Host-guest inclusion complexes formed between a symmetrical tetrasubstituted cucurbit[6]uril and glycine
Yuan, Shang-Wei; Shan, Pei-Hui; Yang, Mao Xia; Ma, PeiHua; Prior, Timothy J.; Redshaw, Carl; Wei, Gang; Tao, Zhu; Xiao, Xin; CrystEngComm  (2022) –; doi:10.1039/D2CE01308H

data_7245808
_publ_section_title
;
 Host-guest inclusion complexes formed between a symmetrical
 tetrasubstituted cucurbit[6]uril and glycine
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01308H
_journal_year                    2022
_chemical_formula_moiety
'C40 H54 Ca N24 O17, 3(Cl), C2 H6 N O2, 16[H2O]'
_chemical_formula_sum            'C42 H92 Ca Cl3 N25 O35'
_chemical_formula_weight         1653.83
_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             2022-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-25 deposited with the CCDC.	2022-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                72.765(7)
_cell_angle_beta                 76.725(7)
_cell_angle_gamma                68.800(7)
_cell_formula_units_Z            2
_cell_length_a                   13.001(4)
_cell_length_b                   14.691(4)
_cell_length_c                   21.030(6)
_cell_measurement_reflns_used    7767
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      22.536
_cell_measurement_theta_min      2.312
_cell_volume                     3542.7(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44481
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.628
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1263 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.8985.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         12511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0909P)^2^+4.2694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8467
_reflns_number_total             12511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01308h2.cif
_cod_data_source_block           complex2
_cod_original_cell_volume        3542.8(18)
_cod_database_code               7245808
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.949
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
2.b Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9), C22(H22), C23(H23), C28(H28), C29(H29)
2.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C11(H11A,H11B), C12(H12A,H12B), C19(H19A,H19B),
 C20(H20A,H20B), C25(H25A,H25B), C26(H26A,H26B), C31(H31A,H31B), C32(H32A,H32B),
  C39(H39A,H39B), C40(H40A,H40B), C42(H42A,H42B)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C35(H35A,H35B,H35C), C37(H37A,H37B,
 H37C), N25(H25C,H25D,H25E)
2.e Idealised tetrahedral OH refined as rotating group:
 O14(H14)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 321 electrons were 
found in a volume of 950\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
16[H2O] per Asymmetric Unit 
which account for 320 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              86057
_shelx_fab_checksum              61939
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'