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_4038721
_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 H2 N2'
_chemical_formula_sum            'C54 H50 N2 O8'
_chemical_formula_weight         854.96
_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             2019-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 89.7135(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3833(2)
_cell_length_b                   25.6910(5)
_cell_length_c                   16.5120(3)
_cell_measurement_reflns_used    9474
_cell_measurement_temperature    170.00(14)
_cell_measurement_theta_max      74.7250
_cell_measurement_theta_min      3.4400
_cell_volume                     5677.26(17)
_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(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.948
_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    -23.00  59.00   0.50    1.24    --   47.20 -38.00 -60.00  164
  2  \w     31.00 127.00   0.50    4.98    --  103.25 -86.00-159.00  192
  3  \w     95.00 121.00   0.50    4.98    --  103.25  45.00 -90.00   52
  4  \w    124.00 150.00   0.50    4.98    --  103.25  86.00 -41.00   52
  5  \w     87.00 163.00   0.50    4.98    --  103.25  61.00  30.00  152
  6  \w     78.00 120.00   0.50    4.98    --  103.25 -61.00  60.00   84
  7  \w     31.00  82.00   0.50    4.98    --  103.25-125.00  60.00  102
  8  \w     32.00  69.00   0.50    4.98    --  103.25 -61.00  60.00   74
  9  \w     29.00 115.00   0.50    4.98    --  103.25 -30.00-150.00  172
 10  \w     -6.00  72.00   0.50    1.24    --   47.20 -86.00-159.00  156
 11  \w    -13.00  24.00   0.50    1.24    --  -47.20  86.00 -41.00   74
 12  \w    -58.00 -32.00   0.50    1.24    --  -47.20  86.00 -41.00   52
 13  \w    -65.00 -39.00   0.50    4.98    --  -99.00  86.00 -41.00   52
 14  \w   -162.00-132.00   0.50    4.98    --  -99.00 -86.00-159.00   60
 15  \w   -126.00 -83.00   0.50    4.98    --  -99.00 -86.00-159.00   86
 16  \w   -119.00 -83.00   0.50    4.98    --  -99.00-125.00 -90.00   72
 17  \w    -97.00 -72.00   0.50    1.24    --  -47.20-125.00   0.00   50
 18  \w   -119.00 -78.00   0.50    1.24    --  -47.20-125.00 -30.00   82
 19  \w   -147.00-121.00   0.50    4.98    --  -99.00-125.00 -90.00   52
 20  \w   -163.00 -86.00   0.50    4.98    --  -99.00 -45.00 -90.00  154
;
_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      0.0621774000
_diffrn_orient_matrix_UB_12      0.0097591000
_diffrn_orient_matrix_UB_13      0.0767389000
_diffrn_orient_matrix_UB_21      0.0353251000
_diffrn_orient_matrix_UB_22      0.0524968000
_diffrn_orient_matrix_UB_23      -0.0350422000
_diffrn_orient_matrix_UB_31      -0.0901469000
_diffrn_orient_matrix_UB_32      0.0273649000
_diffrn_orient_matrix_UB_33      0.0398124000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19302
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.530
_diffrn_reflns_theta_min         3.441
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75368
_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    1.000
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0976P)^2^+3.1422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4574
_reflns_number_total             5600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01558_si_002.cif
_cod_data_source_block           tx1739c_sq
_cod_original_cell_volume        5677.28(17)
_cod_database_code               4038721
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHON
_reflns_odcompleteness_completeness 99.79
_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:
 C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C7(H7), C10(H10), C14(H14), C17(H17), C23(H23), C27(H27)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C25(H25A,H25B,
 H25C)
;
_shelx_res_checksum              12903
_shelx_hkl_checksum              64662
_shelx_fab_checksum              71112
_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 3.180
_oxdiff_exptl_absorpt_empirical_full_min 0.509