Complexation between a triptycene-derived oxacalixarene and π-extended viologens: linker-length-dependent orientation of the macrocycles in pseudo[3]rotaxanes.
Wang, Han-Xiao; Hu, Shu-Zhen; Shi, Qiang; Chen, Chuan-Feng; Organic & biomolecular chemistry 14 (2016) 10481–10488; doi:10.1039/c6ob02093c

data_7155317
_publ_section_title
;
 Complexation between a triptycene-derived oxacalixarene and \p-extended
 viologens: linker-length-dependent orientation of the macrocycles in
 pseudo[3]rotaxanes.
;
_journal_issue                   44
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              10481
_journal_page_last               10488
_journal_paper_doi               10.1039/c6ob02093c
_journal_volume                  14
_journal_year                    2016
_chemical_formula_moiety         '2(C56 H32 N4 O4), C16 H18 N2, 2(F6 P)'
_chemical_formula_sum            'C128 H82 F12 N10 O8 P2'
_chemical_formula_weight         2177.97
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_audit_update_record
;
2016-03-30 deposited with the CCDC.
2016-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   31.334(4)
_cell_length_b                   31.334(4)
_cell_length_c                   27.064(4)
_cell_measurement_reflns_used    20476
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4838
_cell_measurement_theta_min      1.0626
_cell_volume                     23012(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  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2013)'
_computing_structure_solution
;
'SHELXS (Sheldrick, 2013)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 18.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.2441
              2theta: -20.0586
scan:
    Number of images: 240
               Slice: -80.0000 - 40.0000
         Image width: 0.5000
            Exp time: 18.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 45.2441
              2theta: -20.0586
;
_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      -0.0303
_diffrn_orient_matrix_UB_12      0.0185
_diffrn_orient_matrix_UB_13      -0.0099
_diffrn_orient_matrix_UB_21      -0.0206
_diffrn_orient_matrix_UB_22      -0.0122
_diffrn_orient_matrix_UB_23      -0.0280
_diffrn_orient_matrix_UB_31      -0.0200
_diffrn_orient_matrix_UB_32      -0.0202
_diffrn_orient_matrix_UB_33      0.0236
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            52994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         1.682
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8323
_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    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             10098
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.731
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         11715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.731
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.1049
_refine_ls_shift/su_max          0.001
_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          0.2751
_refine_ls_wR_factor_ref         0.2806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10510
_reflns_number_total             11715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ob02093c2.cif
_cod_data_source_block           mx3498
_cod_depositor_comments
'Adding full bibliography for 7155316--7155317.cif.'
_cod_original_cell_volume        23012(7)
_cod_database_code               7155317
_diffrn_number_total             11722
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C15(H15), C22(H22), C43(H43), C50(H50)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C10(H10), C13(H13), C14(H14), C17(H17),
 C18(H18), C19(H19), C20(H20), C24(H24), C25(H25), C27(H27), C30(H30), C31(H31),
  C33(H33), C34(H34), C38(H38), C41(H41), C42(H42), C45(H45), C46(H46),
 C47(H47), C48(H48), C52(H52), C54(H54), C55(H55), C58(H58), C59(H59), C61(H61),
  C62(H62), C63(H63), C64(H64)
2.c Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C)
;
_shelx_res_checksum              84067
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'