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_4133638
_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         'C48 H20 Cl4 N12 O12, 4(C3 H7 N O), 2(C2 H3 N)'
_chemical_formula_sum            'C64 H54 Cl4 N18 O16'
_chemical_formula_weight         1473.05
_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   mixed
_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                82.49(3)
_cell_angle_beta                 67.68(3)
_cell_angle_gamma                67.96(2)
_cell_formula_units_Z            1
_cell_length_a                   12.036(5)
_cell_length_b                   12.274(6)
_cell_length_c                   13.289(5)
_cell_measurement_reflns_used    5313
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      31.2119
_cell_measurement_theta_min      1.6567
_cell_volume                     1683.2(13)
_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
;
'SHELXT (Sheldrick, 2015)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0410
_diffrn_orient_matrix_UB_12      -0.0862
_diffrn_orient_matrix_UB_13      -0.0108
_diffrn_orient_matrix_UB_21      -0.0070
_diffrn_orient_matrix_UB_22      0.0208
_diffrn_orient_matrix_UB_23      0.0851
_diffrn_orient_matrix_UB_31      -0.0811
_diffrn_orient_matrix_UB_32      -0.0054
_diffrn_orient_matrix_UB_33      -0.0042
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0809
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6040
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.199
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_min         1.790
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.774
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         6040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.774
_refine_ls_R_factor_all          0.1525
_refine_ls_R_factor_gt           0.1334
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3218
_refine_ls_wR_factor_ref         0.3341
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4853
_reflns_number_total             6040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12018_si_003.cif
_cod_data_source_block           sa3316
_cod_original_cell_volume        1683.3(13)
_cod_database_code               4133638
_shelx_shelxl_version_number     2014/7
_diffrn_number_total             7622
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.849(4) 0.151(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Riding coordinates:
 C31(H31A,H31B,H31C)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C9(H9), C14(H14), C16(H16), C17(H17), C18(H18), C21(H21),
 C23(H23), C24(H24), C30(H30), C27(H27)
3.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C)
;
_shelx_res_checksum              43335
_shelx_hkl_checksum              49163
_olex2_submission_special_instructions 'No special instructions were received'