A flexible metal‒organic framework with adaptive pores for high column-capacity gas chromatographic separation
He, Chun-Ting; Ye, Zi-Ming; Xu, Yan-Tong; Xie, Yi; Lian, Xin-Lu; Zhang, Jie-Peng; Chen, Xiao-Ming; Inorganic Chemistry Frontiers 5 (2018) 2777–; doi:10.1039/C8QI00684A

data_4349886
_publ_section_title
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 A flexible metal--organic framework with adaptive pores for high
 column-capacity gas chromatographic separation
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2777
_journal_paper_doi               10.1039/C8QI00684A
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C36 H32 N6 O6 Zn2, 2(C1 H4 O1), 2(C O)'
_chemical_formula_sum            'C40 H48 N6 O10 Zn2'
_chemical_formula_weight         903.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2018-07-11 deposited with the CCDC.
2018-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.7490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.3668(17)
_cell_length_b                   16.5004(10)
_cell_length_c                   22.5401(13)
_cell_measurement_reflns_used    6786
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.686
_cell_measurement_theta_min      2.192
_cell_volume                     8453.5(9)
_computing_cell_refinement       'SAINT V6.36A (?, 2016)'
_computing_data_reduction        'SAINT V6.36A (?, 2016)'
_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      153.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21239
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.525
_exptl_absorpt_coefficient_mu    1.197
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.437
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         8234
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+28.7355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6885
_reflns_number_total             8234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00684a2.cif
_cod_data_source_block           1meoh
_cod_database_code               4349886
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.796
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O10-C40 = O9A-C39A = O9-C39 = O7-C37 = O7A-C37A = O8-C38
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C40A \\sim O10 \\sim C40 \\sim C39A \\sim O9A \\sim O9 \\sim C39: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C38 \\sim O8: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O7 \\sim C37 \\sim C37A \\sim O7A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(O10A)=Sof(H10A)=Sof(O9A)=Sof(H9A)=
 Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(1)
 Sof(O10)=Sof(H10)=Sof(O9)=Sof(H9)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
 Sof(C37A)=Sof(O7A)=1-FVAR(2)
 Sof(C37)=Sof(O7)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), C3(H3A), C4(H4), C6(H6), C7(H7), C15(H15), C16(H16), C18(H18),
  C19(H19), C27(H27), C28(H28), C30(H30), C31(H31)
5.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C40A(H40D,H40E,H40F), C39A(H39D,H39E,H39F)
5.c Idealised tetrahedral OH refined as rotating group:
 O10(H10), O9(H9), O10A(H10A), O9A(H9A)
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_shelx_res_checksum              30977
_shelx_hkl_checksum              91468
_olex2_submission_special_instructions 'No special instructions were received'