Controlled Hierarchical Self-Assembly of Catenated Cages.
Sun, Zhongwei; Li, Pan; Xu, Shijun; Li, Zi-Ying; Nomura, Yoshiaki; Li, Zimu; Liu, Xiaoyun; Zhang, Shaodong; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c03330

data_4135059
_publ_section_title
;
 Controlled Hierarchical Self-Assembly of Catenated Cages.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c03330
_journal_year                    2020
_chemical_formula_moiety         '2(C84 H66 N6 S6)'
_chemical_formula_sum            'C168 H132 N12 S12'
_chemical_formula_weight         2703.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                74.473(3)
_cell_angle_beta                 75.276(3)
_cell_angle_gamma                84.941(3)
_cell_formula_units_Z            2
_cell_length_a                   18.3116(16)
_cell_length_b                   19.4359(18)
_cell_length_c                   29.992(3)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    206(2)
_cell_measurement_theta_max      54.27
_cell_measurement_theta_min      7.51
_cell_volume                     9944.6(16)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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      205.82
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            117664
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.138
_diffrn_reflns_theta_min         2.784
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1275 before and 0.0877 after correction. The Ratio of minimum to maximum transmission is 0.6773. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.903
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.114
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1783
_refine_ls_number_reflns         37560
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.1000
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2672
_refine_ls_wR_factor_ref         0.2876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21902
_reflns_number_total             37560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c03330_si_002.cif
_cod_data_source_block           CSC-1
_cod_database_code               4135059
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.889
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 S13-C143 = S12-C141 = S12-C140 = S13-C140
 1.75 with sigma of 0.02
 C1AA-C111 = C109-C0AA
 1.53 with sigma of 0.02
 C1AA-C109
 1.53 with sigma of 0.02
 C0AA-C111
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C107 \\sim C108 \\sim C111 \\sim C109: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C140 \\sim S13 \\sim C143 \\sim C142 \\sim C141 \\sim S12 \\sim C139: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C111 \\sim C1AA \\sim C0AA \\sim C109 \\sim S2AA \\sim S3AA \\sim C108 \\sim
S0AA \\sim S1AA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(S13) \\sim Ueq, Uanis(C143) \\sim Ueq, Uanis(C142) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: S1(0.5) S2(0.5) H1B(0.5) H1A(0.5) H2BC(0.5) H2BD(0.5) H2AA(0.5)
 H2AB(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5)
 H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5) H10A(0.5) H108(0.5) H10B(0.5) H10C(0.5)
 H10D(0.5) H10E(0.5) H11C(0.5) H11D(0.5) H11A(0.5) H11B(0.5) S0AA(0.5)
 S1AA(0.5) S2AA(0.5) S3AA(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) C1AA(0.5)
 H1AA(0.5) H1AB(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1B), C1(H1A), C24(H24), C56(H56), C87(H87), C108(H10A), C108(H108),
 C140(H140)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2BC,H2BD), C2(H2AA,H2AB), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,
 H6B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C57(H57A,H57B), C58(H58A,
 H58B), C59(H59A,H59B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B),
 C109(H10B,H10C), C109(H10D,H10E), C111(H11C,H11D), C111(H11A,H11B), C141(H14A,
 H14B), C142(H14C,H14D), C143(H14E,H14F), C0AA(H0AA,H0AB), C1AA(H1AA,H1AB)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C13(H13), C15(H15), C17(H17), C19(H19), C22(H22), C28(H28),
 C31(H31), C33(H33), C35(H35), C37(H37), C39(H39), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C47(H47), C49(H49), C51(H51), C54(H54), C60(H60),
 C63(H63), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72),
  C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81),
 C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C92(H92), C95(H95), C97(H97),
  C99(H99), C101(H101), C103(H103), C106(H106), C112(H112), C115(H115),
 C117(H117), C119(H119), C121(H121), C123(H123), C126(H126), C127(H127),
 C128(H128), C129(H129), C130(H130), C131(H131), C133(H133), C135(H135),
 C138(H138), C144(H144), C147(H147), C149(H149), C151(H151), C152(H152),
 C153(H153), C154(H154), C155(H155), C156(H156), C157(H157), C158(H158),
 C159(H159), C160(H160), C161(H161), C162(H162), C163(H163), C164(H164),
 C165(H165), C166(H166), C167(H167), C168(H168), C169(H169), C170(H170),
 C3AA(H3AA), C2AA(H2AC)
;
_shelx_res_checksum              30986
_shelx_hkl_checksum              40652
_shelx_fab_checksum              1561
_olex2_submission_special_instructions 'No special instructions were received'