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_1562688
_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         '2(I3), 2(Br), C90 H54 N12 O12'
_chemical_formula_sum            'C90 H54 Br2 I6 N12 O12'
_chemical_formula_weight         2416.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 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                90
_cell_angle_beta                 99.440(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1313(8)
_cell_length_b                   23.4871(17)
_cell_length_c                   31.769(2)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      52.84
_cell_measurement_theta_min      2.95
_cell_volume                     8929.3(10)
_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      172.99
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.980
_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  0.1417
_diffrn_reflns_av_unetI/netI     0.1407
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            84247
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.430
_diffrn_reflns_theta_min         2.949
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.046
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1664 before and 0.1052 after correction. The Ratio of minimum to maximum transmission is 0.6252. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       block
_exptl_crystal_F_000             4648
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         5.206
_refine_diff_density_min         -2.003
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.649
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1114
_refine_ls_number_reflns         16949
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.646
_refine_ls_R_factor_all          0.2937
_refine_ls_R_factor_gt           0.1652
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+80.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3397
_refine_ls_wR_factor_ref         0.3825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6308
_reflns_number_total             16949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02242c2.cif
_cod_data_source_block           201215fs_164i3_0m
_cod_depositor_comments
'Adding full bibliography for 1562686--1562691.cif.'
_cod_original_cell_volume        8929.4(11)
_cod_database_code               1562688
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C6, C8
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C60 \\sim C61: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C70) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C73)
\\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C90) \\sim Ueq,
Uanis(C64) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Fixed Sof: I6(0.5) I7(0.5) Br1(0.5) Br2(0.5) Br3(0.5) Br4(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C9(H9A,H9B), C34(H34A,H34B), C41(H41A,H41B),
 C42(H42A,H42B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C14(H14), C17(H17),
 C18(H18), C23(H23), C24(H24), C30(H30), C31(H31), C32(H32), C33(H33), C36(H36),
  C38(H38), C40(H40), C43(H43), C44(H44), C45(H45), C47(H47), C56(H56),
 C57(H57), C50(H50), C51(H51), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67),
  C68(H68), C69(H69), C71(H71), C74(H74), C75(H75), C80(H80), C81(H81),
 C87(H87), C88(H88), C89(H89), C90(H90)
5.c Fitted hexagon refined as free rotating group:
 C60(C49,C50,C51,C52,C61)
;
_shelx_res_checksum              66184
_shelx_hkl_checksum              20633
_shelx_fab_checksum              21554
_olex2_submission_special_instructions 'No special instructions were received'