data_shelx_a
_audit_creation_date               2023-09-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      
;
College of Chemistry and Molecular Engineering, Beijing National Laboratory for Molecular Sciences, 
Peking University, Beijing 100871, People's Republic of China.
;
_audit_contact_author_email        ?
_audit_contact_author_name         ?
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_contact_author_name          'Zeyue Zhang'
_publ_contact_author_address       
;
College of Chemistry and Molecular Engineering, 
Beijing National Laboratory for Molecular Sciences, Peking University, Beijing 100871, People's Republic of China.
;
_publ_contact_author_email         'thuliumzhang@pku.edu.cn'
_publ_requested_journal            'Nature Chemistry'
_publ_section_title                'Three-Dimensional Covalent Organic Frameworks Constructed from Irregular Polyhedral Building Blocks'
_publ_author_name
;
Jianhong Chang, Zeyue Zhang, Haorui Zheng, Hui Li, Jinquan Suo, Chunqing Ji,
Fenqian Chen, Valentin Valtchev, Shilun Qiu, Junliang Sun and Qianrong Fang
;
_publ_author_address
;
1. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, Changchun 130012, 
People's Republic of China. E-mail: qrfang@jlu.edu.cn or postlh@jlu.edu.cn 
2. College of Chemistry and Molecular Engineering, Beijing National Laboratory for Molecular Sciences, 
Peking University, Beijing 100871, People's Republic of China. E-mail: junliang.sun@pku.edu.cn 
3.Department of Chemical and Biomolecular Engineering, National University of Singapore, Singapore 117585
4.Qingdao Institute of Bioenergy and Bioprocess Technology, Chinese Academy of Sciences.
189 Song Ling Rd, Qingdao, Shandong 266101, People's Republic of China 
5.Normandie Univ, ENSICAEN, UNICAEN, CNRS, Laboratoire Catalyse et Spectrochimie, 14050 Caen, France 
;
_publ_section_abstract
;
The development of three-dimensional (3D) covalent organic frameworks (COFs) has paramount significance 
across numerous applications. However, the conventional design approach that relies on regular building 
blocks significantly restricts the structural diversity of COFs. In this study, we have successfully 
designed and synthesized two 3D COFs, named JUC-643 and JUC-644, employing a novel strategy based on 
irregular 8-connected (8-c) building blocks. By using continuous rotation electron diffraction 
technique combined with powder X-ray diffraction patterns, their structural characterization reveals a 
unique linkage with double helical structure, a phenomenon previously unreported in COFs. In order to 
precisely describe the topology, these structures should be deconstructed into the unprecedented 
[4+3(+2)]-c nets instead of the traditional [8(+2)]-c or [6(+2)]-c net. Furthermore, JUC-644 has 
demonstrated exceptional adsorption capability towards C3H8 and n-C4H10 (11.28 and 10.45 mmol g-1 
at 298 K and 1 bar respectively), surpassing the adsorption performance of all known porous materials, 
and breakthrough experiments have also highlighted the remarkable C3H8/C2H6 and n-C4H10/C2H6 selectivity. 
This pioneering concept of incorporating irregular building blocks in 3D COFs introduces a promising 
avenue for the design of intricate architectures while enhancing their potential application in the 
recovery of C2H6 from natural gas liquids.
;
_publ_section_references
;
D. Kratzert, I. Krossing, (2018), J. Appl. Cryst. 51, 928-934. 

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Kratzert, D., Holstein, J.J. & Krossing, I. (2015). J. Appl. Cryst. 48, 933-938.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C0.347 N0.038'
_chemical_formula_sum              'C0.35 N0.04'
_chemical_formula_weight           4.70
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'orthorhombic'
_space_group_IT_number             54
_space_group_name_H-M_alt          'P c c a'
_space_group_name_Hall             '-P 2a 2ac'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z'
 '-x, y, -z+1/2'
 'x+1/2, -y, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y, -z'
 'x, -y, z-1/2'
 '-x-1/2, y, z-1/2'

_cell_length_a                     31.320(6)
_cell_length_b                     17.390(4)
_cell_length_c                     25.020(5)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       13627(5)
_cell_formula_units_Z              852
_cell_measurement_reflns_used      2093
_cell_measurement_temperature      100
_cell_measurement_theta_max        0.479
_cell_measurement_theta_min        0.041
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      0.000
_exptl_absorpt_correction_T_max    ?
_exptl_absorpt_correction_T_min    ?
_exptl_absorpt_correction_type     none
_exptl_absorpt_process_details     ?
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'yellow'
_exptl_crystal_density_diffrn      0.488
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         'macroscople yellow powder. rectangle under the observation in TEM (~500 nm)'
_exptl_crystal_F_000               813
_exptl_crystal_size_max            0.00200
_exptl_crystal_size_mid            0.00200
_exptl_crystal_size_min            0.00050
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.2774
_diffrn_reflns_av_unetI/netI       0.1094
_diffrn_reflns_Laue_measured_fraction_full  0.967
_diffrn_reflns_Laue_measured_fraction_max  0.967
_diffrn_reflns_limit_h_max         22
_diffrn_reflns_limit_h_min         -22
_diffrn_reflns_limit_k_max         11
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -17
_diffrn_reflns_number              40277
_diffrn_reflns_point_group_measured_fraction_full  0.967
_diffrn_reflns_point_group_measured_fraction_max  0.967
_diffrn_reflns_theta_full          0.479
_diffrn_reflns_theta_max           0.479
_diffrn_reflns_theta_min           0.041
_diffrn_ambient_temperature        100
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.967
_diffrn_measured_fraction_theta_max  0.967
_diffrn_measurement_device_type    'multiwire proportional'
_diffrn_measurement_method         'continuous rotational electron diffraction'
_diffrn_radiation_monochromator    graphite
_diffrn_radiation_type             '200 kV electron'
_diffrn_radiation_wavelength       0.0251
_diffrn_standards_number           2613
_diffrn_standards_interval_time    0.00833
_diffrn_source                     ?
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  1762
_reflns_number_total               2613
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement    'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution      'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max           0.128
_refine_diff_density_min           -0.295
_refine_diff_density_rms           0.059
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.811
_refine_ls_hydrogen_treatment      undef
_refine_ls_matrix_type             full
_refine_ls_number_parameters       158
_refine_ls_number_reflns           2613
_refine_ls_number_restraints       51
_refine_ls_R_factor_all            0.2649
_refine_ls_R_factor_gt             0.2286
_refine_ls_restrained_S_all        1.810
_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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.4951
_refine_ls_wR_factor_ref           0.5182
_refine_special_details            ?
_olex2_refinement_description
;
1. Restrained distances
 C1A-C1B = C1D-C1E = C1E-C1F
 1.37 with sigma of 0.02
 C1B-C1C = C1C-C1D
 1.36 with sigma of 0.02
 C1A-C1F
 1.38 with sigma of 0.02
 N33-C12
 3 with sigma of 0.02
 N33-C32
 1.35 with sigma of 0.02
 C1B-C1D
 2.36 with sigma of 0.04
 C1A-C1E
 2.38 with sigma of 0.04
 C1A-C1C = C1C-C1E = C1D-C1F
 2.37 with sigma of 0.04
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1F \\sim C1F-C1A
 with sigma of 0.02
 C1A-C1E \\sim C1A-C1C \\sim C1E-C1C \\sim C1D-C1B \\sim C1D-C1F \\sim C1F-C1B
 with sigma of 0.04
2. Restrained planarity
 C1A, C1B, C1C, C1D, C1E, C1F
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C1D, C1E, C1F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N1)=1-FVAR(1)
 Sof(N33)=FVAR(1)
6.a Fitted hexagon refined as free rotating group:
 C21(C16,C17,C18,C19,C20)
;
_atom_sites_solution_hydrogens     .
_atom_sites_solution_primary       direct
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 N23 N 0.6809(6) 0.5966(11) 0.4487(6) 0.064(6) Uiso 1 1 d . . . . .
 N30 N 0.8358(6) 0.6957(12) 0.5384(6) 0.066(6) Uiso 1 1 d . . . . .
 N33 N 0.5212(8) 0.3043(17) 0.4102(10) 0.046(16) Uiso 0.54(4) 1 d D . P A 1
 N40 N 0.4925(8) 0.9811(14) 0.4223(8) 0.111(8) Uiso 1 1 d . . . . .
 C1 C 0.4461(6) 0.7504(11) 0.2817(7) 0.072(7) Uiso 1 1 d . . . . .
 C2 C 0.5558(5) 0.5356(10) 0.2715(6) 0.057(6) Uiso 1 1 d . . . . .
 C3 C 0.5097(5) 0.6381(10) 0.4534(6) 0.056(6) Uiso 1 1 d . . . . .
 C4 C 0.4760(5) 0.6952(10) 0.3113(7) 0.049(6) Uiso 1 1 d . . . . .
 C5 C 0.5019(5) 0.6443(11) 0.2801(5) 0.047(6) Uiso 1 1 d . . . . .
 C6 C 0.5288(5) 0.5912(10) 0.3053(7) 0.054(6) Uiso 1 1 d . . . . .
 C7 C 0.5308(5) 0.5917(10) 0.3617(7) 0.049(6) Uiso 1 1 d . . . . .
 C8 C 0.5064(5) 0.6404(11) 0.3920(7) 0.055(6) Uiso 1 1 d . . . . .
 C9 C 0.4799(5) 0.6955(10) 0.3669(7) 0.047(6) Uiso 1 1 d . . . . .
 C10 C 0.5600(6) 0.5343(11) 0.3889(6) 0.053(6) Uiso 1 1 d . . . B 2
 C11 C 0.5445(5) 0.4584(11) 0.3929(6) 0.050(6) Uiso 1 1 d . . . B 2
 C12 C 0.5725(7) 0.4052(12) 0.4191(7) 0.072(7) Uiso 1 1 d . . . B 2
 C13 C 0.6128(6) 0.4249(12) 0.4408(7) 0.069(6) Uiso 1 1 d . . . B 2
 C14 C 0.6244(6) 0.5047(12) 0.4328(6) 0.060(6) Uiso 1 1 d . . . B 2
 C15 C 0.5988(6) 0.5627(10) 0.4072(6) 0.048(6) Uiso 1 1 d . . . B 2
 C21 C 0.4147(5) 0.7277(6) 0.4187(5) 0.060(6) Uiso 1 1 d G . . . .
 C16 C 0.4540(4) 0.7496(8) 0.3981(4) 0.059(6) Uiso 1 1 d G . . . .
 C17 C 0.4690(3) 0.8240(10) 0.4062(5) 0.084(7) Uiso 1 1 d G . . . .
 C18 C 0.4446(5) 0.8763(6) 0.4351(5) 0.099(8) Uiso 1 1 d G . . . .
 C19 C 0.4053(5) 0.8544(8) 0.4557(5) 0.082(7) Uiso 1 1 d G . . . .
 C20 C 0.3903(3) 0.7800(9) 0.4476(5) 0.071(7) Uiso 1 1 d G . . . .
 C22 C 0.6669(6) 0.5272(12) 0.4557(7) 0.070(6) Uiso 1 1 d . . . . .
 C24 C 0.7198(7) 0.6178(12) 0.4721(8) 0.079(7) Uiso 1 1 d . . . . .
 C25 C 0.7453(7) 0.6635(13) 0.4400(8) 0.100(8) Uiso 1 1 d . . . . .
 C26 C 0.7857(6) 0.6942(11) 0.4620(7) 0.071(7) Uiso 1 1 d . . . . .
 C27 C 0.7966(6) 0.6713(12) 0.5163(8) 0.075(7) Uiso 1 1 d . . . . .
 C28 C 0.7692(6) 0.6202(11) 0.5450(7) 0.067(6) Uiso 1 1 d . . . . .
 C29 C 0.7287(6) 0.5971(11) 0.5246(8) 0.070(7) Uiso 1 1 d . . . . .
 C31 C 0.8476(6) 0.7605(13) 0.5285(7) 0.073(7) Uiso 1 1 d . . . . .
 C32 C 0.5594(7) 0.3214(12) 0.4258(6) 0.053(6) Uiso 1 1 d D . . . .
 C41 C 0.4563(8) 0.9594(14) 0.4443(9) 0.127(9) Uiso 1 1 d . . . . .
 C1A C 0.5064(12) 1.0617(14) 0.4265(10) 0.188(9) Uiso 1 1 d D U . C 1
 C1B C 0.4768(7) 1.118(2) 0.4385(8) 0.199(9) Uiso 1 1 d D U . C 1
 C1C C 0.4904(11) 1.1946(18) 0.4363(10) 0.213(9) Uiso 1 1 d D U . C 1
 C1D C 0.5320(12) 1.2097(14) 0.4225(12) 0.207(9) Uiso 1 1 d D U . C 1
 C1E C 0.5615(8) 1.152(2) 0.4124(11) 0.214(9) Uiso 1 1 d D U . C 1
 C1F C 0.5480(10) 1.0756(18) 0.4112(11) 0.198(9) Uiso 1 1 d D U . C 1
 N1 N 0.5790(11) 0.258(2) 0.4396(13) 0.054(19) Uiso 0.46(4) 1 d . . P A 2

_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 N23 C22 1.30(2) . ?
 N23 C24 1.40(2) . ?
 N30 C27 1.41(2) . ?
 N30 C31 1.21(2) . ?
 N33 C32 1.292(16) . ?
 N33 C1D 1.71(4) 1_545 ?
 N40 C41 1.31(2) . ?
 N40 C1A 1.47(3) . ?
 C1 C4 1.53(2) . ?
 C2 C6 1.54(2) . ?
 C3 C8 1.54(2) . ?
 C4 C5 1.431(19) . ?
 C4 C9 1.395(18) . ?
 C5 C5 1.51(3) 3_655 ?
 C5 C6 1.401(19) . ?
 C6 C7 1.410(19) . ?
 C7 C8 1.369(19) . ?
 C7 C10 1.52(2) . ?
 C8 C9 1.415(19) . ?
 C9 C16 1.467(17) . ?
 C10 C11 1.411(19) . ?
 C10 C15 1.390(19) . ?
 C11 C12 1.43(2) . ?
 C12 C13 1.42(2) . ?
 C12 C32 1.52(2) . ?
 C13 C14 1.45(2) . ?
 C14 C15 1.44(2) . ?
 C14 C22 1.50(2) . ?
 C21 C16 1.3900 . ?
 C21 C20 1.3900 . ?
 C16 C17 1.3900 . ?
 C17 C18 1.3900 . ?
 C18 C19 1.3900 . ?
 C18 C41 1.51(3) . ?
 C19 C20 1.3900 . ?
 C20 C31 1.506(19) 6_556 ?
 C24 C25 1.38(2) . ?
 C24 C29 1.39(2) . ?
 C25 C26 1.48(2) . ?
 C26 C27 1.46(2) . ?
 C27 C28 1.43(2) . ?
 C28 C29 1.42(2) . ?
 C32 N1 1.31(3) . ?
 C1A C1B 1.385(12) . ?
 C1A C1F 1.378(12) . ?
 C1B C1C 1.395(12) . ?
 C1C C1D 1.374(11) . ?
 C1D C1E 1.384(12) . ?
 C1E C1F 1.400(12) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 C22 N23 C24 119.0(19) . . ?
 C31 N30 C27 118(2) . . ?
 C32 N33 C1D 89(2) . 1_545 ?
 C41 N40 C1A 120(3) . . ?
 C5 C4 C1 118.0(15) . . ?
 C9 C4 C1 122.2(16) . . ?
 C9 C4 C5 119.8(16) . . ?
 C4 C5 C5 120.0(15) . 3_655 ?
 C6 C5 C4 120.2(15) . . ?
 C6 C5 C5 119.7(15) . 3_655 ?
 C5 C6 C2 119.8(16) . . ?
 C5 C6 C7 118.2(16) . . ?
 C7 C6 C2 122.0(17) . . ?
 C6 C7 C10 118.1(17) . . ?
 C8 C7 C6 122.2(18) . . ?
 C8 C7 C10 119.6(16) . . ?
 C7 C8 C3 120.0(17) . . ?
 C7 C8 C9 120.0(17) . . ?
 C9 C8 C3 120.0(16) . . ?
 C4 C9 C8 119.4(16) . . ?
 C4 C9 C16 119.0(16) . . ?
 C8 C9 C16 121.5(15) . . ?
 C11 C10 C7 116.1(17) . . ?
 C15 C10 C7 116.3(18) . . ?
 C15 C10 C11 127.6(18) . . ?
 C10 C11 C12 115.2(17) . . ?
 C11 C12 C32 120(2) . . ?
 C13 C12 C11 124(2) . . ?
 C13 C12 C32 115(2) . . ?
 C12 C13 C14 113.7(18) . . ?
 C13 C14 C22 114.7(18) . . ?
 C15 C14 C13 126.4(18) . . ?
 C15 C14 C22 118.8(18) . . ?
 C10 C15 C14 112.7(17) . . ?
 C16 C21 C20 120.0 . . ?
 C21 C16 C9 120.8(14) . . ?
 C17 C16 C9 119.2(14) . . ?
 C17 C16 C21 120.0 . . ?
 C18 C17 C16 120.0 . . ?
 C17 C18 C19 120.0 . . ?
 C17 C18 C41 125.0(17) . . ?
 C19 C18 C41 114.9(17) . . ?
 C20 C19 C18 120.0 . . ?
 C21 C20 C31 123.2(15) . 6_556 ?
 C19 C20 C21 120.0 . . ?
 C19 C20 C31 116.8(15) . 6_556 ?
 N23 C22 C14 119.5(18) . . ?
 C25 C24 N23 114(2) . . ?
 C25 C24 C29 125(2) . . ?
 C29 C24 N23 120(2) . . ?
 C24 C25 C26 119.1(19) . . ?
 C27 C26 C25 116.6(18) . . ?
 N30 C27 C26 119.1(19) . . ?
 N30 C27 C28 120.9(19) . . ?
 C28 C27 C26 119.8(19) . . ?
 C29 C28 C27 122.1(18) . . ?
 C24 C29 C28 116.3(18) . . ?
 N30 C31 C20 113(5) . 6_656 ?
 N1 C32 C12 135(3) . . ?
 N40 C41 C18 115(2) . . ?
 C1B C1A N40 120(3) . . ?
 C1F C1A N40 115(3) . . ?
 C1F C1A C1B 124.6(15) . . ?
 C1A C1B C1C 117.6(14) . . ?
 C1D C1C C1B 118.8(14) . . ?
 C1C C1D N33 92(3) . 1_565 ?
 C1C C1D C1E 122.8(14) . . ?
 C1E C1D N33 143(3) . 1_565 ?
 C1D C1E C1F 119.3(14) . . ?
 C1A C1F C1E 116.6(14) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 N23 C24 C25 C26 175.5(17) . . . . ?
 N23 C24 C29 C28 179.1(17) . . . . ?
 N30 C27 C28 C29 177.3(17) . . . . ?
 N33 C1D C1E C1F -152(3) 1_565 . . . ?
 N40 C1A C1B C1C -173(2) . . . . ?
 N40 C1A C1F C1E 177(2) . . . . ?
 C1 C4 C5 C5 -2(2) . . . 3_655 ?
 C1 C4 C5 C6 -178.1(15) . . . . ?
 C1 C4 C9 C8 176.8(15) . . . . ?
 C1 C4 C9 C16 1(2) . . . . ?
 C2 C6 C7 C8 -179.2(16) . . . . ?
 C2 C6 C7 C10 -1(2) . . . . ?
 C3 C8 C9 C4 -177.7(14) . . . . ?
 C3 C8 C9 C16 -2(2) . . . . ?
 C4 C5 C6 C2 178.7(14) . . . . ?
 C4 C5 C6 C7 -2(2) . . . . ?
 C4 C9 C16 C21 93.4(15) . . . . ?
 C4 C9 C16 C17 -85.7(15) . . . . ?
 C5 C4 C9 C8 -6(2) . . . . ?
 C5 C4 C9 C16 178.2(16) . . . . ?
 C5 C5 C6 C2 3(2) 3_655 . . . ?
 C5 C5 C6 C7 -178.6(15) 3_655 . . . ?
 C5 C6 C7 C8 2(2) . . . . ?
 C5 C6 C7 C10 -179.9(16) . . . . ?
 C6 C7 C8 C3 179.7(14) . . . . ?
 C6 C7 C8 C9 -4(3) . . . . ?
 C6 C7 C10 C11 -78.6(19) . . . . ?
 C6 C7 C10 C15 101.7(18) . . . . ?
 C7 C8 C9 C4 6(2) . . . . ?
 C7 C8 C9 C16 -178.8(15) . . . . ?
 C7 C10 C11 C12 -179.7(14) . . . . ?
 C7 C10 C15 C14 179.6(14) . . . . ?
 C8 C7 C10 C11 99.6(19) . . . . ?
 C8 C7 C10 C15 -80(2) . . . . ?
 C8 C9 C16 C21 -82.3(17) . . . . ?
 C8 C9 C16 C17 98.6(16) . . . . ?
 C9 C4 C5 C5 -179.3(14) . . . 3_655 ?
 C9 C4 C5 C6 5(2) . . . . ?
 C9 C16 C17 C18 179.1(12) . . . . ?
 C10 C7 C8 C3 2(2) . . . . ?
 C10 C7 C8 C9 178.3(15) . . . . ?
 C10 C11 C12 C13 1(2) . . . . ?
 C10 C11 C12 C32 -179.9(14) . . . . ?
 C11 C10 C15 C14 0(2) . . . . ?
 C11 C12 C13 C14 -2(2) . . . . ?
 C11 C12 C32 N1 167(3) . . . . ?
 C12 C13 C14 C15 2(3) . . . . ?
 C12 C13 C14 C22 179.7(14) . . . . ?
 C13 C12 C32 N1 -13(3) . . . . ?
 C13 C14 C15 C10 -1(2) . . . . ?
 C13 C14 C22 N23 177.1(16) . . . . ?
 C15 C10 C11 C12 0(2) . . . . ?
 C15 C14 C22 N23 -5(2) . . . . ?
 C21 C16 C17 C18 0.0 . . . . ?
 C16 C21 C20 C19 0.0 . . . . ?
 C16 C21 C20 C31 -179.6(12) . . . 6_556 ?
 C16 C17 C18 C19 0.0 . . . . ?
 C16 C17 C18 C41 -176.8(15) . . . . ?
 C17 C18 C19 C20 0.0 . . . . ?
 C17 C18 C41 N40 0(3) . . . . ?
 C18 C19 C20 C21 0.0 . . . . ?
 C18 C19 C20 C31 179.6(11) . . . 6_556 ?
 C19 C18 C41 N40 -176.6(15) . . . . ?
 C20 C21 C16 C9 -179.1(13) . . . . ?
 C20 C21 C16 C17 0.0 . . . . ?
 C22 N23 C24 C25 140(2) . . . . ?
 C22 N23 C24 C29 -44(3) . . . . ?
 C22 C14 C15 C10 -178.7(14) . . . . ?
 C24 N23 C22 C14 177.4(15) . . . . ?
 C24 C25 C26 C27 2(3) . . . . ?
 C25 C24 C29 C28 -5(3) . . . . ?
 C25 C26 C27 N30 176.9(17) . . . . ?
 C25 C26 C27 C28 1(3) . . . . ?
 C26 C27 C28 C29 -7(3) . . . . ?
 C27 N30 C31 C20 -178(3) . . . 6_656 ?
 C27 C28 C29 C24 9(3) . . . . ?
 C29 C24 C25 C26 0(3) . . . . ?
 C31 N30 C27 C26 39(3) . . . . ?
 C31 N30 C27 C28 -145(2) . . . . ?
 C32 C12 C13 C14 179.1(13) . . . . ?
 C41 N40 C1A C1B -20(3) . . . . ?
 C41 N40 C1A C1F 168(2) . . . . ?
 C41 C18 C19 C20 177.1(13) . . . . ?
 C1A N40 C41 C18 177.4(18) . . . . ?
 C1A C1B C1C C1D 0(2) . . . . ?
 C1B C1A C1F C1E 5(4) . . . . ?
 C1B C1C C1D N33 164.4(18) . . . 1_565 ?
 C1B C1C C1D C1E -2(4) . . . . ?
 C1C C1D C1E C1F 6(5) . . . . ?
 C1D C1E C1F C1A -7(4) . . . . ?
 C1F C1A C1B C1C -2(2) . . . . ?

_olex2_submission_special_instructions  'No special instructions were received'

# start Validation Reply Form
_vrf_ATOM007_shelx_a
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: Only Uiso is refined because this is a set of merged continuous 
          rotational electron diffraction data with resolution up to 
          1.5 Angstrom, which is not enough for the refinement of Uaniso. 
;
_vrf_RINTA01_shelx_a
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: This is a set of merged continuous rotational electron data, 
          so the value of Rint is higher than that of SC-XRD data. 
;
_vrf_THETM01_shelx_a
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The resolution of this dataset is up to 1.5 Angstrom after 
          merging, which is lower than expected value of checkCIF process.
          However, using dataset with this resolution is enough
          for determining the topological structure of COFs.
;
_vrf_PLAT020_shelx_a
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.277 Report
RESPONSE: This is a set of merged continuous rotational electron data, 
          so the value of Rint is higher than that of SC-XRD data. 
;
_vrf_PLAT082_shelx_a
;
PROBLEM: High R1 Value ..................................       0.23 Report
RESPONSE: This is a set of merged continuous rotational electron data, 
          so the value of R1 is higher than that of SC-XRD data. 
;
_vrf_PLAT084_shelx_a
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.52 Report
RESPONSE: This is a set of merged continuous rotational electron data, 
          so the value of wR2 is higher than that of SC-XRD data.
;
_vrf_PLAT602_shelx_a
;
PROBLEM: Solvent Accessible VOID(S) in Structure ........          ! Check 
RESPONSE: This is a COF structure with pores in the framework. Since the
          cRED data resolotion is not enough for determing the possible 
          solvent molecules (probably water), the existence of void is 
          reasonable. 
;
_vrf_PLAT049_shelx_a
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 ......... 0.4878 Check
RESPONSE: That's quite normal for COF structures.
;
_vrf_PLAT196_shelx_a
;
PROBLEM: No TEMP record and _measurement_temperature .NE. 293 Degree
RESPONSE: The data is collected under 100 K. No Hydrogens are added, so there 
          is no TMEP order
;
_vrf_PLAT340_shelx_a
;
PROBLEM:  Low Bond Precision on C-C Bonds ............... 0.02785 Ang
RESPONSE: That precision is enough for determining the topology.
;
# end Validation Reply Form