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_7235111
_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, O'
_chemical_formula_sum            'C14 H8 Cu N2 O6'
_chemical_formula_weight         363.76
_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
_atom_sites_solution_primary     iterative
_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                   18.4309(18)
_cell_length_b                   18.4309(18)
_cell_length_c                   70.011(16)
_cell_measurement_reflns_used    1073
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      55.9978
_cell_measurement_theta_min      2.7661
_cell_volume                     20596(5)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            8429
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        55.942
_diffrn_reflns_theta_max         55.942
_diffrn_reflns_theta_min         3.043
_exptl_absorpt_coefficient_mu    1.556
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_description       block
_exptl_crystal_F_000             6588
_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   18.4309   18.4309   70.0110     90.00     90.00    120.00
SPGR R-3c
Q101 0.047 0.546 0.266 !       1.61 eA-3
C102 1.001 1.000 0.250 !       1.26 eA-3
Q103 0.800 0.156 0.132 !       1.20 eA-3
C104 0.031 0.453 0.443 !       1.06 eA-3
C105 0.497 0.907 0.434 !       1.04 eA-3
C106 0.549 0.578 0.440 !       1.03 eA-3
C107 0.968 0.810 0.235 !       1.02 eA-3
C108 0.110 0.483 0.426 !       0.98 eA-3
C109 0.562 0.440 0.050 !       0.95 eA-3
Q110 0.849 0.405 0.141 !       0.92 eA-3
C111 0.169 0.215 0.274 !       0.92 eA-3
C112 0.878 0.535 0.078 !       0.92 eA-3
C113 0.903 0.794 0.226 !       0.91 eA-3
C114 0.686 0.124 0.102 !       0.91 eA-3
C115 0.136 0.173 0.305 !       0.91 eA-3
C116 0.732 0.559 0.137 !       0.90 eA-3
C117 0.032 0.858 0.306 !       0.90 eA-3
C118 0.625 0.268 0.095 !       0.90 eA-3
C119 1.000 0.999 0.274 !       0.89 eA-3
C120 0.203 0.487 0.379 !       0.88 eA-3
C121 0.536 0.372 0.548 !       0.87 eA-3
C122 0.409 0.270 0.601 !       0.87 eA-3
Q123 0.260 0.375 0.398 !       0.85 eA-3
C124 0.251 0.156 0.187 !       0.85 eA-3
C125 0.838 0.844 0.249 !       0.84 eA-3
C126 0.074 0.031 0.230 !       0.84 eA-3
Q127 0.710 0.921 0.770 !       0.84 eA-3
C128 0.840 0.953 0.272 !       0.83 eA-3
C129 0.853 0.941 0.267 !       0.83 eA-3
C130 0.200 0.565 0.371 !       0.82 eA-3
C131 0.298 0.596 0.411 !       0.82 eA-3
C132 0.562 0.280 0.050 !       0.82 eA-3
C133 0.147 0.952 0.269 !       0.81 eA-3
C134 0.281 0.517 0.888 !       0.81 eA-3
C135 0.521 0.796 0.399 !       0.81 eA-3
C136 0.250 0.530 0.402 !       0.80 eA-3
C137 0.147 0.528 0.938 !       0.80 eA-3
C138 0.864 0.922 0.764 !       0.80 eA-3
C139 0.468 0.866 0.430 !       0.80 eA-3
C140 0.567 0.391 0.082 !       0.80 eA-3
C141 0.309 0.732 0.383 !       0.80 eA-3
Q142 0.527 0.563 0.490 !       0.80 eA-3
C143 0.197 0.608 0.954 !       0.80 eA-3
C144 0.735 0.159 0.090 !       0.80 eA-3
C145 0.252 0.795 0.406 !       0.78 eA-3
C146 0.119 0.168 0.777 !       0.77 eA-3
C147 0.170 0.516 0.413 !       0.76 eA-3
Q148 0.454 0.453 0.250 !       0.76 eA-3
Q149 0.012 0.455 0.043 !       0.74 eA-3
Q150 0.262 0.502 0.472 !       0.74 eA-3
C151 0.128 0.611 0.409 !       0.74 eA-3
C152 0.561 0.343 0.096 !       0.73 eA-3
Q153 0.615 0.985 0.414 !       0.72 eA-3
C154 0.152 0.950 0.280 !       0.72 eA-3
Q155 0.797 0.118 0.918 !       0.71 eA-3
Q156 0.089 0.485 0.485 !       0.71 eA-3
C157 0.766 0.488 0.043 !       0.71 eA-3
Q158 0.390 0.511 0.449 !       0.71 eA-3
C159 0.465 0.108 0.099 !       0.70 eA-3
C160 0.166 0.232 0.285 !       0.70 eA-3
Q161 0.244 0.411 0.383 !       0.70 eA-3
C162 0.634 0.778 0.407 !       0.70 eA-3
C163 0.985 0.779 0.264 !       0.70 eA-3
C164 0.253 0.486 0.153 !       0.69 eA-3
C165 0.564 0.941 0.414 !       0.69 eA-3
C166 0.408 0.690 0.367 !       0.68 eA-3
C167 0.394 0.657 0.464 !       0.67 eA-3
C168 0.998 0.077 0.214 !       0.67 eA-3
C169 0.218 0.643 0.926 !       0.67 eA-3
C170 0.272 0.231 0.753 !       0.67 eA-3
Q171 0.427 0.434 0.470 !       0.66 eA-3
Q172 0.262 0.893 0.358 !       0.66 eA-3
C173 0.395 0.129 0.584 !       0.66 eA-3
Q174 0.596 0.769 0.051 !       0.65 eA-3
C175 0.875 0.936 0.469 !       0.65 eA-3
Q176 0.357 0.206 0.916 !       0.65 eA-3
Q177 1.000 0.783 0.304 !       0.64 eA-3
C178 0.158 0.595 0.398 !       0.64 eA-3
Q179 0.409 0.359 0.074 !       0.63 eA-3
C180 0.048 0.269 0.016 !       0.63 eA-3
C181 0.952 0.731 0.984 !       0.63 eA-3
Q182 0.858 0.125 0.418 !       0.63 eA-3
C183 0.616 0.386 0.106 !       0.63 eA-3
C184 0.402 0.634 0.469 !       0.62 eA-3
C185 0.374 0.642 0.132 !       0.62 eA-3
C186 0.245 0.250 0.249 !       0.62 eA-3
C187 0.067 0.034 0.020 !       0.61 eA-3
C188 0.620 0.062 0.317 !       0.61 eA-3
Q189 0.578 0.671 0.372 !       0.61 eA-3
C190 0.030 0.768 0.280 !       0.61 eA-3
Q191 0.331 0.152 0.153 !       0.61 eA-3
Q192 0.455 0.841 0.458 !       0.61 eA-3
C193 0.889 0.109 0.249 !       0.61 eA-3
Q194 0.610 0.825 0.055 !       0.60 eA-3
C195 0.263 0.987 0.256 !       0.60 eA-3
Q196 0.853 0.170 0.110 !       0.60 eA-3
Q197 0.926 0.308 0.591 !       0.60 eA-3
C198 0.173 0.013 0.263 !       0.60 eA-3
C199 0.401 0.289 0.848 !       0.60 eA-3
;
_refine_diff_density_max         1.297
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2909
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.1133
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3015
_refine_ls_wR_factor_ref         0.3499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1995
_reflns_number_total             2909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra07301a2.cif
_cod_data_source_block           1_sq
_cod_original_cell_volume        20596(6)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7235111
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.860
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 C6A-O1A \\sim C6B-O1B
 with sigma of 0.02
 C6A-N2 \\sim C6B-N2
 with sigma of 0.02
 C4-C6A \\sim C4-C6B
 with sigma of 0.02
3. Restrained planarity
 N2, C6A, O1A, C4
 with sigma of 0.02
 O1B, C6B, C4, N2
 with sigma of 0.02
4. Others
 Fixed Sof: O1(0.5) O1A(0.7) O1B(0.3) O2W(0.5) H2A(0.7) H2B(0.3) C6A(0.7)
 C6B(0.3)
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2A), N2(H2B), C1(H1), C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C12(H12)
5.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,N1)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'