A water-soluble naphthalenediimide-containing hexacationic cage.
Fang, Shuai; Li, Errui; Zhu, Dingsheng; Wu, Guangcheng; Zhang, Qinhao; Lin, Chuhao; Huang, Feihe; Li, Hao; Chemical communications (Cambridge, England) 57 (2021) 6074–6077; doi:10.1039/d1cc02242c

data_1562689
_publ_section_title
;
 A water-soluble naphthalenediimide-containing hexacationic cage.
;
_journal_issue                   49
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6074
_journal_page_last               6077
_journal_paper_doi               10.1039/d1cc02242c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'6(Br), C90 H54 N12 O12, 12(C5 H4 O), 3(H2 O)'
_chemical_formula_sum            'C150 H108 Br6 N12 O27'
_chemical_formula_weight         2989.94
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-09 deposited with the CCDC.	2021-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                106.9800(10)
_cell_angle_beta                 100.1400(10)
_cell_angle_gamma                109.1810(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4602(5)
_cell_length_b                   21.9065(8)
_cell_length_c                   25.8360(10)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.767
_cell_measurement_theta_min      2.40
_cell_volume                     7049.7(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 0.989
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            76545
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.813
_diffrn_reflns_theta_min         2.212
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.785
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1093 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.7963.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             3036
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.802
_refine_diff_density_min         -2.115
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1717
_refine_ls_number_reflns         26612
_refine_ls_number_restraints     314
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1767
_refine_ls_R_factor_gt           0.1393
_refine_ls_shift/su_max          0.008
_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^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3247
_refine_ls_wR_factor_ref         0.3485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16972
_reflns_number_total             26612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02242c2.cif
_cod_data_source_block           191118_fang_164_hg_0m
_cod_depositor_comments
'Adding full bibliography for 1562686--1562691.cif.'
_cod_database_code               1562689
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.717
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 O04L-C050
 1.45 with sigma of 0.02
 O30-C20
 1.45 with sigma of 0.02
 O28-C27
 1.45 with sigma of 0.02
 O9-C9 = O049-C04K
 1.4 with sigma of 0.02
 O9-C9
 1.4 with sigma of 0.02
 O049-C04K
 1.4 with sigma of 0.01
 C23-O28 \\sim O28-C26
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C04Z \\sim O049 \\sim C04K \\sim C04P \\sim C04O \\sim C04Q \\sim C04S \\sim
C04A \\sim C04W \\sim C48 \\sim C057 \\sim O051: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O30 \\sim O04L \\sim C050 \\sim C05B \\sim C14 \\sim C04F \\sim C04X \\sim C04M
\\sim C04V \\sim C05E \\sim C055 \\sim C20: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O28 \\sim C23 \\sim C27 \\sim C11 \\sim C26 \\sim C15 \\sim C19 \\sim C24 \\sim
C12 \\sim C0AA \\sim C9 \\sim O9: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O28) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(O9) \\sim Ueq, : with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Fixed Sof: Br1(0.5) Br2(0.75) Br3(0.75) Br05(0.5)
5.a Free rotating group:
 O010(H01B,H01C), O03D(H03E,H03F), O048(H04X,H04Y)
5.b Secondary CH2 refined with riding coordinates:
 C022(H02A,H02B), C02T(H02C,H02D), C039(H03A,H03B), C043(H04A,H04B), C047(H04C,
 H04D), C04N(H04L,H04M)
5.c Aromatic/amide H refined with riding coordinates:
 C016(H016), C017(H017), C01A(H01A), C01D(H01D), C01E(H01E), C01F(H01F),
 C01G(H01G), C01J(H01J), C01O(H01O), C01R(H01R), C01X(H01X), C01Y(H01Y),
 C023(H023), C029(H029), C02A(H02E), C02D(H02F), C02G(H02G), C02H(H02H),
 C02I(H02I), C02K(H02K), C02M(H02M), C02S(H02S), C02V(H02V), C02W(H02W),
 C02Y(H02Y), C030(H030), C031(H031), C032(H032), C033(H033), C034(H034),
 C035(H035), C036(H036), C037(H037), C03C(H03C), C03G(H03G), C03I(H03I),
 C03J(H03J), C03L(H03L), C03M(H03M), C03Q(H03Q), C03R(H03R), C03S(H03S),
 C03T(H03T), C03W(H03W), C03X(H03X), C03Y(H03Y), C03Z(H03Z), C041(H041),
 C044(H044), C046(H046), C04B(H04E), C04C(H04F), C04D(H04G), C04E(H04H),
 C04G(H04I), C04H(H04J), C04I(H04S), C04J(H04K), C04Q(H04Q), C04P(H04P),
 C04O(H04O), C48(H48), C04Z(H04Z), C04W(H04W), C04T(H04T), C04U(H04U),
 C05E(H05E), C055(H055), C04V(H04V), C04F(H04R), C05B(H05B), C14(H14), C23(H23),
  C26(H26), C24(H24), C19(H19), C0AA(H0AA), C12(H12)
5.d Tetrahedral OH refined with riding coordinates:
 O013(H013), O04L(H04N), O28(H28)
5.e Naphthalene refined as free rotating group:
 C04Q(C04P,C04K,C04O,C04S,C04A,C48,C057,C04Z,C04W), C05E(C20,C055,C04V,C04X,
 C04M,C04F,C05B,C050,C14), C23(C27,C26,C24,C15,C11,C19,C0AA,C9,C12)
5.f Idealised tetrahedral OH refined as rotating group:
 O00B(H00B), O00H(H00H), O00L(H00L), O02Q(H02Q), O03B(H03D), O049(H049),
 O051(H051), O30(H30), O9(H9)
;
_shelx_res_checksum              2608
_shelx_hkl_checksum              76017
_shelx_fab_checksum              42001
_olex2_submission_special_instructions 'No special instructions were received'