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_4038719
_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         'C25 H24 O4'
_chemical_formula_sum            'C26 H26 O5'
_chemical_formula_weight         418.47
_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             2019-05-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.186(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.7398(2)
_cell_length_b                   18.1447(2)
_cell_length_c                   16.4868(2)
_cell_measurement_reflns_used    11287
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      75.1110
_cell_measurement_theta_min      2.8120
_cell_volume                     4473.33(11)
_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(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.951
_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   -110.00 -85.00   0.50    0.05    --  -47.20-153.00-166.00   50
  2  \w    -74.00 -49.00   0.50    0.05    --  -47.20 121.00  75.00   50
  3  \w   -120.00 -95.00   0.50    0.05    --  -47.20-121.00  -7.00   50
  4  \w     28.00  93.00   0.50    0.05    --   47.20-121.00  -7.00  130
  5  \w     65.00  90.00   0.50    0.05    --   47.20 153.00-125.00   50
  6  \w     47.00  72.00   0.50    0.05    --   47.20-153.00-166.00   50
  7  \w   -105.00 -80.00   0.50    0.12    --  -99.00 153.00-125.00   50
  8  \w   -145.00-120.00   0.50    0.12    --  -99.00-121.00  -7.00   50
  9  \w     33.00 135.00   0.50    0.12    --  103.25-153.00-166.00  204
 10  \w     98.00 164.00   0.50    0.12    --  103.25 121.00  75.00  132
 11  \w     72.00 113.00   0.50    0.12    --  103.25-121.00  -7.00   82
 12  \w   -118.00 -71.00   0.50    0.05    --  -47.20-125.00  60.00   94
 13  \w     26.00 116.00   0.50    0.05    --   47.20  77.00  90.00  180
 14  \w     37.00 119.00   0.50    0.05    --   47.20  38.00-180.00  164
 15  \w   -114.00 -86.00   0.50    0.12    --  -99.00 -30.00-120.00   56
 16  \w   -110.00 -29.00   0.50    0.12    --  -99.00  45.00 -60.00  162
 17  \w   -162.00-136.00   0.50    0.12    --  -99.00 -30.00-120.00   52
 18  \w   -122.00 -28.00   0.50    0.12    --  -99.00  77.00  60.00  188
 19  \w    131.00 169.00   0.50    0.12    --  103.25  61.00  60.00   76
 20  \w     32.00 115.00   0.50    0.12    --  103.25 -45.00 -30.00  166
 21  \w     91.00 129.00   0.50    0.12    --  103.25  61.00  60.00   76
 22  \w     91.00 134.00   0.50    0.12    --  103.25  30.00-180.00   86
;
_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      -0.0577786000
_diffrn_orient_matrix_UB_12      -0.0700199000
_diffrn_orient_matrix_UB_13      -0.0246491000
_diffrn_orient_matrix_UB_21      0.0794922000
_diffrn_orient_matrix_UB_22      -0.0471155000
_diffrn_orient_matrix_UB_23      0.0527296000
_diffrn_orient_matrix_UB_31      -0.0309649000
_diffrn_orient_matrix_UB_32      0.0096015000
_diffrn_orient_matrix_UB_33      0.0792221000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17389
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.490
_diffrn_reflns_theta_min         3.831
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70346
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0667P)^2^+2.4764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3872
_reflns_number_total             4412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01558_si_002.cif
_cod_data_source_block           tx694_sq
_cod_original_cell_volume        4473.33(10)
_cod_database_code               4038719
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHO
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C10(H10), C14(H14), C17(H17), C20(H20)
2.d Idealised Me refined as rotating group:
 C4AA(H4AA,H4AB,H4AC), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              6228
_shelx_hkl_checksum              46009
_shelx_fab_checksum              6206
_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 1.734
_oxdiff_exptl_absorpt_empirical_full_min 0.642