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_7118205
_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, C10 H10 N2, 2(F6 P), 2(C H Cl3)'
_chemical_formula_sum            'C80 H88 Cl6 F12 N2 O16 P2'
_chemical_formula_weight         1836.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-08-14
_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                90
_cell_angle_beta                 109.498(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.956(7)
_cell_length_b                   17.451(5)
_cell_length_c                   24.943(8)
_cell_measurement_reflns_used    12341
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4735
_cell_measurement_theta_min      1.5571
_cell_volume                     8599(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.1295
              2theta: -19.9598
scan:
    Number of images: 240
               Slice: -80.0000 - 40.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 45.1295
              2theta: -19.9598
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0018
_diffrn_orient_matrix_UB_12      -0.0257
_diffrn_orient_matrix_UB_13      -0.0435
_diffrn_orient_matrix_UB_21      -0.0006
_diffrn_orient_matrix_UB_22      0.0493
_diffrn_orient_matrix_UB_23      -0.0292
_diffrn_orient_matrix_UB_31      0.0406
_diffrn_orient_matrix_UB_32      -0.0061
_diffrn_orient_matrix_UB_33      -0.0112
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23915
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.557
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       rod
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.377
_exptl_crystal_size_min          0.178
_refine_diff_density_max         1.660
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.347
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         7957
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      2.333
_refine_ls_R_factor_all          0.1618
_refine_ls_R_factor_gt           0.1450
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_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          0.3594
_refine_ls_wR_factor_ref         0.3734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6621
_reflns_number_total             7957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08166a2.cif
_cod_data_source_block           sa4299a_sq
_cod_original_cell_volume        8598(5)
_cod_database_code               7118205
_shelxl_version_number           2013-4
_diffrn_number_total             10063
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21-C20 = C21A-C20
 1.54 with sigma of 0.01
 O7-C21 = O7A-C21A
 1.43 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O7 \\sim C21 \\sim C22 \\sim C23 \\sim O7A \\sim C21A \\sim C22A \\sim C23A:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O7) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(O7A) \\sim Ueq,
Uanis(C21A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H20C)=Sof(H20D)=Sof(O7A)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=
 Sof(H22C)=Sof(H22D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=1-FVAR(1)
 Sof(H20A)=Sof(H20B)=Sof(O7)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=
 Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C40(H40)
5.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C20(H20C,H20D), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C21A(H21C,
 H21D), C22A(H22C,H22D), C23A(H23C,H23D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C15(H15), C18(H18), C24(H24), C27(H27),
 N1(H1), C35(H35), C36(H36), C38(H38), C39(H39)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              68740
_shelx_hkl_checksum              17148
_shelx_fab_checksum              88507
_olex2_submission_special_instructions 'No special instructions were received'