Cage Based Crystalline Covalent Organic Frameworks.
Ma, Jian-Xin; Li, Jian; Chen, Yi-Fan; Ning, Rui; Ao, Yu-Fei; Liu, Jun-Min; Sun, Junliang; Wang, De-Xian; Wang, Qi-Qiang; Journal of the American Chemical Society 141 (2019) 3843–3848; doi:10.1021/jacs.9b00665

data_4128509
_publ_section_title
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 Cage Based Crystalline Covalent Organic Frameworks.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3843
_journal_page_last               3848
_journal_paper_doi               10.1021/jacs.9b00665
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C60 H36 N12 O6, C4 H10 O, 2(C7 H8)'
_chemical_formula_sum            'C78 H62 N12 O7'
_chemical_formula_weight         1279.39
_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
_audit_creation_date             2018-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.050(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9724(7)
_cell_length_b                   29.8124(9)
_cell_length_c                   16.4699(9)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.7050
_cell_measurement_theta_min      1.7920
_cell_volume                     6522.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_unetI/netI     0.1044
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36441
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.675
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     943
_refine_ls_number_reflns         11487
_refine_ls_number_restraints     334
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1556
_refine_ls_R_factor_gt           0.0823
_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^)+(0.1072P)^2^+4.8427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1988
_refine_ls_wR_factor_ref         0.2385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6397
_reflns_number_total             11487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00665_si_002.cif
_cod_data_source_block           mx5995f
_cod_database_code               4128509
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C78-C73 = C78-C77 = C77-C76 = C76-C75 = C75-C74 = C74-C73
 1.38 with sigma of 0.01
 C76A-C75A = C77A-C76A = C78A-C77A = C78A-C73A = C74A-C73A = C75A-C74A
 1.38 with sigma of 0.01
 C73A-C72A = C73-C72
 1.51 with sigma of 0.01
 C66-C65
 1.51 with sigma of 0.01
 C67-C66 = C68-C67 = C69-C68 = C70-C69 = C71-C70 = C71-C66
 1.38 with sigma of 0.001
3. Rigid bond restraints
 C71, C66
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C73A
\\sim C72A \\sim C74A \\sim C78A \\sim C76A \\sim C77A \\sim C75A: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq,
Uanis(C73A) \\sim Ueq, Uanis(C74A) \\sim Ueq, Uanis(C78A) \\sim Ueq,
Uanis(C76A) \\sim Ueq, Uanis(C77A) \\sim Ueq, Uanis(C75A) \\sim Ueq,
Uanis(C72A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68)
\\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(C73A)=Sof(C72A)=Sof(H72D)=Sof(H72E)=Sof(H72F)=Sof(C74A)=Sof(H74A)=
 Sof(C78A)=Sof(H78A)=Sof(C76A)=Sof(H76A)=Sof(C77A)=Sof(H77A)=Sof(C75A)=
 Sof(H75A)=1-FVAR(1)
 Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C73)=Sof(C74)=Sof(H74)=Sof(C75)=
 Sof(H75)=Sof(C76)=Sof(H76)=Sof(C77)=Sof(H77)=Sof(C78)=Sof(H78)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C62(H62A,H62B), C63(H63A,H63B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12),
 C13(H13), C18(H18), C20(H20), C22(H22), C27(H27), C28(H28), C30(H30), C31(H31),
  C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C43(H43),
 C45(H45), C47(H47), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C56(H56),
  C57(H57), C58(H58), C59(H59), C60(H60), C67(H67), C68(H68), C69(H69),
 C70(H70), C71(H71), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78),
 C74A(H74A), C78A(H78A), C76A(H76A), C77A(H77A), C75A(H75A)
6.c Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C72(H72A,H72B,
 H72C), C72A(H72D,H72E,H72F)
;
_shelx_res_checksum              7136
_shelx_hkl_checksum              77556
_olex2_submission_special_instructions 'No special instructions were received'