Triptycene walled glycoluril trimer: synthesis and recognition properties
Ndendjio, Sandra Zebaze; Liu, Wenjin; Yvanez, Nicolas; Meng, Zihui; Zavalij, Peter Y.; Isaacs, Lyle; New Journal of Chemistry 44 (2020) 338–345; doi:10.1039/C9NJ05336K

data_7059158
_publ_section_title
;
 Triptycene walled glycoluril trimer: synthesis and recognition properties
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              338
_journal_page_last               345
_journal_paper_doi               10.1039/C9NJ05336K
_journal_volume                  44
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety
'Na12, 3(C76 H74 N12 O22 S4), 2(C2 H F3 O2), 117(H2 O)'
_chemical_formula_sum            'C232 H458 F6 N36 Na12 O217 S12'
_chemical_formula_weight         7998.92
_chemical_name_systematic        'Trimer Trip'
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2015 & ZCIF'
_audit_update_record
;
2019-08-27 deposited with the CCDC.	2019-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.369(2)
_cell_length_b                   29.369(2)
_cell_length_c                   50.089(4)
_cell_measurement_reflns_used    23969
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.4
_cell_measurement_theta_min      2.2
_cell_volume                     43204(5)
_computing_cell_refinement       'Apex2, Saint'
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'Olex2 (Dolomanov, 2009)'
_computing_publication_material  'Apex2, SHELXL-2015, Platon (Spek, 2015)'
_computing_structure_refinement  'ShelXL-2015 (Sheldrick, 2015c)'
_computing_structure_solution    'ShelXT-2014 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0254070
_diffrn_orient_matrix_UB_12      -0.0227050
_diffrn_orient_matrix_UB_13      0.0002432
_diffrn_orient_matrix_UB_21      -0.0192745
_diffrn_orient_matrix_UB_22      -0.0219044
_diffrn_orient_matrix_UB_23      -0.0102973
_diffrn_orient_matrix_UB_31      0.0119647
_diffrn_orient_matrix_UB_32      0.0128553
_diffrn_orient_matrix_UB_33      -0.0171136
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            106628
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_min         1.751
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause et al, 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             16864
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water / ethanol'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 6471 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1709
_refine_ls_number_reflns         28094
_refine_ls_number_restraints     870
_refine_ls_restrained_S_all      1.295
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+11.0900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                17961
_reflns_number_total             28094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05336k2.cif
_cod_data_source_block           UM3234
_cod_depositor_comments
;Adding full bibliography for 7059158.cif.

 Adding full bibliography for 7059158.cif.
;
_cod_original_cell_volume        43204(7)
_cod_database_code               7059158
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.950
_shelx_res_checksum              2677
_shelx_fab_checksum              89901