Formation of 1:2 host-guest complexes based on triptycene-derived macrotricycle and paraquat derivatives: anion-π interactions between PF6(-) and bipyridinium rings in the solid state.
Guo, Jia-Bin; Han, Ying; Cao, Jing; Chen, Chuan-Feng; Organic letters 13 (2011) 5688–5691; doi:10.1021/ol2024168

data_1502548
_publ_section_title
;
 Formation of 1:2 host-guest complexes based on triptycene-derived
 macrotricycle and paraquat derivatives: anion-\p interactions between
 PF6(-) and bipyridinium rings in the solid state.
;
_journal_issue                   20
_journal_name_full               'Organic letters'
_journal_page_first              5688
_journal_page_last               5691
_journal_paper_doi               10.1021/ol2024168
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C108 H84 F30 N4 O20 P5'
_chemical_formula_weight         2482.64
_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                98.87(3)
_cell_angle_beta                 96.79(3)
_cell_angle_gamma                92.84(3)
_cell_formula_units_Z            3
_cell_length_a                   14.087(3)
_cell_length_b                   24.772(5)
_cell_length_c                   26.889(5)
_cell_measurement_reflns_used    21442
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.3139
_cell_measurement_theta_min      1.2250
_cell_volume                     9184(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            88952
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         0.77
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3777
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
;
_refine_diff_density_max         1.664
_refine_diff_density_min         -2.069
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       0.00032(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   2.602
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2025
_refine_ls_number_reflns         33273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.602
_refine_ls_R_factor_all          0.2659
_refine_ls_R_factor_gt           0.2277
_refine_ls_shift/su_max          0.143
_refine_ls_shift/su_mean         0.017
_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          0.5147
_refine_ls_wR_factor_ref         0.5319
_reflns_number_gt                20495
_reflns_number_total             33273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol2024168_si_002.cif
_cod_data_source_block           a
_cod_depositor_comments
;

2019-04-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C324 H252 F88 N12 O60 P15'
_cod_original_formula_weight         7409.93
_cod_original_formula_units_Z            1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1502548