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_4349883
_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         'C36 H32 N6 O6 Zn2, 1.5(C6), C3 H6'
_chemical_formula_sum            'C48 H38 N6 O6 Zn2'
_chemical_formula_weight         925.58
_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             2018-07-12
_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                 127.455(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.90(2)
_cell_length_b                   16.978(14)
_cell_length_c                   22.451(18)
_cell_measurement_reflns_used    24081
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      56.39
_cell_measurement_theta_min      2.201
_cell_volume                     8745(12)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_av_unetI/netI     0.1448
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20182
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.492
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  0.8937
_exptl_absorpt_correction_T_min  0.8027
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.279
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         7530
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.0911
_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^)+(0.1544P)^2^+25.2056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2521
_refine_ls_wR_factor_ref         0.2899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4830
_reflns_number_total             7530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00684a2.cif
_cod_data_source_block           1c6h12
_cod_database_code               4349883
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.802
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C47-C49 = C49-C45 = C45-C47 = C48-C50 = C50-C46 = C46-C48
 2.54 with sigma of 0.005
 C49-C48 = C50-C49 = C50-C45 = C46-C45 = C47-C46 = C48-C47
 1.53 with sigma of 0.005
 C41-C40 = C42-C41 = C43-C42 = C44-C43 = C44-C39 = C40-C39
 1.53 with sigma of 0.005
 C41-C39 = C39-C43 = C43-C41 = C40-C44 = C44-C42 = C42-C40
 2.54 with sigma of 0.005
3. Restrained angles
 C48-C47-C46
 fixed at 112 with sigma of 0.02
 C46-C47-C48
 fixed at 112 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uiso(C45) = Uiso(C50) = Uiso(C49) = Uiso(C48) = Uiso(C47) = Uiso(C46)
Uiso(C44) = Uiso(C43) = Uiso(C42) = Uiso(C41) = Uiso(C39) = Uiso(C40)
5. Others
 Fixed Sof: C39(0.5) C40(0.5) C41(0.5) C42(0.5) C43(0.5) C44(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B)
6.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N6(H6), C3(H3), C4(H4A), C6(H6A), C7(H7), C15(H15), C16(H16),
 C18(H18), C26(H26), C27(H27), C29(H29), C30(H30), C84(H84)
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_olex2_submission_special_instructions 'No special instructions were received'