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_4027050
_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_sum            'C76 H82 F12 N2 O14 P2'
_chemical_formula_weight         1537.38
_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                61.238(11)
_cell_angle_beta                 64.049(13)
_cell_angle_gamma                78.738(16)
_cell_formula_units_Z            1
_cell_length_a                   12.469(3)
_cell_length_b                   13.495(4)
_cell_length_c                   13.729(3)
_cell_measurement_reflns_used    5629
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4800
_cell_measurement_theta_min      1.7217
_cell_volume                     1820.6(8)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'MM007HF + CCD (Saturn724+)'
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14950
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       plate
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8188
_refine_ls_number_restraints     669
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0988P)^2^+1.3506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2055
_refine_ls_wR_factor_ref         0.2196
_reflns_number_gt                6603
_reflns_number_total             8188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo3000755_si_004.cif
_cod_data_source_block           a
_cod_original_cell_volume        1820.5(7)
_cod_database_code               4027050