Supramolecular assemblies controlled by cucurbit[n]uril size (n = 6, 7, 8 and 10)
Xu, Weitao; Deng, Xinyu; Xiao, Xin; Bian, Bing; Chen, Qing; Dalgarno, Scott J.; Tao, Zhu; Redshaw, Carl; New Journal of Chemistry 44 (2020) 4311–4318; doi:10.1039/D0NJ00087F

data_7059331
_publ_section_title
;
 Supramolecular assemblies controlled by cucurbit[n]uril size (n = 6, 7, 8
 and 10)
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4311
_journal_page_last               4318
_journal_paper_doi               10.1039/D0NJ00087F
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         '2(C24 H24 N16 O8), C12 H12 N, Cd3 Cl11'
_chemical_formula_sum            'C60 H79 Cd3 Cl11 N34 O20'
_chemical_formula_weight         2323.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-11 deposited with the CCDC.	2020-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.9000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6911(4)
_cell_length_b                   32.6874(6)
_cell_length_c                   20.6631(4)
_cell_measurement_reflns_used    9733
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.34
_cell_measurement_theta_min      3.47
_cell_volume                     13723.1(5)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex III'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            228968
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.122
_diffrn_reflns_theta_min         2.560
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.143
_refine_diff_density_min         -1.667
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1114
_refine_ls_number_reflns         26957
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24210
_reflns_number_total             26957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0nj00087f2.cif
_cod_data_source_block           Q8GCd
_cod_depositor_comments
;Adding full bibliography for 7059329--7059331.cif.

 Adding full bibliography for 7059329--7059331.cif.
;
_cod_database_code               7059331
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.345
_shelx_estimated_absorpt_t_min   0.223
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C52-C51 = C51-C50 = C50-C49 = C54-C49 = C53-C52 = C54-C53
 1.39 with sigma of 0.02
 N33-C60 = N33-C56 = C57-C56 = C59-C58 = C58-C57 = C60-C59
 1.39 with sigma of 0.02
 C55-C49 = N33-C55
 1.45 with sigma of 0.02
 C50-C55 \\sim C55-C54
 with sigma of 0.001
3. Restrained planarity
 C56, C57, C58, C59, C60, N33
 with sigma of 0.1
 C49, C50, C51, C52, C53, C54
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C55) \\sim Ueq,
Uanis(N33) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C49, C50, C54, C55, C51, C53, N33, C52, C56, C60, C57, C59, C58
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C49(0.5) C50(0.5) H50(0.5) C51(0.5) H51(0.5) C52(0.5) H52(0.5)
 C53(0.5) H53(0.5) C54(0.5) H54(0.5) C55(0.5) H55A(0.5) H55B(0.5) C56(0.5)
 H56(0.5) C57(0.5) H57(0.5) C58(0.5) H58(0.5) C59(0.5) H59(0.5) C60(0.5)
 H60(0.5) N33(0.5) C1A(0.5) C1B(0.5) H1BA(0.5) C1C(0.5) H1C(0.5) C1D(0.5)
 H1DA(0.5) H1DB(0.5) C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5) N1A(0.5) C1G(0.5)
 H1G(0.5) C1H(0.5) H1H(0.5) C1I(0.5) H1I(0.5) C1J(0.5) H1J(0.5) C1K(0.5)
 H1K(0.5) C1L(0.5) H1L(0.5)
 Fixed Uiso: C1A(0.2) C1B(0.2) C1C(0.2) C1D(0.2) C1E(0.2) C1F(0.2) N1A(0.2)
 C1G(0.2) C1H(0.2) C1I(0.2) C1J(0.2) C1K(0.2) C1L(0.2)
7.a Free rotating group:
 C1A(C1B,C1C,C1D,C1E,C1F,N1A,C1G,C1H,C1I,C1J,C1K,C1L)
7.b Ternary CH refined with riding coordinates:
 C2(H2), C7(H7), C8(H8), C13(H13), C14(H14), C19(H19), C20(H20), C24(H24),
 C27(H27), C28(H28), C33(H33), C34(H34), C39(H39), C40(H40), C45(H45), C46(H46)
7.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B), C10(H10A,H10B), C11(H11A,H11B),
 C16(H16A,H16B), C17(H17A,H17B), C22(H22A,H22B), C25(H25A,H25B), C30(H30A,H30B),
  C31(H31A,H31B), C36(H36A,H36B), C37(H37A,H37B), C42(H42A,H42B), C43(H43A,
 H43B), C48(H48A,H48B), C55(H55A,H55B), C1D(H1DA,H1DB)
7.d Aromatic/amide H refined with riding coordinates:
 C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
 C58(H58), C59(H59), C60(H60), C1B(H1BA), C1C(H1C), C1E(H1E), C1F(H1F),
 C1G(H1G), C1H(H1H), C1I(H1I), C1J(H1J), C1K(H1K), C1L(H1L)
;
_olex2_submission_special_instructions 'No special instructions were received'