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_4133941
_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            'C48 H57 Cl6 N6 O4'
_chemical_formula_weight         994.69
_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                78.46(3)
_cell_angle_beta                 88.91(3)
_cell_angle_gamma                69.37(3)
_cell_formula_units_Z            2
_cell_length_a                   12.130(2)
_cell_length_b                   14.831(3)
_cell_length_c                   16.344(3)
_cell_measurement_reflns_used    51063
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      0.37
_cell_volume                     2691.9(11)
_computing_cell_refinement       HKL3000
_computing_data_collection
;
marccd, control software for MarCCD-300 detector
;
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type
;
Shanghai Synchrotron Radiation Facility, beam line station 
BL17B, Bruker/ARINAX MD2 equipped with a MarCCD-300 detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68875
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8980
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        24.295
_diffrn_reflns_theta_max         24.295
_diffrn_reflns_theta_min         1.701
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995, 1997)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1042
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.667
_refine_diff_density_min         -1.235
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.084(10)
_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   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         8980
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.2016
_refine_ls_R_factor_gt           0.1903
_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^)+(0.1000P)^2^+30.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3995
_refine_ls_wR_factor_ref         0.4041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8025
_reflns_number_total             8980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11566_si_003.cif
_cod_data_source_block           output_Compound_7
_cod_depositor_comments
'Adding full bibliography for 4133937--4133942.cif.'
_cod_original_cell_volume        2691.9(10)
_cod_database_code               4133941
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              30321
_shelx_hkl_checksum              54357
_shelx_fab_checksum              40273