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_4134609
_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-11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_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                90.00
_cell_angle_beta                 92.334(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            52
_cell_length_a                   28.8499(8)
_cell_length_b                   30.8381(9)
_cell_length_c                   41.3583(12)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    100
_cell_measurement_theta_max      56.08
_cell_measurement_theta_min      2.95
_cell_volume                     36765.0(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0887
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            290327
_diffrn_reflns_theta_full        56.20
_diffrn_reflns_theta_max         56.20
_diffrn_reflns_theta_min         2.14
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.7510
_exptl_absorpt_correction_T_min  0.6693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1125 before and 0.0710 after correction.
The Ratio of minimum to maximum transmission is 0.8912.
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    1.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11856
_exptl_crystal_recrystallization_method 'solvothermal method'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.894
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3707
_refine_ls_number_reflns         47984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1453
_refine_ls_R_factor_gt           0.0941
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1417P)^2^+85.4027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2752
_refine_ls_wR_factor_ref         0.3182
_reflns_number_gt                26430
_reflns_number_total             47984
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0c02406_si_002.cif
_cod_data_source_block           PFC-11
_cod_database_code               4134609
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Riding coordinates:
 O15(H15), O13(H13), O17(H17), O3(H3), O6(H6), O1(H1), O29(H29), O27(H27),
 O25(H25), O7(H7), O0AA(H0AA), O11(H11A), O65(H65), O63(H63), O61(H61A),
 O55(H55), O57(H57), O59(H59A), O19(H19A), O10(H10), O21(H21A), O45(H45A),
 O47(H47), O43(H43A), O51(H51A), O53(H53A), O49(H49), O31(H31), O33(H33),
 O72(H72), O67(H67A), O69(H69A), O76(H76A), O78(H78A), O74(H74), O37(H37A),
 O41(H41), O39(H39)
2.b Aromatic/amide H refined with riding coordinates:
 C61(H61), C52(H52), C59(H59), C60(H60), C51(H51), C53(H53), C70(H70),
 C67(H67), C62(H62), C54(H54), C68(H68), C69(H69), C11(H11), C16(H16),
 C15(H15A), C20(H20), C12(H12), C22(H22), C6(H6A), C4(H4), C3(H3A), C19(H19),
 C21(H21), C5(H5), C100(H100), C102(H102), C101(H101), C117(H117), C111(H111),
 C116(H116), C99(H99), C115(H115), C112(H112), C107(H107), C108(H108),
 C118(H118), C28(H28), C37(H37), C38(H38), C30(H30), C35(H35), C43(H43),
 C29(H29A), C36(H36), C45(H45), C27(H27A), C46(H46), C44(H44), C244(H244),
 C259(H259), C253(H253), C252(H252), C260(H260), C261(H261), C254(H254),
 C246(H246), C243(H243), C245(H245), C251(H251), C262(H262), C205(H205),
 C203(H203), C204(H204), C211(H211), C212(H212), C213(H213), C206(H206),
 C196(H196), C214(H214), C198(H198), C195(H195), C197(H197), C92(H92), C84(H84),
  C82(H82), C76(H76), C83(H83), C91(H91), C85(H85), C93(H93), C90(H90),
 C75(H75), C78(H78), C77(H77), C171(H171), C189(H189), C181(H181), C172(H172),
 C187(H187), C173(H173), C174(H174), C180(H180), C190(H190), C179(H179),
 C182(H182), C188(H188), C220(H220), C229(H229), C238(H238), C237(H237),
 C236(H236), C221(H221), C228(H228), C230(H230), C222(H222), C235(H235),
 C227(H227), C219(H219), C124(H124), C123(H123), C125(H125), C134(H134),
 C142(H142), C133(H133), C132(H132), C141(H141), C131(H131), C139(H139),
 C140(H140), C126(H126), C277(H277), C268(H268), C283(H283), C269(H269),
 C275(H275), C267(H267), C270(H270), C285(H285), C278(H278), C276(H276),
 C286(H286), C284(H284), C293(H293), C309(H309), C300(H300), C308(H308),
 C292(H292), C307(H307), C301(H301), C310(H310), C294(H294), C299(H299),
 C291(H291), C302(H302), C149(H149), C147(H147), C163(H163), C157(H157),
 C158(H158), C150(H150), C166(H166), C165(H165), C148(H148), C164(H164),
 C156(H156), C155(H155)
2.c Fitted hexagon refined as free rotating group:
 C56(N9,C65,N7,C57,N8), C9(N1,C8,N2,C17,N3), C104(N16,C113,N14,C105,N15),
 C32(N5,C41,N6,C33,N4), C257(N34,C256,N32,C248,N33), C209(N27,C200,N26,C208,
 N28), C81(N13,C80,N11,C88,N12), C177(N19,C185,N17,C176,N18), N30(C233,N31,C224,
 N29,C232), C129(N24,C128,N23,C137,N25), C272(N35,C281,N36,C273,N37), N38(C304,
 N39,C296,N40,C305), N21(C153,N22,C161,N20,C152)
2.d Idealised tetrahedral OH refined as rotating group:
 O35(H35A)
;
_olex2_submission_original_sample_id PFC-11
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20