Self-Assembled Cagelike Receptor That Binds Biologically Relevant Dicarboxylic Acids via Proton-Coupled Anion Recognition.
Wang, Fei; Sen, Sajal; Chen, Chuang; Bähring, Steffen; Lei, Chuanhu; Duan, Zhiming; Zhang, Zhan; Sessler, Jonathan L.; Jana, Atanu; Journal of the American Chemical Society 142 (2020) 1987–1994; doi:10.1021/jacs.9b11566

data_4133940
_publ_section_title
;
 Self-Assembled Cagelike Receptor That Binds Biologically Relevant
 Dicarboxylic Acids via Proton-Coupled Anion Recognition.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1987
_journal_page_last               1994
_journal_paper_doi               10.1021/jacs.9b11566
_journal_volume                  142
_journal_year                    2020
_chemical_formula_sum            'C52 H68 N6 O9'
_chemical_formula_weight         921.12
_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   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                73.739(2)
_cell_angle_beta                 86.373(3)
_cell_angle_gamma                68.275(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0076(6)
_cell_length_b                   14.8684(7)
_cell_length_c                   17.0843(8)
_cell_measurement_reflns_used    9699
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.075
_cell_measurement_theta_min      2.697
_cell_volume                     2717.3(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'APEX3 v2017.3-0'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  CCD-area-detector
_diffrn_measurement_method       CCD-area-detector
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2760
_diffrn_reflns_av_unetI/netI     0.0838
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            103564
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         2.697
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.00092(7)
_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   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         9699
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.2511
_refine_ls_R_factor_gt           0.1250
_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^)+(0.0050P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3367
_reflns_number_total             9699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11566_si_005.cif
_cod_data_source_block           Host_with_Oxalic_acid
_cod_depositor_comments
'Adding full bibliography for 4133937--4133942.cif.'
_cod_database_code               4133940
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              22321
_shelx_hkl_checksum              72750
_shelx_fab_checksum              51529