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_7059330
_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
'C96 H96 N64 Na2 O40, 4(Cl4 Zn), 0.5(C32 H36 N4)'
_chemical_formula_sum            'C112 H146 Cl16 N66 Na2 O45 Zn4'
_chemical_formula_weight         4011.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.023(3)
_cell_length_b                   22.025(2)
_cell_length_c                   28.035(3)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.45
_cell_volume                     19773(3)
_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      222.98
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD Diffractometer'
_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  0.0354
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            94549
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.326
_diffrn_reflns_theta_min         2.451
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             8216
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.502
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         12491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.001
_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          0.2562
_refine_ls_wR_factor_ref         0.2777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9807
_reflns_number_total             12491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00087f2.cif
_cod_data_source_block           Q8GNaZn
_cod_depositor_comments
;Adding full bibliography for 7059329--7059331.cif.

 Adding full bibliography for 7059329--7059331.cif.
;
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7059330
_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
Uanis(O12) = Uanis(O11)
Uanis(O13) = Uanis(O14)
3. Others
 Fixed Sof: O11(0.5) O12(0.5) O13(0.5) O14(0.5) C1B(0.25) C1C(0.25) H1C(0.25)
 C1D(0.25) H1D(0.25) C1E(0.25) H1EA(0.25) H1EB(0.25) C1F(0.25) H1F(0.25)
 C1G(0.25) H1G(0.25) N19(0.25) C1H(0.25) H1H(0.25) C1I(0.25) H1I(0.25)
 C1J(0.25) H1J(0.25) C1K(0.25) H1K(0.25) C1L(0.25) H1L(0.25) C1M(0.25)
 N26(0.25) C1N(0.25) H1NA(0.25) H1NB(0.25) C1O(0.25) H1O(0.25) C1P(0.25)
 H1PA(0.25) H1PB(0.25) C1Q(0.25) H1QA(0.25) H1QB(0.25)
 Fixed Uiso: C1B(0.125) C1C(0.125) H1C(0.125) C1D(0.125) H1D(0.125) C1E(0.125)
 H1EA(0.125) H1EB(0.125) C1F(0.125) H1F(0.125) C1G(0.125) H1G(0.125) N19(0.125)
 C1H(0.125) H1H(0.125) C1I(0.125) H1I(0.125) C1J(0.125) H1J(0.125) C1K(0.125)
 H1K(0.125) C1L(0.125) H1L(0.125) C1M(0.125) N26(0.125) C1N(0.125) H1NA(0.125)
 H1NB(0.125) C1O(0.125) H1O(0.125) C1P(0.125) H1PA(0.125) H1PB(0.125)
 C1Q(0.125) H1QA(0.125) H1QB(0.125)
4.a Free rotating group:
 C1B(C1C,C1D,C1E,C1F,C1G,N19,C1H,C1I,C1J,C1K,C1L,C1M,N26,C1N,C1O,C1P,C1Q)
4.b Ternary CH refined with riding coordinates:
 C2(H2), C7(H7), C9(H9), C13(H13), C15(H15), C19(H19), C21(H21), C25(H25)
4.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C10(H10A,H10B), C11(H11A,H11B), C16(H16A,H16B),
 C17(H17A,H17B), C22(H22A,H22B), C23(H23A,H23B), C1E(H1EA,H1EB), C1N(H1NA,H1NB),
  C1P(H1PA,H1PB), C1Q(H1QA,H1QB)
4.d Aromatic/amide H refined with riding coordinates:
 C1C(H1C), C1D(H1D), C1F(H1F), C1G(H1G), C1H(H1H), C1I(H1I), C1J(H1J),
 C1K(H1K), C1L(H1L), C1O(H1O)
;
_olex2_submission_special_instructions 'No special instructions were received'