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_7235110
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_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                   17.993(3)
_cell_length_b                   17.993(3)
_cell_length_c                   69.267(14)
_cell_measurement_reflns_used    563
_cell_measurement_temperature    435(2)
_cell_measurement_theta_max      59.1957
_cell_measurement_theta_min      2.8319
_cell_volume                     19421(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      435.15
_diffrn_measured_fraction_theta_full 0.779
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1102
_diffrn_reflns_av_unetI/netI     0.1027
_diffrn_reflns_Laue_measured_fraction_full 0.779
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_number            8927
_diffrn_reflns_point_group_measured_fraction_full 0.779
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         58.910
_diffrn_reflns_theta_min         3.110
_exptl_absorpt_coefficient_mu    1.594
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.070
_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
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       0.00013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3058
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.1962
_refine_ls_R_factor_gt           0.1294
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_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          0.3374
_refine_ls_wR_factor_ref         0.3791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1589
_reflns_number_total             3058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra07301a2.cif
_cod_data_source_block           a
_cod_original_cell_volume        19420(7)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7235110
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.857
_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-C1 = C1-C2A = C2A-C3A = C3A-C4A = C4A-C5A = C5A-N1
 1.4 with sigma of 0.02
 N1-C1 = C1-C2B = C2B-C3B = C3B-C4B = C4B-C5B = C5B-N1
 1.4 with sigma of 0.02
3. Restrained planarity
 N2, C6B, O1B, C4B
 with sigma of 0.02
 C6A, C4A, O1A, N2
 with sigma of 0.02
 N1, C1, C2A, C3A, C4A, C5A
 with sigma of 0.02
 N1, C1, C2B, C3B, C4B, C5B
 with sigma of 0.02
4. Others
 Sof(C5B)=Sof(H5B)=1-FVAR(1)
 Sof(C5A)=Sof(H5A)=FVAR(1)
 Fixed Sof: O1A(0.5) O1B(0.5) H2B(0.5) H2A(0.5) H1A(0.5) H1B(0.5) C2A(0.5)
 H2AA(0.5) C3A(0.5) H3A(0.5) C3B(0.5) H3B(0.5) C4A(0.5) C4B(0.5) C6A(0.5)
 C6B(0.5) C2B(0.5) H2BA(0.5)
 Fixed Uiso: C2B(0.1)
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2B), N2(H2A), C1(H1A), C1(H1B), C2A(H2AA), C3A(H3A), C3B(H3B), C5A(H5A),
 C5B(H5B), C8(H8), C10(H10), C12(H12), C2B(H2BA)
;
_shelx_res_checksum              50083