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_4038722
_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         'C50 H48 O8, C6 H8 N2'
_chemical_formula_sum            'C56 H56 N2 O8'
_chemical_formula_weight         885.02
_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             2019-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.45320(10)
_cell_length_b                   25.5222(2)
_cell_length_c                   16.78170(10)
_cell_measurement_reflns_used    13694
_cell_measurement_temperature    170.00(11)
_cell_measurement_theta_max      75.0510
_cell_measurement_theta_min      3.4560
_cell_volume                     5762.08(7)
_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      170.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_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    -55.00  24.00   0.50    0.10    --  -47.20  50.00  -4.00  158
  2  \w   -120.00 -35.00   0.50    0.10    --  -47.20 -50.00-150.00  170
  3  \w     45.00  78.00   0.50    0.10    --   47.20  50.00  -4.00   66
  4  \w    -16.00  34.00   0.50    0.10    --   47.20 -50.00-150.00  100
  5  \w    -69.00 -44.00   0.50    0.50    --  -99.00  50.00  -4.00   50
  6  \w   -165.00 -85.00   0.50    0.50    --  -99.00 -50.00-150.00  160
  7  \w     93.00 118.00   0.50    0.50    --  103.25  50.00  -4.00   50
  8  \w     31.00 116.00   0.50    0.50    --  103.25 -50.00-150.00  170
  9  \w   -117.00 -89.00   0.50    0.10    --  -47.20-125.00 -30.00   56
 10  \w   -119.00 -73.00   0.50    0.10    --  -47.20-125.00   0.00   92
 11  \w   -113.00 -24.00   0.50    0.50    --  -99.00  15.00-180.00  178
 12  \w   -110.00 -46.00   0.50    0.50    --  -99.00  45.00 120.00  128
 13  \w   -111.00 -65.00   0.50    0.50    --  -99.00  30.00   0.00   92
 14  \w   -166.00-117.00   0.50    0.50    --  -99.00-125.00   0.00   98
 15  \w    -97.00 -71.00   0.50    0.50    --  -99.00-125.00   0.00   52
 16  \w    129.00 154.00   0.50    0.50    --  103.25  45.00-150.00   50
 17  \w     34.00  92.00   0.50    0.50    --  103.25 -94.00  30.00  116
 18  \w     41.00 103.00   0.50    0.50    --  103.25 -30.00   0.00  124
;
_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      -0.1129878000
_diffrn_orient_matrix_UB_12      0.0078155000
_diffrn_orient_matrix_UB_13      -0.0087308000
_diffrn_orient_matrix_UB_21      -0.0001582000
_diffrn_orient_matrix_UB_22      -0.0362260000
_diffrn_orient_matrix_UB_23      -0.0733973000
_diffrn_orient_matrix_UB_31      -0.0184580000
_diffrn_orient_matrix_UB_32      -0.0476886000
_diffrn_orient_matrix_UB_33      0.0543922000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19657
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.215
_diffrn_reflns_theta_min         3.463
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72316
_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            'pale colourless'
_exptl_crystal_density_diffrn    1.020
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5669
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0817P)^2^+7.4168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5099
_reflns_number_total             5669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01558_si_002.cif
_cod_data_source_block           tx1739_sq
_cod_database_code               4038722
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHON
_reflns_odcompleteness_completeness 99.85
_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. Restrained distances
 C28-C27 = C28-C28_$1 = C28_$1-C27_$1
 1.54 with sigma of 0.01
 C26-C27 = C26_$1-C27_$1
 1.46 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C18(H18)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C11(H11A,H11B), C27(H27A,H27B), C28(H28A,H28B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C9(H9), C13(H13), C16(H16), C20(H20), C21(H21)
3.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C)
;
_shelx_res_checksum              98742
_shelx_hkl_checksum              48419
_shelx_fab_checksum              36908
_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 1.393
_oxdiff_exptl_absorpt_empirical_full_min 0.655