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_4135060
_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         'C84 H72 N6 S6, 1.5(C4 H8 O)'
_chemical_formula_sum            'C90 H84 N6 O1.5 S6'
_chemical_formula_weight         1465.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-01-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 118.0400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   70.5814(19)
_cell_length_b                   15.2442(4)
_cell_length_c                   41.8633(11)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      46.671
_cell_measurement_theta_min      3.142
_cell_volume                     39755.9(19)
_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      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       85
_diffrn_reflns_limit_h_min       -86
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            216292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.073
_diffrn_reflns_theta_min         2.875
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1636 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.8034.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.980
_exptl_crystal_description       block
_exptl_crystal_F_000             12384
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.273
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1864
_refine_ls_number_reflns         37817
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1643
_refine_ls_R_factor_gt           0.1069
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1878P)^2^+114.4029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3125
_refine_ls_wR_factor_ref         0.3594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20221
_reflns_number_total             37817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c03330_si_003.cif
_cod_data_source_block           CDC-1_3THF
_cod_depositor_comments
;

2025-07-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C180 H168 N12 O3 S12'
_cod_original_formula_weight         2931.97
_cod_original_formula_moiety         '2(C84 H72 N6 S6), 3(C4 H8 O)'
_cod_original_formula_units_Z            8
_cod_database_code               4135060
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.922
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C115-C114
 2.2 with sigma of 0.001
 C64-C65
 2.2 with sigma of 0.001
 C35-C36
 2.2 with sigma of 0.001
 C99-C100
 2.2 with sigma of 0.001
 C148-C149
 2.2 with sigma of 0.001
 C119-C120
 2.2 with sigma of 0.001
 N4-C36 = N6-C64 = N8-C99 = N9-C115 = N12-C148
 1.4 with sigma of 0.001
 N5-C51
 1.4 with sigma of 0.001
 N6-C65 = N4-C36 = N3-C30 = N12-C149 = N10-C120 = N9-C114
 1.4 with sigma of 0.001
 N10-C119
 1.4 with sigma of 0.001
 N4-C35
 1.4 with sigma of 0.001
3.a Riding coordinates:
 N3(H3), N4(H4), N6(H6), N9(H9A), N10(H10), N12(H12)
3.b Ternary CH refined with riding coordinates:
 C1(H1), C22(H22), C42(H42), C85(H85), C106(H106), C126(H126)
3.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C23(H23A,H23B), C24(H24A,H24B),
 C25(H25A,H25B), C31(H31A,H31B), C35(H35A,H35B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C64(H64A,H64B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,
 H88B), C107(H10A,H10B), C108(H10C,H10D), C109(H10E,H10F), C115(H11A,H11B),
 C119(H11C,H11D), C127(H12A,H12B), C128(H12C,H12D), C129(H12E,H12F), C148(H14A,
 H14B), C169(H16A,H16B), C170(H17A,H17B), C171(H17C,H17D), C172(H17E,H17F),
 C173(H17G,H17H), C174(H17I,H17J), C175(H17K,H17L), C176(H17M,H17N), C177(H17O,
 H17P), C178(H17Q,H17R), C179(H17S,H17T), C180(H18A,H18B)
3.d Aromatic/amide H refined with riding coordinates:
 C6(H6A), C9(H9), C11(H11), C13(H13), C15(H15), C17(H17), C20(H20), C26(H26),
 C29(H29), C33(H33), C37(H37), C40(H40), C46(H46), C49(H49), C51(H51), C53(H53),
  C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
 C61(H61), C62(H62), C66(H66), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73),
  C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80),
 C81(H81), C82(H82), C83(H83), C84(H84), C90(H90), C93(H93), C95(H95), C97(H97),
  C99(H99), C101(H101), C104(H104), C110(H110), C113(H113), C117(H117),
 C121(H121), C124(H124), C130(H130), C133(H133), C135(H135), C137(H137),
 C138(H138), C139(H139), C140(H140), C141(H141), C142(H142), C143(H143),
 C144(H144), C145(H145), C146(H146), C150(H150), 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)
;
_shelx_res_checksum              91796
_shelx_hkl_checksum              24046
_shelx_fab_checksum              72675
_olex2_submission_special_instructions 'No special instructions were received'