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_7130966
_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, C24 H12, 6(F6 P), 7[CH3CN]'
_chemical_formula_sum            'C146 H119 F36 N13 O2 P6'
_chemical_formula_weight         2957.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2cz0p2
_audit_creation_date             2022-10-15
_audit_creation_method
;
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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2022-11-01 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   48.4768(18)
_cell_length_b                   17.0639(7)
_cell_length_c                   16.7750(7)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      54.22
_cell_measurement_theta_min      3.17
_cell_volume                     13876.3(10)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       Bruker
_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      150.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            147092
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        52.981
_diffrn_reflns_theta_max         52.981
_diffrn_reflns_theta_min         2.755
_diffrn_source_current           2.86
_diffrn_source_power             0.1997996
_diffrn_source_voltage           69.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1348 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.8201.
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    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             6064
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1514
_refine_ls_number_reflns         21996
_refine_ls_number_restraints     3697
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0910
_refine_ls_shift/su_max          0.005
_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^+40.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.1891
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_full    0.790
_reflns_Friedel_fraction_max     0.790
_reflns_number_gt                19701
_reflns_number_total             21996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05153b2.cif
_cod_data_source_block           a_a
_cod_database_code               7130966
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.784
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.92(5)
 0.08(5)
2. 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
3. Restrained distances
 C65-C7 = C129-C65 = C59-C129 = C59-C123 = C123-C102 = C7-C102
 1.39 with sigma of 0.01
 C31-C117 = C125-C31 = C65-C125 = C117-C57
 1.39 with sigma of 0.01
 C57-C7 = C57-C113 = C113-C104 = C115-C104 = C115-C102 = C115-C111 = C111-C29 =
  C61-C29 = C61-C123 = C61-C121
 1.39 with sigma of 0.01
 C125-C31 = C31-C117 = C117-C57 = C2-C110 = C110-C98 = C119-C98 = C57-C7 =
 C113-C104 = C57-C113 = C115-C104
 1.39 with sigma of 0.01
 C125-C117
 2.39 with sigma of 0.01
 C104-C102
 2.39 with sigma of 0.01
 C7-C129
 2.39 with sigma of 0.01
 C102-C57
 2.39 with sigma of 0.01
 C117-C7
 2.39 with sigma of 0.01
 C110-C129
 2.39 with sigma of 0.01
 C57-C104
 2.39 with sigma of 0.01
 C2-C98
 2.39 with sigma of 0.01
 C102-C65
 2.39 with sigma of 0.01
 C110-C119
 2.39 with sigma of 0.01
 C65-C31
 2.39 with sigma of 0.01
 C98-C59
 2.39 with sigma of 0.01
 C31-C57
 2.39 with sigma of 0.01
 C119-C129
 2.39 with sigma of 0.01
 C57-C65
 2.39 with sigma of 0.01
 C59-C2
 2.39 with sigma of 0.01
 C7-C113
 2.39 with sigma of 0.01
 C129-C123
 2.39 with sigma of 0.01
 C113-C115
 2.39 with sigma of 0.01
 C59-C102
 2.39 with sigma of 0.01
 C115-C7
 2.39 with sigma of 0.01
 C123-C7
 2.39 with sigma of 0.01
 P2-F9 = P2-F21 = P2-F17 = P2-F11 = P2-F23B
 1.63 with sigma of 0.01
 P4-F39 = P4-F3B = P4-F38 = P4-F23A = P4-F41 = P4-F40
 1.63 with sigma of 0.01
 F3A-P2
 1.63 with sigma of 0.01
 F3A-F23B
 2.4 with sigma of 0.01
 F3A-F9
 2.4 with sigma of 0.01
 F38-F3B
 2.4 with sigma of 0.01
 F38-F40
 2.4 with sigma of 0.01
 F41-F3B
 2.4 with sigma of 0.01
 F23A-F41
 2.4 with sigma of 0.01
 F41-F39
 2.4 with sigma of 0.01
 F40-F41
 2.4 with sigma of 0.01
 C111-C102
 2.39 with sigma of 0.01
 C29-C115
 2.39 with sigma of 0.01
 C115-C123
 2.39 with sigma of 0.01
 C102-C61
 2.39 with sigma of 0.01
 C61-C111
 2.39 with sigma of 0.01
 C123-C29
 2.39 with sigma of 0.01
 C29-C111 = C115-C111 = C115-C102 = C61-C29 = C123-C102 = C59-C129 = C7-C102 =
 C7-C65 = C31-C125 = C31-C117 = C57-C117 = C7-C57 = C57-C113 = C113-C104 = C115-
 C104 = C98-C119 = C98-C110 = C2-C110
 1.39 with sigma of 0.001
4. 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
5. 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(P3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C111) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C104)
\\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C113) \\sim Ueq,
Uanis(C57) \\sim Ueq, Uanis(C115) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C117)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C121) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C123) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C127) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(C129) \\sim Ueq, Uanis(C65) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
7. Others
 Sof(P4)=Sof(F3B)=Sof(F23A)=Sof(F38)=Sof(F39)=Sof(F40)=Sof(F41)=1-FVAR(1)
 Sof(P2)=Sof(F3A)=Sof(F9)=Sof(F11)=Sof(F17)=Sof(F21)=Sof(F23B)=FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C53(H53A,H53B), C64(H64A,H64B), C96(H96A,H96B), C106(H10A,
 H10B), C109(H10C,H10D)
8.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C72(H72), C38(H38), C107(H107), C76(H76), C73(H73), C34(H34),
 C37(H37), C128(H128), C26(H26), C5(H5), C14(H14), C40(H40), C10(H10), C97(H97),
  C51(H51), C62(H62), C75(H75), C32(H32), C39(H39), C100(H100), C84(H84),
 C89(H89), C20(H20), C13(H13), C19(H19), C27(H27), C33(H33), C41(H41), C43(H43),
  C108(H108), C103(H103), C101(H101), C132(H132), C114(H114), C22(H22),
 C24(H24), C47(H47), C50(H50), C25(H25), C95(H95), C66(H66), C69(H69), C30(H30),
  C80(H80), C9(H9), C68(H68), C78(H78), C105(H105), C88(H88), C99(H99),
 C79(H79), C48(H48), C92(H92), C82(H82), C83(H83), C87(H87), C85(H85), C86(H86),
  C42(H42), C94(H94), C130(H130), C1(H1), C8(H8), C18(H18), C122(H122),
 C126(H126), C131(H131), C29(H29), C31(H31), C15(H15), C121(H121), C98(H98),
 C104(H104), C110(H110), C111(H111), C113(H113), C117(H117), C63(H63),
 C127(H127)
8.c Fitted hexagon refined as free rotating group:
 N1(C46,C72,C21,C38,C107), N4(C76,C73,C4,C34,C37), N6(C128,C26,C116,C5,C14),
 C3(C40,C10,C12,C97,C51), C6(C62,C75,C71,C32,C39), C11(C100,C84,C60,C89,C20),
 C49(C43,C108,C93,C103,C101), C52(C132,C114,C124,C22,C24), C54(C47,C50,C58,C25,
 C95), C67(C69,C30,C35,C80,C9), C74(C78,C105,C56,C88,C99), C77(C79,C48,C81,C92,
 C82), C91(C87,C85,C36,C86,C42), C118(C130,C1,C28,C8,C18), C59(C119,C15,C121,
 C61,C123), C125(C63,C127,C2,C129,C65)
8.d Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C120(H12A,H12B,H12C)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 648 electrons were 
found in a volume of 2332\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
7[CH3CN] per Asymmetric Unit 
which account for 616 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61653
_shelx_hkl_checksum              37632
_shelx_fab_checksum              84215
_olex2_submission_special_instructions 'No special instructions were received'