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_4038720
_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, C4 H4 N2'
_chemical_formula_sum            'C61 H66 Cl2 N2 O9'
_chemical_formula_weight         1042.05
_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             2019-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.36730(10)
_cell_length_b                   25.6000(2)
_cell_length_c                   16.49370(10)
_cell_measurement_reflns_used    15066
_cell_measurement_temperature    170.00(11)
_cell_measurement_theta_max      75.1460
_cell_measurement_theta_min      3.4550
_cell_volume                     5644.00(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 0.984
_diffrn_measured_fraction_theta_max 0.942
_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   -120.00 -35.00   0.50    0.05    --  -47.20 -31.00-140.00  170
  2  \w    -15.00  57.00   0.50    0.05    --   47.20 -31.00-140.00  144
  3  \w     37.00  63.00   0.50    0.05    --   47.20  31.00  19.00   52
  4  \w     67.00 106.00   0.50    0.05    --   47.20  31.00  19.00   78
  5  \w   -134.00 -93.00   0.50    0.10    --  -99.00 -31.00-140.00   82
  6  \w    -93.00 -68.00   0.50    0.10    --  -99.00  31.00  19.00   50
  7  \w     30.00 115.00   0.50    0.10    --  103.25 -31.00-140.00  170
  8  \w     94.00 169.00   0.50    0.10    --  103.25  31.00  19.00  150
  9  \w    -41.00 -16.00   0.50    0.05    --  -47.20  31.00  19.00   50
 10  \w     18.00  93.00   0.50    0.05    --   47.20-125.00  90.00  150
 11  \w   -109.00 -24.00   0.50    0.10    --  -99.00  30.00-120.00  170
 12  \w    -65.00 -30.00   0.50    0.10    --  -99.00  61.00-150.00   70
 13  \w   -117.00 -56.00   0.50    0.10    --  -99.00 125.00  60.00  122
 14  \w   -168.00-106.00   0.50    0.10    --  -99.00 -30.00 -90.00  124
 15  \w     28.00  57.00   0.50    0.10    --  103.25 -30.00  30.00   58
 16  \w     31.00 114.00   0.50    0.10    --  103.25 -15.00  30.00  166
 17  \w     60.00  86.00   0.50    0.10    --  103.25 -30.00  30.00   52
 18  \w     73.00 105.00   0.50    0.10    --  103.25 -94.00   0.00   64
 19  \w     45.00  72.00   0.50    0.10    --  103.25 -94.00-180.00   54
;
_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      -0.0499485000
_diffrn_orient_matrix_UB_12      0.0120209000
_diffrn_orient_matrix_UB_13      0.0817810000
_diffrn_orient_matrix_UB_21      -0.1002305000
_diffrn_orient_matrix_UB_22      -0.0208402000
_diffrn_orient_matrix_UB_23      -0.0333826000
_diffrn_orient_matrix_UB_31      0.0271031000
_diffrn_orient_matrix_UB_32      -0.0551338000
_diffrn_orient_matrix_UB_33      0.0305628000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19641
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.350
_diffrn_reflns_theta_min         4.372
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74186
_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 light colourless'
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       plate
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0712P)^2^+2.9124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5027
_reflns_number_total             5518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01558_si_002.cif
_cod_data_source_block           tx857d_sq
_cod_database_code               4038720
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHON
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.807
_reflns_odcompleteness_completeness 99.45
_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.a Ternary CH refined with riding coordinates:
 C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B), C26(H26A,H26B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C7(H7), C10(H10), C13(H13), C16(H16), C21(H21)
2.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              34635
_shelx_hkl_checksum              8600
_shelx_fab_checksum              97656
_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 1.300
_oxdiff_exptl_absorpt_empirical_full_min 0.715