Acid/base controllable complexation of a triptycene-derived macrotricyclic host and protonated 4,4'-bipyridinium/pyridinium salts.
Han, Ying; Meng, Zheng; Chen, Chuan-Feng; Chemical communications (Cambridge, England) 52 (2016) 590–593; doi:10.1039/c5cc08166a

data_7118204
_publ_section_title
;
 Acid/base controllable complexation of a triptycene-derived
 macrotricyclic host and protonated 4,4'-bipyridinium/pyridinium salts.
;
_journal_issue                   3
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              590
_journal_page_last               593
_journal_paper_doi               10.1039/c5cc08166a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C68 H76 O16, 2(C11 H10 N), 2(F6 P)'
_chemical_formula_sum            'C90 H96 F12 N2 O16 P2'
_chemical_formula_weight         1751.62
_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
_audit_creation_date             2015-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-28 deposited with the CCDC.
2015-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                104.60(3)
_cell_angle_beta                 96.36(3)
_cell_angle_gamma                107.93(3)
_cell_formula_units_Z            2
_cell_length_a                   13.799(3)
_cell_length_b                   15.700(3)
_cell_length_c                   22.416(5)
_cell_measurement_reflns_used    14235
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4507
_cell_measurement_theta_min      1.4303
_cell_volume                     4377(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 40.1988
              2theta: -19.7696
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 40.1988
              2theta: -19.7696
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0123
_diffrn_orient_matrix_UB_12      0.0649
_diffrn_orient_matrix_UB_13      0.0411
_diffrn_orient_matrix_UB_21      -0.0571
_diffrn_orient_matrix_UB_22      0.0335
_diffrn_orient_matrix_UB_23      -0.0235
_diffrn_orient_matrix_UB_31      -0.0362
_diffrn_orient_matrix_UB_32      -0.0126
_diffrn_orient_matrix_UB_33      0.0273
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.1211
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32892
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.199
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_min         0.959
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       rod
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.673
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1103
_refine_ls_number_reflns         15564
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.707
_refine_ls_R_factor_all          0.2537
_refine_ls_R_factor_gt           0.1931
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3720
_refine_ls_wR_factor_ref         0.4032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9340
_reflns_number_total             15564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08166a2.cif
_cod_data_source_block           mx3807a_sq
_cod_original_cell_volume        4376.8(18)
_cod_database_code               7118204
_diffrn_number_total             19551
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-F6 = P1-F1 = P1-F3 = P1-F2 = P1-F4 = P1-F5
 1.55 with sigma of 0.01
 F6-F4
 2.2 with sigma of 0.02
 F2-F1
 2.2 with sigma of 0.02
3. Rigid bond restraints
 C7, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C42, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(P1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim
Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C57(H57A,H57B), C58(H58A,H58B),
  C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,
 H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B),
 C68(H68A,H68B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C20(H20),
 C36(H36), C39(H39), C45(H45), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53),
  N1(H1), C69(H69), C70(H70), C72(H72), C73(H73), C75(H75), C76(H76), C77(H77),
 C78(H78), C79(H79), N2(H2A), C80(H80), C81(H81), C83(H83), C84(H84), C86(H86),
 C87(H87), C88(H88), C89(H89), C90(H90)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C)
;
_shelx_res_checksum              13775
_shelx_hkl_checksum              13289
_shelx_fab_checksum              97203
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'