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_7118206
_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(C12 H12 N O), 2(F6 P), 2(H2 O)'
_chemical_formula_sum            'C92 H104 F12 N2 O20 P2'
_chemical_formula_weight         1847.71
_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   mixed
_atom_sites_solution_primary     direct
_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                108.815(19)
_cell_angle_beta                 93.025(12)
_cell_angle_gamma                100.752(11)
_cell_formula_units_Z            1
_cell_length_a                   12.778(12)
_cell_length_b                   12.983(14)
_cell_length_c                   14.022(14)
_cell_measurement_reflns_used    7692
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4441
_cell_measurement_theta_min      1.5457
_cell_volume                     2147(4)
_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 0.997
_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: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.3505
              2theta: -19.9355
scan:
    Number of images: 336
               Slice: -110.0000 - 58.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 45.3505
              2theta: -19.9355
scan:
    Number of images: 332
               Slice: -110.0000 - 56.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.3505
              2theta: -19.9355
scan:
    Number of images: 200
               Slice: -42.5000 - 57.5000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.3505
              2theta: -19.9355
;
_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      0.0030
_diffrn_orient_matrix_UB_12      -0.0234
_diffrn_orient_matrix_UB_13      -0.0767
_diffrn_orient_matrix_UB_21      0.0237
_diffrn_orient_matrix_UB_22      0.0697
_diffrn_orient_matrix_UB_23      -0.0391
_diffrn_orient_matrix_UB_31      0.0756
_diffrn_orient_matrix_UB_32      0.0011
_diffrn_orient_matrix_UB_33      -0.0070
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_Laue_measured_fraction_full 0.997
_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       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29359
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.385
_diffrn_reflns_theta_min         1.546
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.525
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         9623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.525
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0950
_refine_ls_shift/su_max          0.002
_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          0.2632
_refine_ls_wR_factor_ref         0.2738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8297
_reflns_number_total             9623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08166a2.cif
_cod_data_source_block           mx4011a
_cod_database_code               7118206
_shelxl_version_number           2013-4
_diffrn_number_total             9626
_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, All O(H,H) groups
2.a Free rotating group:
 O10(H10A,H10B)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), 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)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C13(H13), C16(H16), C21(H21), C24(H24),
 N1(H1), C35(H35), C36(H36), C38(H38), C39(H39), C41(H41), C42(H42), C44(H44),
 C45(H45)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              49597
_shelx_hkl_checksum              99429
_olex2_submission_special_instructions 'No special instructions were received'