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_4028115
_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
;
2(C38 H41.89718 O10), 2(C6 H7 N), 2(F4.3176 P), 3.59324(H), 3.36492(F)
;
_chemical_formula_sum            'C96 H122 F12 N2 O22 P2'
_chemical_formula_weight         1945.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                102.491(2)
_cell_angle_beta                 101.542(2)
_cell_angle_gamma                108.119(2)
_cell_formula_units_Z            1
_cell_length_a                   13.7223(14)
_cell_length_b                   14.0686(14)
_cell_length_c                   14.3950(14)
_cell_measurement_reflns_used    4877
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.36
_cell_volume                     2469.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12616
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.518804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS v.2.10 (Bruker,2003) was used for absorption correction.
 R(int) was 0.0572 before and 0.0155 after correction.
 The Ratio of minimum to maximum transmission is 0.518804.
 The \l/2 correction factor is 0.0015
;
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_F_000             1026
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         8644
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0919P)^2^+1.9789P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1986
_reflns_number_gt                5769
_reflns_number_total             8644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo400148b_si_003.cif
_cod_data_source_block           50601C
_cod_database_code               4028115