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_4133637
_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         '6(C H Cl3), C48 H20 Cl4 N12 O12'
_chemical_formula_sum            'C54 H26 Cl22 N12 O12'
_chemical_formula_weight         1814.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
????
;
_cell_angle_alpha                90
_cell_angle_beta                 94.079(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.035(3)
_cell_length_b                   21.931(7)
_cell_length_c                   17.509(6)
_cell_measurement_reflns_used    12307
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4172
_cell_measurement_theta_min      1.1660
_cell_volume                     3844(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0034
_diffrn_orient_matrix_UB_12      0.0997
_diffrn_orient_matrix_UB_13      0.0047
_diffrn_orient_matrix_UB_21      0.0071
_diffrn_orient_matrix_UB_22      0.0023
_diffrn_orient_matrix_UB_23      -0.0450
_diffrn_orient_matrix_UB_31      -0.0565
_diffrn_orient_matrix_UB_32      0.0026
_diffrn_orient_matrix_UB_33      -0.0088
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26065
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.196
_diffrn_reflns_theta_max         25.196
_diffrn_reflns_theta_min         1.491
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6892
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.1023
_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^)+(0.1080P)^2^+10.1746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2567
_refine_ls_wR_factor_ref         0.2666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6009
_reflns_number_total             6892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12018_si_002.cif
_cod_data_source_block           mx2823
_cod_original_cell_volume        3843(2)
_cod_database_code               4133637
_shelx_shelxl_version_number     2014/7
_diffrn_number_total             8935
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Cl9 \\sim Cl10 \\sim Cl11 \\sim C27 \\sim Cl9A \\sim C27A \\sim Cl \\sim Cl12:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(Cl9) \\sim Ueq, Uanis(Cl10) \\sim Ueq, Uanis(Cl11) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(Cl9A) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(Cl) \\sim Ueq,
Uanis(Cl12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Cl9A)=Sof(C27A)=Sof(H27A)=Sof(Cl)=Sof(Cl12)=1-FVAR(1)
 Sof(Cl9)=Sof(Cl10)=Sof(Cl11)=Sof(C27)=Sof(H27)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C27(H27), C26(H26), C25(H25), C27A(H27A)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C9(H9), C14(H14), C15(H15), C16(H16), C18(H18), C21(H21),
 C22(H22), C24(H24)
;
_shelx_res_checksum              92622
_shelx_hkl_checksum              46068
_olex2_submission_special_instructions 'No special instructions were received'