Regulating the Structures of Self-Assembled Mechanically Interlocked Moleculecular Constructs via Dianion Precursor Substituent Effects.
Chen, Xu-Lang; Shen, Yun-Jia; Gao, Chao; Yang, Jian; Sun, Xin; Zhang, Xin; Yang, Yu-Dong; Wei, Gong-Ping; Xiang, Jun-Feng; Sessler, Jonathan L.; Gong, Han-Yuan; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b13473

data_4134656
_publ_section_title
;
 Regulating the Structures of Self-Assembled Mechanically Interlocked
 Moleculecular Constructs via Dianion Precursor Substituent Effects.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13473
_journal_year                    2020
_chemical_formula_sum            'C102 H99 Br16 Eu4 N10 O56.5'
_chemical_formula_weight         4255.31
_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                84.418(4)
_cell_angle_beta                 67.062(5)
_cell_angle_gamma                84.129(4)
_cell_formula_units_Z            1
_cell_length_a                   14.0288(8)
_cell_length_b                   14.7086(8)
_cell_length_c                   17.4117(8)
_cell_measurement_reflns_used    11543
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      3.364
_cell_volume                     3284.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 5.3127
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27775
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.364
_exptl_absorpt_coefficient_mu    6.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91152
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.151
_exptl_crystal_description       block
_exptl_crystal_F_000             2045
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         4.118
_refine_diff_density_min         -2.359
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         11543
_refine_ls_number_restraints     323
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0648
_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^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8214
_reflns_number_total             11543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13473_si_024.cif
_cod_data_source_block           D_SQ
_cod_original_formula_sum        'C102 H99 Br16 Eu4 N10 O56.50'
_cod_database_code               4134656
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              28447
_shelx_hkl_checksum              9891
_shelx_fab_checksum              15908