A tetraphenylethene-based hexacationic molecular cage with an open cavity
Cao, Fan; Duan, Honghong; Li, Qingfang; Cao, Liping; Chemical Communications  (2022) –; doi:10.1039/D2CC05153B

data_7130965
_publ_section_title
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 A tetraphenylethene-based hexacationic molecular cage with an open cavity
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC05153B
_journal_year                    2022
_chemical_formula_moiety         'C108 H86 N6 O2, 6(Cl), C H4 O, 18[CH3OH]'
_chemical_formula_sum            'C127 H162 Cl6 N6 O21'
_chemical_formula_weight         2321.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2dfgq1
_audit_creation_date             2022-11-04
_audit_creation_method
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Olex2 1.5 
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) 
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_audit_update_record
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2022-11-04 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 113.007(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.948(3)
_cell_length_b                   20.5987(16)
_cell_length_c                   41.696(3)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      49.78
_cell_measurement_theta_min      2.54
_cell_volume                     26048(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.00
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.1004
_diffrn_reflns_av_unetI/netI     0.0955
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            234734
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        52.982
_diffrn_reflns_theta_max         52.982
_diffrn_reflns_theta_min         1.898
_diffrn_source_current           2.86
_diffrn_source_power             0.1997996
_diffrn_source_voltage           69.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1465 before and 0.0969 after correction. 
The Ratio of minimum to maximum transmission is 0.7158. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            'dull light orange'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       block
_exptl_crystal_F_000             9888
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.332
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2259
_refine_ls_number_reflns         44462
_refine_ls_number_restraints     2372
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1758
_refine_ls_R_factor_gt           0.1197
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2527
_refine_ls_wR_factor_ref         0.2778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22661
_reflns_number_total             44462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05153b2.cif
_cod_data_source_block           20220310ac_0m_a
_cod_database_code               7130965
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.780
_olex2_refinement_description
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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, All O(H) groups 
2. Restrained distances 
 O3-C168 
 1.45 with sigma of 0.01 
 C27-C31 = C33-C27 = C33-C32 = C30-C31 = N4-C32 = N4-C30 
 1.39 with sigma of 0.01 
 H18-H19A 
 2.1 with sigma of 0.01 
 O10-C221 = O9-C222 
 1.42 with sigma of 0.001 
 N4-C30 \\sim N4-C32 
 with sigma of 0.02 
 C27-C31 \\sim C27-C33 
 with sigma of 0.02 
 C31-C30 \\sim C33-C32 
 with sigma of 0.02 
 N4-C31 \\sim N4-C33 
 with sigma of 0.04 
 C27-C30 \\sim C27-C32 
 with sigma of 0.04 
3. Rigid bond restraints 
 All non-hydrogen atoms 
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 
4. Uiso/Uaniso restraints and constraints 
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma 
for terminal atoms of 0.02 within 2A 
Uanis(Cl) \\sim Ueq, Uanis(Cl11) \\sim Ueq: with sigma of 0.001 and sigma for 
terminal atoms of 0.002 
Uanis(Cl9) \\sim Ueq, Uanis(Cl13) \\sim Ueq: with sigma of 0.001 and sigma for 
terminal atoms of 0.002 
Uanis(Cl5) = Uanis(Cl2) 
5. Others 
 Sof(Cl)=Sof(Cl13)=1-FVAR(1) 
 Sof(Cl9)=Sof(Cl11)=FVAR(1) 
 Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=1-FVAR(2) 
 Sof(C31)=Sof(H31)=Sof(C30)=Sof(H30)=FVAR(2) 
6.a Riding coordinates: 
 O9(H9), O10(H10C) 
6.b Secondary CH2 refined with riding coordinates: 
 C34(H34A,H34B), C41(H41A,H41B), C65(H65A,H65B), C72(H72A,H72B), C103(H10A, 
 H10B), C110(H11A,H11B), C142(H14A,H14B), C149(H14C,H14D), C181(H18A,H18B), 
 C188(H18C,H18D), C202(H20A,H20B), C209(H20C,H20D) 
6.c Aromatic/amide H refined with riding coordinates: 
 C1(H1), C2(H2), C29(H29), C28(H28), C31(H31), C30(H30), C4(H4), C5(H5), 
 C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C15(H15), C16(H16), C18(H18), 
 C22(H22), C23(H23), C25(H25), C26(H26), C32(H32), C33(H33), C36(H36), C37(H37), 
  C39(H39), C40(H40), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48), 
 C49(H49), C51(H51), C52(H52), C55(H55), C56(H56), C58(H58), C59(H59), C61(H61), 
  C62(H62), C63(H63), C64(H64), C67(H67), C68(H68), C70(H70), C71(H71), 
 C73(H73), C74(H74), C76(H76), C77(H77), C79(H79), C80(H80), C81(H81), C83(H83), 
  C86(H86), C87(H87), C89(H89), C90(H90), C93(H93), C94(H94), C96(H96), 
 C97(H97), C99(H99), C100(H100), C101(H101), C102(H102), C105(H105), C106(H106), 
  C108(H108), C109(H109), C111(H111), C112(H112), C117(H117), C118(H118), 
 C120(H120), C121(H121), C124(H124), C125(H125), C127(H127), C128(H128), 
 C132(H132), C133(H133), C135(H135), C136(H136), C138(H138), C139(H139), 
 C140(H140), C141(H141), C144(H144), C145(H145), C147(H147), C148(H148), 
 C150(H150), C151(H151), C153(H153), C154(H154), C156(H156), C157(H157), 
 C159(H159), C160(H160), C163(H163), C164(H164), C166(H166), C167(H167), 
 C171(H171), C172(H172), C174(H174), C175(H175), C177(H177), C178(H178), 
 C179(H179), C180(H180), C183(H183), C184(H184), C186(H186), C187(H187), 
 C189(H189), C190(H190), C192(H192), C193(H193), C194(H194), C195(H195), 
 C198(H198), C199(H199), C200(H200), C201(H201), C204(H204), C205(H205), 
 C206(H206), C207(H207), C210(H210), C211(H211), C213(H213), C214(H214), 
 C216(H216), C217(H217), C218(H218), C219(H219) 
6.d Fitted hexagon refined as free rotating group: 
 N4(C29,C28,C27,C31,C30) 
6.e Idealised Me refined as rotating group: 
 C19(H19A,H19B,H19C), C84(H84A,H84B,H84C), C122(H12A,H12B,H12C), C168(H16A, 
 H16B,H16C), C222(H22A,H22B,H22C), C221(H22D,H22E,H22F) 
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_smtbx_masks_special_details
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A solvent mask was calculated and 2583 electrons were 
found in a volume of 10508\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
72[CH3OH] per Asymmetric Unit 
which account for 2592 electrons 
per unit cell. 
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_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25794
_shelx_hkl_checksum              52631
_shelx_fab_checksum              26194
_olex2_submission_special_instructions 'No special instructions were received'