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_7059329
_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(C16 H19 N2), Cd Cl4'
_chemical_formula_sum            'C32 H38 Cd Cl4 N4'
_chemical_formula_weight         732.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-09
_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                 126.789(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.476(4)
_cell_length_b                   16.376(3)
_cell_length_c                   18.658(3)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.40
_cell_measurement_theta_min      2.49
_cell_volume                     6723.2(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker Apex II'
_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      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54015
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.851
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0821 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.8326.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       Block
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00052(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6596
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+7.6175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4425
_reflns_number_total             6596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00087f2.cif
_cod_data_source_block           G
_cod_depositor_comments
;Adding full bibliography for 7059329--7059331.cif.

 Adding full bibliography for 7059329--7059331.cif.
;
_cod_original_cell_volume        6723.1(18)
_cod_database_code               7059329
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C32B \\sim C30B \\sim C31B \\sim C29B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C13 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C31A) \\sim Ueq, Uanis(C31B) \\sim Ueq, Uanis(C30A) \\sim Ueq,
Uanis(C30B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C32A, C31B, C30A, C29A, N4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C29B, C32B, C30B, C31A, N4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C29B)=Sof(H29A)=Sof(H29B)=Sof(C30B)=Sof(H30A)=Sof(H30B)=Sof(C32B)=
 Sof(H32A)=Sof(H32B)=Sof(C31A)=Sof(H31C)=Sof(H31D)=1-FVAR(1)
 Sof(C31B)=Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(C30A)=
 Sof(H30C)=Sof(H30D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
 C23(H23A,H23B), C29B(H29A,H29B), C30B(H30A,H30B), C31B(H31A,H31B), C32B(H32A,
 H32B), C32A(H32C,H32D), C31A(H31C,H31D), C30A(H30C,H30D), C29A(H29C,H29D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27),
  C28(H28)
;
_olex2_submission_special_instructions 'No special instructions were received'