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_4028116
_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_sum            'C124 H136 F24 N4 O20 P4'
_chemical_formula_weight         2582.25
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.520(8)
_cell_angle_beta                 83.827(8)
_cell_angle_gamma                65.386(4)
_cell_formula_units_Z            1
_cell_length_a                   14.418(2)
_cell_length_b                   15.829(3)
_cell_length_c                   15.956(3)
_cell_measurement_reflns_used    10206
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4795
_cell_measurement_theta_min      1.6135
_cell_volume                     3290.7(10)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24500
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.68229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.92
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
;
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         11510
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+5.5630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.1924
_reflns_number_gt                9332
_reflns_number_total             11510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo400148b_si_004.cif
_cod_data_source_block           a
_cod_original_cell_volume        3290.7(9)
_cod_database_code               4028116