Record Complexity in the Polycatenation of Three Porous Hydrogen-bonded Organic Frameworks with Stepwise Adsorption Behaviors.
Li, Yu-Lin; Alexandrov, Eugeny V.; Yin, Qi; Li, Lan; Fang, Zhi-Bin; Yuan, Wenbing; Proserpio, Davide M.; Liu, Tian-Fu; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c02406

data_4134610
_publ_section_title
;
 Record Complexity in the Polycatenation of Three Porous Hydrogen-bonded
 Organic Frameworks with Stepwise Adsorption Behaviors.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c02406
_journal_year                    2020
_chemical_formula_moiety
'0.33(C24 H14 N3 O6), 0.33(C24 H16 N3 O6), 0.33(C24 H15 N3 O6)'
_chemical_formula_sum            'C24 H15 N3 O6'
_chemical_formula_weight         441.39
_chemical_name_systematic        PFC-12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   30.910
_cell_length_b                   27.384
_cell_length_c                   20.633
_cell_measurement_reflns_used    3973
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      58.55
_cell_measurement_theta_min      3.04
_cell_volume                     17464.585
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      272.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1268
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            40721
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        60.743
_diffrn_reflns_theta_max         60.743
_diffrn_reflns_theta_min         3.039
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.5701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1508 before and 0.0678 after correction.
The Ratio of minimum to maximum transmission is 0.7583.
The \l/2 correction factor is Not present.
;
_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    1.007
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
TITL 085_a.res in Cmca
CELL   30.9100   27.3840   20.6326     90.00     90.00     90.00
SPGR Cmca
C101 0.344 0.157 0.390 !       0.64 eA-3
C102 0.788 0.148 0.205 !       0.63 eA-3
C103 0.308 0.114 0.425 !       0.62 eA-3
C104 0.203 0.123 0.157 !       0.62 eA-3
C105 0.192 0.879 0.919 !       0.61 eA-3
C106 0.319 0.044 0.577 !       0.61 eA-3
C107 0.843 0.444 0.450 !       0.60 eA-3
C108 0.837 0.031 0.329 !       0.59 eA-3
C109 0.186 0.102 0.218 !       0.57 eA-3
C110 0.314 0.129 0.326 !       0.55 eA-3
C111 0.643 0.378 0.919 !       0.55 eA-3
C112 0.329 0.381 0.887 !       0.55 eA-3
C113 0.695 0.167 0.326 !       0.55 eA-3
C114 0.695 0.470 0.595 !       0.55 eA-3
C115 0.322 0.435 0.738 !       0.54 eA-3
C116 0.812 0.470 0.801 !       0.54 eA-3
C117 0.672 0.380 0.887 !       0.53 eA-3
C118 0.157 0.397 0.470 !       0.53 eA-3
C119 0.157 0.016 0.876 !       0.53 eA-3
C120 0.140 0.148 0.032 !       0.53 eA-3
C121 0.656 0.426 0.079 !       0.52 eA-3
C122 0.201 0.088 0.078 !       0.51 eA-3
C123 0.217 0.153 0.142 !       0.51 eA-3
C124 0.321 0.335 0.860 !       0.51 eA-3
C125 0.827 0.061 0.359 !       0.50 eA-3
C126 0.249 0.139 0.325 !       0.50 eA-3
C127 0.140 0.042 0.847 !       0.50 eA-3
;
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         6722
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1778
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1596P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2219
_refine_ls_wR_factor_ref         0.3022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2329
_reflns_number_total             6722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02406_si_003.cif
_cod_data_source_block           pfc_12_sq
_cod_original_cell_volume        17464.0
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               4134610
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.836
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1AA-H1AA
 0.84 with sigma of 0.02
3. Others
 Fixed Sof: H2(0.5)
4.a Riding coordinates:
 C42(H1AA,H2,H6)
4.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C32(H32), C18(H18), C10(H10), C9(H9), C17(H17), C3(H3), C37(H37),
 C31(H31), C4(H4), C40(H40), C25(H25), C11(H11), C38(H38), C20(H20), C12(H12),
 C26(H26), C19(H19)
4.c Idealised tetrahedral OH refined as rotating group:
 O5(H5), O9(H9A)
;
_shelx_res_checksum              85709
_shelx_hkl_checksum              69594
_shelx_fab_checksum              87558
_olex2_submission_original_sample_id PFC-12
_olex2_submission_special_instructions 'No special instructions were received'