Helic[1]triptycene[3]arene: Synthesis, Complexation and Formation of [2]Rotaxane Shuttle.
Li, Jing; Han, Xiao-Ni; Zhou, He-Ye; Han, Ying; Chen, Chuan-Feng; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c01558

data_4038723
_publ_section_title
;
 Helic[1]triptycene[3]arene: Synthesis, Complexation and Formation of
 [2]Rotaxane Shuttle.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01558
_journal_year                    2020
_chemical_formula_moiety         'C4 H8 Br2, C50 H48 O8'
_chemical_formula_sum            'C54 H56 Br2 O8'
_chemical_formula_weight         992.80
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.5070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3525(2)
_cell_length_b                   25.8179(4)
_cell_length_c                   16.7371(2)
_cell_measurement_reflns_used    14071
_cell_measurement_temperature    169.99(13)
_cell_measurement_theta_max      74.8500
_cell_measurement_theta_min      3.4140
_cell_volume                     5769.61(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -24.00  65.00   0.50    1.34    --   47.20 -65.00  87.00  178
  2  \w     31.00 121.00   0.50    5.36    --  103.25 -65.00  87.00  180
  3  \w     91.00 169.00   0.50    5.36    --  103.25  45.00 -30.00  156
  4  \w     85.00 169.00   0.50    5.36    --  103.25  65.00-137.00  168
  5  \w     29.00 120.00   0.50    1.34    --   47.20  65.00-137.00  182
  6  \w     31.00 109.00   0.50    5.36    --  103.25 -94.00 -60.00  156
  7  \w    -65.00  26.00   0.50    1.34    --  -47.20  65.00-137.00  182
  8  \w   -117.00 -26.00   0.50    5.36    --  -99.00  65.00-137.00  182
  9  \w   -120.00 -84.00   0.50    1.34    --  -47.20 -77.00 120.00   72
 10  \w   -168.00 -81.00   0.50    5.36    --  -99.00 -65.00  87.00  174
 11  \w   -168.00 -85.00   0.50    5.36    --  -99.00 -15.00   0.00  166
 12  \w   -120.00 -71.00   0.50    1.34    --  -47.20-125.00-150.00   98
 13  \w   -120.00 -71.00   0.50    1.34    --  -47.20-125.00-180.00   98
 14  \w   -168.00 -82.00   0.50    5.36    --  -99.00 -61.00 -30.00  172
 15  \w   -168.00 -86.00   0.50    5.36    --  -99.00 -30.00 120.00  164
 16  \w   -168.00 -81.00   0.50    5.36    --  -99.00 -94.00  60.00  174
 17  \w   -168.00 -82.00   0.50    5.36    --  -99.00 -61.00 150.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0793385000
_diffrn_orient_matrix_UB_12      -0.0406980000
_diffrn_orient_matrix_UB_13      0.0223891000
_diffrn_orient_matrix_UB_21      -0.0674170000
_diffrn_orient_matrix_UB_22      0.0188526000
_diffrn_orient_matrix_UB_23      -0.0692831000
_diffrn_orient_matrix_UB_31      0.0498338000
_diffrn_orient_matrix_UB_32      -0.0393464000
_diffrn_orient_matrix_UB_33      -0.0562713000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27949
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.539
_diffrn_reflns_theta_min         3.424
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5766
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0676
_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^)+(0.1375P)^2^+2.5525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2183
_refine_ls_wR_factor_ref         0.2311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4454
_reflns_number_total             5766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01558_si_002.cif
_cod_data_source_block           tx1082b_sq
_cod_database_code               4038723
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOBrCl
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Br1-C26 = Br2-C29
 1.94 with sigma of 0.01
 C27-C26 = C28-C27 = C29-C28
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Br1 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim Br2: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(Br1) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(Br2) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Br1(0.5) Br2(0.5) C26(0.5) H26A(0.5) H26B(0.5) C27(0.5) H27A(0.5)
 H27B(0.5) C28(0.5) H28A(0.5) H28B(0.5) C29(0.5) H29A(0.5) H29B(0.5)
5.a Ternary CH refined with riding coordinates:
 C22(H22)
5.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C4(H4A,H4B),
 C14(H14A,H14B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C10(H10), C16(H16), C19(H19), C24(H24), C25(H25)
5.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              45240
_shelx_hkl_checksum              89558
_shelx_fab_checksum              9620
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.686
_oxdiff_exptl_absorpt_empirical_full_min 0.516