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_4349882
_publ_section_title
;
 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), 2(C6 H6)'
_chemical_formula_sum            'C48 H44 N6 O6 Zn2'
_chemical_formula_weight         931.63
_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             2018-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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                   17.2385(11)
_cell_length_b                   22.5360(14)
_cell_length_c                   23.4694(15)
_cell_measurement_reflns_used    3705
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.689
_cell_measurement_theta_min      2.286
_cell_volume                     9117.6(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17687
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         1.807
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_T_max  0.8090
_exptl_absorpt_correction_T_min  0.7325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4469
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0696P)^2^+40.3113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3430
_reflns_number_total             4469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00684a2.cif
_cod_data_source_block           1C6H6
_cod_database_code               4349882
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.732
_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
 C25-C24
 1.36 with sigma of 0.001
 C26-C25
 1.36 with sigma of 0.001
 C27-C26
 1.36 with sigma of 0.001
 C27-C26_$1
 1.36 with sigma of 0.001
 C26_$1-C25_$1
 1.36 with sigma of 0.001
 C25_$1-C24
 1.36 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C27) = Uanis(C26) = Uanis(C25) = Uanis(C24) = Uanis(C25) = Uanis(C26)
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C6(H6), C7(H7), C17(H17), C18(H18), C23(H23),
 C22(H22), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27)
4.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'