Synthesis of Triptycene-Derived Macrotricyclic Host Containing Two Dibenzo-[18]-crown-6 Moieties and Its Complexation with Paraquat Derivatives: Li±Ion-Controlled Binding and Release of the Guests in the Complexes
Ying Han; Hai-Yan Lu; Qian-Shou Zong; Jia-Bin Guo; Chuan-Feng Chen; Journal of Organic Chemistry 77 (2012) 2422–2430; doi:10.1021/jo3000755

data_4027049
_publ_section_title
;
 Synthesis of Triptycene-Derived Macrotricyclic Host Containing Two
 Dibenzo-[18]-crown-6 Moieties and Its Complexation with Paraquat
 Derivatives: Li+-Ion-Controlled Binding and Release of the Guests in the
 Complexes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2422
_journal_page_last               2430
_journal_paper_doi               10.1021/jo3000755
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C60 H60 O12, 2(C14 H18 N2 O2), 4(F6 P)'
_chemical_formula_sum            'C88 H96 F24 N4 O16 P4'
_chemical_formula_weight         2045.57
_chemical_name_systematic
; 
 ? 
;
_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                73.342(12)
_cell_angle_beta                 76.401(12)
_cell_angle_gamma                71.387(11)
_cell_formula_units_Z            2
_cell_length_a                   13.274(2)
_cell_length_b                   16.473(3)
_cell_length_c                   21.939(4)
_cell_measurement_reflns_used    11994
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.47
_cell_volume                     4300.7(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    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0766
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33191
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  0.9937
_exptl_absorpt_correction_T_min  0.9354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       plate
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.007
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1263
_refine_ls_number_reflns         15580
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      2.053
_refine_ls_R_factor_all          0.1797
_refine_ls_R_factor_gt           0.1456
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3436
_refine_ls_wR_factor_ref         0.3608
_reflns_number_gt                10925
_reflns_number_total             15580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo3000755_si_003.cif
_cod_data_source_block           mx985
_cod_original_cell_volume        4300.6(12)
_cod_database_code               4027049