Complexation of Triptycene-Derived Macrotricyclic Polyether with Paraquat Derivatives, Diquat, and a 2,7-Diazapyrenium Salt: Guest-Induced Conformational Changes of the Host
Ying Han; Jing Cao; Peng-Fei Li; Qian-Shou Zong; Jian-Min Zhao; Jia-Bin Guo; Jun-Feng Xiang; Chuan-Feng Chen; Journal of Organic Chemistry 78 (2013) 3235–3242; doi:10.1021/jo400148b

data_4028114
_publ_section_title
;
 Complexation of Triptycene-Derived Macrotricyclic Polyether with Paraquat
 Derivatives, Diquat, and a 2,7-Diazapyrenium Salt: Guest-Induced
 Conformational Changes of the Host
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3235
_journal_page_last               3242
_journal_paper_doi               10.1021/jo400148b
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C76 H92 O20, 2(C2 H3 N)'
_chemical_formula_sum            'C80 H98 N2 O20'
_chemical_formula_weight         1407.60
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 107.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.5258(17)
_cell_length_b                   34.215(7)
_cell_length_c                   13.071(3)
_cell_measurement_reflns_used    11852
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4625
_cell_measurement_theta_min      1.7349
_cell_volume                     3645.2(15)
_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      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26796
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.292
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         6403
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.293
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0960
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+5.1022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                5678
_reflns_number_total             6403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo400148b_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        3645.3(13)
_cod_database_code               4028114