884 !       1.03 eA-3
C191 0.257 0.743 0.196 !       1.03 eA-3
C192 0.991 0.907 0.891 !       1.03 eA-3
Q193 0.209 0.547 0.168 !       1.02 eA-3
Q194 0.877 0.789 0.367 !       1.02 eA-3
C195 0.642 0.305 0.509 !       1.02 eA-3
C196 0.069 0.516 0.913 !       1.02 eA-3
C197 0.132 0.229 0.792 !       1.02 eA-3
C198 0.893 0.790 0.323 !       1.01 eA-3
C199 0.275 0.779 0.476 !       1.01 eA-3
;
_refine_diff_density_max         1.066
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7570
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1210
_refine_ls_R_factor_gt           0.0991
_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^)+(0.0651P)^2^+1252.5900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2242
_refine_ls_wR_factor_ref         0.2382
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6087
_reflns_number_total             7570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b01559_si_003.cif
_cod_data_source_block           Im-Fe-MOF
_cod_original_cell_volume        48382(20)
_cod_database_code               4126096
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Shared sites
{N2, C2}
3. Restrained distances
 N1-C1 = C2-C1
 1.4 with sigma of 0.02
4. Restrained planarity
 N3, C5B, N4B, C4B, C3B
 with sigma of 0.1
 C3A, C4A, N4A, C5A, N3
 with sigma of 0.1
 N1, C1_$1, C1, N2_$1, N2
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
Uanis(C4A) \\sim Ueq, Uanis(C3B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.2
Uanis(C4B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(N4B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
Uanis(C1) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.2
Uanis(C26) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.2
Uanis(N2) = Uanis(C2)
6. Others
 Fixed Sof: N2(0.5) C5B(0.25) H5B(0.25) N4B(0.25) H4B(0.25) C4B(0.25)
 H4BA(0.25) C3B(0.25) H3B(0.25) N4A(0.75) H4A(0.75) C2(0.5) C3A(0.75) H3A(0.75)
 C4A(0.75) H4AA(0.75) C5A(0.75) H5A(0.75)
7.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C5B(H5B), N4B(H4B), C4B(H4BA), C3B(H3B), N4A(H4A), C1(H1), C3A(H3A),
 C4A(H4AA), C5A(H5A), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14), C16(H16),
 C18(H18), C21(H21), C22(H22), C24(H24), C25(H25)
7.b Fitted pentagon refined as free rotating group:
 N3(C5B,N4B,C4B,C3B)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'