Inherently Chiral Bambus[4]urils.
Mohite, Amar Ramchandra; Reany, Ofer; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c01174

data_4038523
_publ_section_title
;
 Inherently Chiral Bambus[4]urils.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01174
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C52 H56 N16 O8 [+ solvent]'
_chemical_formula_sum            'C52 H56 N16 O8'
_chemical_formula_weight         1033.12
_chemical_name_common            ro24_sq
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 127.66(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.264(5)
_cell_length_b                   18.390(4)
_cell_length_c                   17.423(4)
_cell_measurement_reflns_used    8386
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.052
_cell_measurement_theta_min      1.565
_cell_volume                     5901(3)
_computing_cell_refinement       'APEX2 v2010.7-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2010.7.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'APEX2 (Bruker AXS)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13822
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.052
_diffrn_reflns_theta_max         25.052
_diffrn_reflns_theta_min         1.565
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       needle
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 2174 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         8386
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0854
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1347P)^2^+14.8296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2310
_refine_ls_wR_factor_ref         0.2551
_reflns_Friedel_coverage         0.616
_reflns_Friedel_fraction_full    0.612
_reflns_Friedel_fraction_max     0.612
_reflns_number_gt                6453
_reflns_number_total             8386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01174_si_002.cif
_cod_data_source_block           ro24_sq
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4038523
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.969
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              15135
_shelx_hkl_checksum              43668
_shelx_fab_checksum              24048