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_4134611
_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         'C24 H15 N3 O6'
_chemical_formula_sum            'C24 H15 N3 O6'
_chemical_formula_weight         441.39
_chemical_name_systematic        PFC-13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-31
_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            48
_cell_length_a                   26.4904(10)
_cell_length_b                   41.3829(15)
_cell_length_c                   30.8788(12)
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.69
_cell_measurement_theta_min      2.34
_cell_volume                     33851(2)
_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      100.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1158
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            165583
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        21.720
_diffrn_reflns_theta_max         21.720
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1047 before and 0.0713 after correction.
The Ratio of minimum to maximum transmission is 0.9359.
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    1.039
_exptl_crystal_description       plate
_exptl_crystal_F_000             10944
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
TITL 1_a.res in Pbcn
CELL   26.4904   41.3829   30.8788     90.00     90.00     90.00
SPGR Pbcn
C101 0.014 0.684 0.299 !       5.76 eA-3
C102 0.015 0.300 0.206 !       5.39 eA-3
C103 0.048 0.328 0.203 !       4.12 eA-3
C104 0.930 0.659 0.160 !       3.95 eA-3
C105 0.953 0.664 0.201 !       3.87 eA-3
C106 0.430 0.838 0.151 !       3.53 eA-3
C107 0.063 0.241 0.172 !       2.93 eA-3
C108 0.899 0.749 0.191 !       2.74 eA-3
C109 0.508 0.306 0.335 !       2.65 eA-3
C110 0.967 0.741 0.156 !       2.64 eA-3
C111 0.471 0.678 0.345 !       2.29 eA-3
C112 0.272 0.594 0.149 !       2.24 eA-3
C113 0.547 0.543 0.366 !       2.16 eA-3
C114 0.343 0.454 0.191 !       2.15 eA-3
C115 0.953 0.810 0.309 !       2.12 eA-3
C116 0.555 0.568 0.374 !       2.08 eA-3
C117 0.618 0.744 0.330 !       2.06 eA-3
C118 0.662 0.439 0.225 !       1.99 eA-3
C119 0.366 0.718 0.155 !       1.93 eA-3
C120 0.968 0.056 0.376 !       1.92 eA-3
C121 0.899 0.912 0.349 !       1.92 eA-3
C122 0.032 0.068 0.126 !       1.92 eA-3
C123 0.438 0.351 0.343 !       1.89 eA-3
C124 0.915 0.749 0.156 !       1.86 eA-3
C125 0.303 0.514 0.184 !       1.85 eA-3
C126 0.280 0.424 0.332 !       1.82 eA-3
C127 0.391 0.450 0.149 !       1.81 eA-3
C128 0.421 0.404 0.310 !       1.77 eA-3
C129 0.288 0.429 0.287 !       1.76 eA-3
C130 0.967 0.205 0.183 !       1.72 eA-3
C131 0.662 0.573 0.325 !       1.71 eA-3
C132 0.322 0.557 0.153 !       1.68 eA-3
C133 0.722 0.567 0.341 !       1.67 eA-3
C134 0.891 0.841 0.128 !       1.57 eA-3
C135 0.690 0.522 0.329 !       1.56 eA-3
C136 0.943 0.088 0.335 !       1.53 eA-3
C137 0.085 0.074 0.175 !       1.52 eA-3
C138 0.500 0.663 0.156 !       1.51 eA-3
C139 0.447 0.343 0.189 !       1.50 eA-3
C140 0.946 0.956 0.161 !       1.47 eA-3
C141 0.803 0.992 0.313 !       1.47 eA-3
C142 0.554 0.252 0.194 !       1.46 eA-3
C143 0.546 0.285 0.279 !       1.44 eA-3
C144 0.505 0.736 0.171 !       1.44 eA-3
C145 0.781 0.015 0.277 !       1.43 eA-3
C146 0.139 0.842 0.368 !       1.39 eA-3
C147 0.099 0.072 0.155 !       1.35 eA-3
C148 0.118 0.117 0.271 !       1.34 eA-3
C149 0.838 0.835 0.153 !       1.30 eA-3
C150 0.335 0.696 0.143 !       1.28 eA-3
C151 0.089 0.211 0.164 !       1.26 eA-3
C152 0.806 0.023 0.234 !       1.25 eA-3
C153 0.622 0.265 0.149 !       1.23 eA-3
C154 0.608 0.586 0.191 !       1.20 eA-3
C155 0.600 0.377 0.124 !       1.16 eA-3
C156 0.331 0.709 0.153 !       1.12 eA-3
C157 0.500 0.327 0.334 !       1.12 eA-3
C158 0.508 0.337 0.323 !       1.11 eA-3
C159 0.858 0.792 0.140 !       1.10 eA-3
C160 0.929 0.932 0.147 !       1.09 eA-3
C161 0.077 0.085 0.138 !       1.07 eA-3
C162 0.612 0.634 0.299 !       1.01 eA-3
C163 0.089 0.126 0.284 !       1.00 eA-3
C164 0.030 0.147 0.361 !       1.00 eA-3
C165 0.656 0.643 0.298 !       0.99 eA-3
C166 0.971 0.062 0.333 !       0.97 eA-3
C167 0.444 0.796 0.180 !       0.96 eA-3
C168 0.335 0.637 0.150 !       0.93 eA-3
C169 0.170 0.156 0.146 !       0.92 eA-3
C170 0.596 0.432 0.312 !       0.91 eA-3
C171 0.421 0.387 0.356 !       0.90 eA-3
C172 0.445 0.276 0.350 !       0.90 eA-3
C173 0.359 0.313 0.360 !       0.90 eA-3
C174 0.431 0.433 0.309 !       0.89 eA-3
C175 0.093 0.093 0.278 !       0.89 eA-3
C176 0.391 0.485 0.333 !       0.88 eA-3
C177 0.803 0.043 0.662 !       0.88 eA-3
C178 0.197 0.957 0.338 !       0.88 eA-3
C179 0.883 0.816 0.120 !       0.88 eA-3
C180 0.897 0.139 0.259 !       0.87 eA-3
C181 0.302 0.534 0.850 !       0.86 eA-3
C182 0.079 0.960 0.138 !       0.85 eA-3
C183 0.361 0.669 0.144 !       0.84 eA-3
C184 0.950 0.901 0.165 !       0.82 eA-3
C185 0.979 0.196 0.280 !       0.82 eA-3
C186 0.842 0.164 0.326 !       0.81 eA-3
C187 0.319 0.421 0.359 !       0.81 eA-3
C188 0.671 0.562 0.294 !       0.81 eA-3
C189 0.471 0.678 0.181 !       0.80 eA-3
C190 0.493 0.639 0.181 !       0.80 eA-3
C191 0.453 0.545 0.854 !       0.80 eA-3
C192 0.608 0.379 0.318 !       0.80 eA-3
C193 0.935 0.290 0.362 !       0.80 eA-3
C194 0.444 0.382 0.320 !       0.79 eA-3
C195 0.791 0.056 0.274 !       0.79 eA-3
C196 0.872 0.180 0.359 !       0.79 eA-3
Q197 0.024 0.335 0.140 !       0.79 eA-3
C198 0.790 0.947 0.773 !       0.79 eA-3
C199 0.788 0.974 0.255 !       0.78 eA-3
;
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.071
_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     1729
_refine_ls_number_reflns         19985
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1345
_refine_ls_R_factor_gt           0.0783
_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^)+(0.1198P)^2^+72.8341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2187
_refine_ls_wR_factor_ref         0.2622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11493
_reflns_number_total             19985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02406_si_004.cif
_cod_data_source_block           PFC_13_sq
_cod_database_code               4134611
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H6 of O6, H8a of O8, H17 of O17, H24 of O24, H25 of O25,
  H28 of O28, H32a of O32
 At 1.5 times of:
  H2 of O2, H4 of O4, H10 of O10, H12a of O12, H14 of O14, H16a of O16, H20a
  of O20, H22a of O22, H30a of O30, H34 of O34, H36a of O36
2. Restrained planarity
 O14, H14, O9, O10, H10, O13
 with sigma of 0.02
 H17, O17, O18, O20, H20a, O19
 with sigma of 0.02
 O24, H24, O26, O25, H25, O23
 with sigma of 0.02
 O30, H30a, O31, O32, H32a, O29
 with sigma of 0.02
 O7, H6, O6, O5, H8a, O8
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6a), C8(H8), C9(H9), C12(H12), C13(H13), C15(H15), C16(H16),
 C19(H19), C20(H20), C22(H22), C23(H23), C29(H29), C30(H30), C32(H32), C33(H33),
  C36(H36), C37(H37), C39(H39), C40(H40), C43(H43), C44(H44), C46(H46),
 C47(H47), C53(H53), C54(H54), C56(H56), C57(H57), C60(H60), C61(H61), C63(H63),
  C64(H64), C67(H67), C68(H68), C70(H70), C71(H71), C77(H77), C78(H78),
 C80(H80), C81(H81), C84(H84), C85(H85), C87(H87), C88(H88), C91(H91), C92(H92),
  C94(H94), C95(H95), C101(H101), C102(H102), C104(H104), C105(H105),
 C108(H108), C109(H109), C111(H111), C112(H112), C115(H115), C116(H116),
 C118(H118), C119(H119), C125(H125), C126(H126), C128(H128), C129(H129),
 C132(H132), C133(H133), C135(H135), C136(H136), C139(H139), C140(H140),
 C142(H142), C143(H143)
3.b Fitted hexagon refined as free rotating group:
 N5(C27,N6,C25,N4,C26), N11(C75,N12,C73,N10,C74), N17(C123,N18,C121,N16,C122),
 C3(N3,C1,N1,C2,N2), C51(N9,C49,N7,C50,N8), C98(N14,C99,N15,C97,N13)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4), O6(H6), O8(H8a), O10(H10), O12(H12a), O14(H14), O16(H16a),
 O17(H17), O20(H20a), O22(H22a), O24(H24), O25(H25), O28(H28), O30(H30a),
 O32(H32a), O34(H34), O36(H36a)
;
_shelx_res_checksum              73009
_shelx_hkl_checksum              34471
_shelx_fab_checksum              10021
_olex2_submission_original_sample_id PFC-13
_olex2_submission_special_instructions 'No special instructions were received'