Toward Anion-π Interactions Directed Self-Assembly with Predesigned Dual Macrocyclic Receptors and Dianions.
Tuo, De-Hui; Liu, Wei; Wang, Xue-Yuan; Wang, Xu-Dong; Ao, Yu-Fei; Wang, Qi-Qiang; Li, Zhi-Yan; Wang, De-Xian; Journal of the American Chemical Society 141 (2019) 1118–1125; doi:10.1021/jacs.8b12018

data_4133634
_publ_section_title
;
 Toward Anion-\p Interactions Directed Self-Assembly with Predesigned Dual
 Macrocyclic Receptors and Dianions.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1118
_journal_page_last               1125
_journal_paper_doi               10.1021/jacs.8b12018
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C44 H18 Cl4 N12 O12'
_chemical_formula_sum            'C44 H18 Cl4 N12 O12'
_chemical_formula_weight         1048.50
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.286(6)
_cell_length_b                   13.537(3)
_cell_length_c                   16.108(3)
_cell_measurement_reflns_used    6858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4839
_cell_measurement_theta_min      1.4169
_cell_volume                     5503(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics
;
 Mercury: visualization and analysis of crystal structures, C. F. Macrae,
 P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
 M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006.
;
_computing_publication_material  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELX-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'MM007HF + CCD (Saturn724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_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            19430
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.701
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6298
_refine_ls_number_restraints     450
_refine_ls_restrained_S_all      1.781
_refine_ls_R_factor_all          0.2087
_refine_ls_R_factor_gt           0.1367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3444
_refine_ls_wR_factor_ref         0.3746
_reflns_number_gt                2983
_reflns_number_total             6298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b12018_si_001.cif
_cod_data_source_block           a
_cod_original_cell_volume        5502.9(19)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4133634