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_4349885
_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         '0.25(C144 H128 N24 O24 Zn8), 1.5(C7 H8)'
_chemical_formula_sum            'C46.5 H44 N6 O6 Zn2'
_chemical_formula_weight         913.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           73
_space_group_name_Hall           '-I 2b 2c'
_space_group_name_H-M_alt        'I b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-11 deposited with the CCDC.
2018-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6880(17)
_cell_length_b                   22.617(2)
_cell_length_c                   23.535(2)
_cell_measurement_reflns_used    3405
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.619
_cell_measurement_theta_min      2.301
_cell_volume                     8882.9(14)
_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 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25507
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.731
_exptl_absorpt_coefficient_mu    1.134
_exptl_absorpt_correction_T_max  0.8487
_exptl_absorpt_correction_T_min  0.8055
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4350
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0593P)^2^+79.7050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.1828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3285
_reflns_number_total             4350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00684a2.cif
_cod_data_source_block           1C7H8
_cod_original_cell_volume        8882.9(15)
_cod_original_formula_sum        'C46.50 H44 N6 O6 Zn2'
_cod_database_code               4349885
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.805
_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
2. Restrained distances
 C31-C32 = C38-C39
 1.5 with sigma of 0.01
 C32-C30 \\sim C32-C26 \\sim C39-C37 \\sim C39-C33
 with sigma of 0.01
3. Restrained planarity
 C2, C3, C4, C5, C6, C7
 with sigma of 0.1
 C2, C5, C8, C9, C10, C11
 with sigma of 0.1
 C26, C27, C28, C29, C30, C31, C32
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C38) =
Uanis(C39)
Uanis(C26) = Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30) = Uanis(C31) =
Uanis(C32)
5. Others
 Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=1-FVAR(1)
 Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=FVAR(1)
 Fixed Sof: C33(0.25) H33(0.25) C34(0.25) H34(0.25) C35(0.25) H35(0.25)
 C36(0.25) H36(0.25) C37(0.25) H37(0.25) C38(0.25) C39(0.25) H39A(0.25)
 H39B(0.25) H39C(0.25) C26(0.5) H26(0.5) C27(0.5) H27(0.5) C28(0.5) H28(0.5)
 C29(0.5) H29(0.5) C30(0.5) H30(0.5) C31(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 H32C(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C17(0.5) H17A(0.5) H17B(0.5)
 H17C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C20(H20), C21(H21), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30)
6.b Fitted hexagon refined as free rotating group:
 C33(C34,C35,C36,C37,C38), C26(C27,C28,C29,C30,C31)
6.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C25(H25A,H25B,H25C), C39(H39A,H39B,H39C), C32(H32A,H32B,
 H32C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'