Unusual adsorption behaviours and responsive structural dynamics via selective gate effects of an hourglass porous metal‒organic framework
Xiong, Ying; Fan, Yan-Zhong; Wei, Zhang-Wen; Chen, Cheng-Xia; Chen, Sha; Wang, Dawei; Barboiu, Mihail; Jiang, Ji-Jun; Su, Cheng-Yong; RSC Advances 9 (2019) 37222–; doi:10.1039/C9RA07301A

data_7235112
_publ_section_title
;
 Unusual adsorption behaviours and responsive structural dynamics via
 selective gate effects of an hourglass porous metal--organic framework
;
_journal_issue                   64
_journal_name_full               'RSC Advances'
_journal_page_first              37222
_journal_paper_doi               10.1039/C9RA07301A
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C14 H8 Cu N2 O5'
_chemical_formula_sum            'C14 H8 Cu N2 O5'
_chemical_formula_weight         347.76
_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 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-31 deposited with the CCDC.	2019-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            36
_cell_length_a                   17.9678(16)
_cell_length_b                   17.9678(16)
_cell_length_c                   69.263(10)
_cell_measurement_reflns_used    1388
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      55.7468
_cell_measurement_theta_min      3.1876
_cell_volume                     19365(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.0981
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            8016
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        55.813
_diffrn_reflns_theta_max         55.813
_diffrn_reflns_theta_min         3.819
_exptl_absorpt_coefficient_mu    1.599
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_description       Block
_exptl_crystal_F_000             6300
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
TITL 1 in R-3c
CELL   17.9678   17.9678   69.2630     90.00     90.00    120.00
SPGR R-3c
C101 0.469 0.144 0.081 !       0.96 eA-3
C102 0.155 0.156 0.250 !       0.82 eA-3
C103 0.346 0.783 0.430 !       0.81 eA-3
Q104 0.906 0.715 0.403 !       0.81 eA-3
Q105 0.800 0.238 0.429 !       0.80 eA-3
C106 0.264 0.794 0.402 !       0.79 eA-3
C107 0.888 0.813 0.473 !       0.78 eA-3
C108 0.252 0.269 0.242 !       0.78 eA-3
C109 0.546 0.907 0.165 !       0.77 eA-3
C110 0.905 0.999 0.024 !       0.75 eA-3
C111 0.645 0.562 0.078 !       0.75 eA-3
C112 0.767 0.270 0.109 !       0.74 eA-3
C113 0.876 0.998 0.492 !       0.74 eA-3
C114 0.752 1.000 0.226 !       0.73 eA-3
C115 0.099 0.936 0.776 !       0.73 eA-3
Q116 0.860 0.748 0.464 !       0.73 eA-3
C117 0.816 0.421 0.067 !       0.73 eA-3
C118 0.612 0.311 0.300 !       0.73 eA-3
C119 0.060 0.784 0.275 !       0.72 eA-3
C120 0.373 0.841 0.403 !       0.72 eA-3
C121 0.798 0.247 0.119 !       0.72 eA-3
C122 0.953 0.036 0.464 !       0.72 eA-3
C123 0.716 0.517 0.332 !       0.71 eA-3
C124 0.810 0.037 0.225 !       0.71 eA-3
C125 0.783 0.794 0.516 !       0.71 eA-3
C126 0.217 0.206 0.484 !       0.71 eA-3
Q127 0.365 0.217 0.398 !       0.70 eA-3
C128 0.429 0.854 0.944 !       0.70 eA-3
C129 0.206 0.564 0.211 !       0.70 eA-3
C130 0.876 0.529 0.821 !       0.70 eA-3
C131 0.528 0.141 0.836 !       0.69 eA-3
C132 0.174 0.248 0.016 !       0.69 eA-3
C133 0.778 0.844 0.012 !       0.68 eA-3
C134 0.222 0.156 0.988 !       0.68 eA-3
C135 0.048 0.175 1.001 !       0.68 eA-3
C136 0.688 0.455 0.340 !       0.68 eA-3
C137 0.833 0.346 0.339 !       0.67 eA-3
Q138 0.081 0.442 0.195 !       0.67 eA-3
Q139 0.546 0.663 0.267 !       0.67 eA-3
Q140 0.842 0.107 0.217 !       0.67 eA-3
C141 0.503 0.734 0.157 !       0.66 eA-3
C142 0.580 0.499 0.101 !       0.65 eA-3
Q143 0.623 0.719 0.383 !       0.65 eA-3
Q144 0.780 0.731 0.490 !       0.65 eA-3
C145 1.003 0.954 0.433 !       0.64 eA-3
C146 0.126 0.534 0.184 !       0.64 eA-3
C147 0.592 0.089 0.329 !       0.63 eA-3
Q148 0.886 0.585 0.847 !       0.63 eA-3
C149 0.484 0.153 0.832 !       0.63 eA-3
Q150 0.927 0.392 0.285 !       0.62 eA-3
Q151 0.480 0.219 0.376 !       0.62 eA-3
C152 0.433 0.251 0.840 !       0.62 eA-3
C153 0.411 0.620 0.457 !       0.61 eA-3
C154 0.925 0.074 0.470 !       0.61 eA-3
C155 0.669 0.284 0.767 !       0.61 eA-3
C156 0.593 0.344 0.078 !       0.60 eA-3
Q157 0.843 0.581 0.326 !       0.60 eA-3
C158 0.684 0.532 0.841 !       0.60 eA-3
Q159 0.247 0.203 0.020 !       0.60 eA-3
Q160 0.765 0.014 0.992 !       0.60 eA-3
Q161 0.765 0.830 0.491 !       0.60 eA-3
Q162 0.170 0.076 0.207 !       0.60 eA-3
Q163 0.594 0.843 0.008 !       0.59 eA-3
Q164 0.425 0.639 0.386 !       0.59 eA-3
C165 0.425 0.688 0.145 !       0.59 eA-3
Q166 0.347 0.045 0.495 !       0.59 eA-3
C167 0.431 0.782 0.439 !       0.58 eA-3
Q168 0.939 0.831 0.285 !       0.58 eA-3
C169 0.957 0.985 0.242 !       0.58 eA-3
Q170 0.359 0.781 0.388 !       0.58 eA-3
Q171 0.254 0.083 0.840 !       0.58 eA-3
Q172 0.979 0.096 0.783 !       0.58 eA-3
C173 0.025 0.074 0.047 !       0.58 eA-3
C174 0.661 0.377 0.890 !       0.58 eA-3
C175 0.956 0.967 0.016 !       0.58 eA-3
Q176 0.606 0.532 0.255 !       0.58 eA-3
C177 0.389 0.628 0.181 !       0.57 eA-3
C178 0.230 0.721 0.385 !       0.57 eA-3
C179 0.030 0.354 0.419 !       0.57 eA-3
Q180 0.760 0.156 0.356 !       0.57 eA-3
Q181 0.581 0.732 0.454 !       0.57 eA-3
Q182 0.726 0.118 0.413 !       0.57 eA-3
C183 0.689 0.282 0.882 !       0.56 eA-3
C184 0.311 0.718 0.118 !       0.56 eA-3
Q185 0.927 0.402 0.178 !       0.56 eA-3
Q186 0.343 0.390 0.501 !       0.56 eA-3
C187 0.764 0.562 0.074 !       0.55 eA-3
Q188 0.302 0.955 0.393 !       0.55 eA-3
Q189 0.828 0.534 0.441 !       0.55 eA-3
C190 0.796 0.925 0.004 !       0.54 eA-3
Q191 0.395 0.479 0.191 !       0.54 eA-3
C192 0.658 0.472 0.055 !       0.54 eA-3
Q193 0.093 0.656 0.122 !       0.54 eA-3
Q194 0.671 0.781 0.378 !       0.54 eA-3
C195 0.110 0.529 0.409 !       0.54 eA-3
C196 0.986 0.953 0.273 !       0.53 eA-3
Q197 0.232 0.861 0.092 !       0.53 eA-3
C198 0.760 0.996 0.008 !       0.53 eA-3
Q199 0.596 0.326 0.890 !       0.53 eA-3
;
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2649
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.1619
_refine_ls_R_factor_gt           0.1193
_refine_ls_shift/su_max          0.092
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3263
_refine_ls_wR_factor_ref         0.3650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1468
_reflns_number_total             2649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra07301a2.cif
_cod_data_source_block           1_CCDC1
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7235112
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.856
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 N1-C1A = C1A-C2A = C2A-C3A = C3A-C4A = C4A-C5 = C5-N1
 1.38 with sigma of 0.02
 N1-C1B = C1B-C2B = C2B-C3B = C3B-C4B = C4B-C5 = C5-N1
 1.38 with sigma of 0.02
3. Restrained planarity
 N2, C4A, C6A, O5A
 with sigma of 0.1
 N2, C4B, C6B, O5B
 with sigma of 0.1
 N1, C1A, C2A, C3A, C4A, C5, C6A
 with sigma of 0.02
 N1, C1B, C2B, C3B, C4B, C5, C6B
 with sigma of 0.02
4. Others
 Fixed Sof: C1A(0.5) H1A(0.5) C2A(0.5) H2A(0.5) C3A(0.5) H3A(0.5) C2B(0.5)
 H2B(0.5) C3B(0.5) H3B(0.5) C4A(0.5) C4B(0.5) H5A(0.5) H5B(0.5) C6A(0.5)
 C6B(0.5) H2AA(0.5) H2BB(0.5) O5A(0.5) O5B(0.5) C1B(0.5) H1B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C2B(H2B), C3B(H3B), C5(H5A), C5(H5B), C8(H8),
 C10(H10), C12(H12), N2(H2AA), N2(H2BB), C1B(H1B)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'