Guest-regulated chirality switching of planar chiral pseudo[1]catenanes.
Yang, Ya-Fen; Hu, Wei-Bo; Shi, Lei; Li, Sheng-Gang; Zhao, Xiao-Li; Liu, Yahu A.; Li, Jiu-Sheng; Jiang, Biao; Wen, Ke; Organic & biomolecular chemistry 16 (2018) 2028–2032; doi:10.1039/c8ob00156a

data_7156122
_publ_section_title
;
 Guest-regulated chirality switching of planar chiral pseudo[1]catenanes.
;
_journal_issue                   12
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2028
_journal_page_last               2032
_journal_paper_doi               10.1039/c8ob00156a
_journal_volume                  16
_journal_year                    2018
_chemical_formula_moiety         'C59 H64 N4 O12'
_chemical_formula_sum            'C59 H64 N4 O12'
_chemical_formula_weight         1021.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2018-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.54060(10)
_cell_length_b                   19.4516(2)
_cell_length_c                   23.9649(2)
_cell_measurement_reflns_used    44594
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.9740
_cell_measurement_theta_min      3.9430
_cell_volume                     5272.56(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -19.00  89.00   1.00    1.00    --    0.00  38.00 -60.00  108
  2  \w     10.00  36.00   1.00    1.00    --    0.00  57.00-150.00   26
  3  \w    -22.00  54.00   1.00    1.00    --    0.00  57.00 120.00   76
  4  \w    -19.00  24.00   1.00    1.00    --    0.00  38.00  60.00   43
  5  \w    -23.00  89.00   1.00    1.00    --    0.00  57.00 150.00  112
  6  \w    -23.00   2.00   1.00    1.00    --    0.00  57.00-150.00   25
  7  \w    -51.00  14.00   1.00    1.00    --    0.00 -77.00-180.00   65
  8  \w    -26.00   2.00   1.00    1.00    --    0.00  77.00-150.00   28
  9  \w     36.00  86.00   1.00    1.00    --    0.00  38.00-120.00   50
 10  \w     47.00  72.00   1.00    1.00    --    0.00  57.00-150.00   25
 11  \w    -18.00  83.00   1.00    1.00    --    0.00  38.00   0.00  101
 12  \w    -19.00  10.00   1.00    1.00    --    0.00  38.00-120.00   29
 13  \w     17.00  65.00   1.00    1.00    --    0.00  77.00-150.00   48
 14  \w     29.00  82.00   1.00    1.00    --    0.00  38.00  60.00   53
 15  \w     69.00 185.00   1.00    2.00    --   95.80  67.00-129.44  116
 16  \w     67.00 185.00   1.00    2.00    --   95.80  71.00 148.55  118
 17  \w     75.00 185.00   1.00    2.00    --   95.80  45.00 -39.73  110
 18  \w     75.00 185.00   1.00    2.00    --   95.80  51.00  80.53  110
 19  \w     67.00 185.00   1.00    2.00    --   95.80  71.00  -8.25  118
 20  \w     68.00  94.00   1.00    2.00    --   95.80  68.00  65.77   26
 21  \w    116.00 181.00   1.00    2.00    --   95.80  54.00 -69.79   65
 22  \w     65.00  90.00   1.00    2.00    --   95.80  76.00 115.14   25
 23  \w     67.00 113.00   1.00    2.00    --   95.80  71.00  21.81   46
 24  \w     64.00  89.00   1.00    2.00    --   95.80  80.00  15.26   25
 25  \w     63.00  88.00   1.00    2.00    --   95.80  81.00 165.81   25
 26  \w     63.00  89.00   1.00    2.00    --   95.80  82.00 -81.67   26
 27  \w    149.00 175.00   1.00    2.00    --   95.80  82.00 -81.67   26
 28  \w     64.00 103.00   1.00    2.00    --   95.80  79.00 -46.74   39
 29  \w    159.00 184.00   1.00    2.00    --   95.80  79.00 -46.74   25
 30  \w     44.00 128.00   1.00    2.00    --   95.80 -82.00-150.00   84
 31  \w     64.00 162.00   1.00    2.00    --   95.80  79.00-167.77   98
 32  \w    124.00 152.00   1.00    2.00    --   95.80  66.00 -18.98   28
 33  \w     63.00  88.00   1.00    2.00    --   95.80  82.00-141.97   25
 34  \w     67.00  92.00   1.00    2.00    --   95.80  73.00  11.99   25
 35  \w     69.00  95.00   1.00    2.00    --   95.80  66.00 -18.98   26
 36  \w     66.00 180.00   1.00    2.00    --   95.80  75.00-150.19  114
 37  \w     53.00 128.00   1.00    2.00    --   95.80 -82.00  90.00   75
 38  \w    141.00 185.00   1.00    2.00    --   95.80  71.00  47.62   44
 39  \w     63.00  88.00   1.00    2.00    --   95.80  82.00  90.00   25
 40  \w     63.00  88.00   1.00    2.00    --   95.80  82.00 150.00   25
 41  \w      6.00  83.00   1.00    2.00    --   95.80 -82.00-120.00   77
 42  \w     89.00 127.00   1.00    2.00    --   95.80 -82.00-120.00   38
 43  \w     65.00  90.00   1.00    2.00    --   95.80  77.00 -90.00   25
 44  \w     63.00  88.00   1.00    2.00    --   95.80  82.00 -60.00   25
 45  \w     63.00  88.00   1.00    2.00    --   95.80  82.00-120.00   25
 46  \w     63.00  89.00   1.00    2.00    --   95.80  82.00-180.00   26
 47  \w     65.00  90.00   1.00    2.00    --   95.80  77.00  60.00   25
 48  \w     65.00  90.00   1.00    2.00    --   95.80  77.00   0.00   25
 49  \w     77.00 128.00   1.00    2.00    --   95.80 -82.00 -60.00   51
 50  \w     37.00  69.00   1.00    2.00    --   95.80 -82.00 -60.00   32
 51  \w     65.00  91.00   1.00    2.00    --   95.80  77.00 150.00   26
 52  \w     65.00  90.00   1.00    2.00    --   95.80  77.00 -30.00   25
 53  \w     72.00 100.00   1.00    2.00    --   95.80  61.00 -90.00   28
 54  \w     63.00  89.00   1.00    2.00    --   95.80  82.00  60.00   26
 55  \w     67.00  92.00   1.00    2.00    --   95.80  71.00  47.62   25
 56  \w     71.00 181.00   1.00    2.00    --   95.80  61.00 120.00  110
 57  \w     65.00  90.00   1.00    2.00    --   95.80  77.00-120.00   25
 58  \w    127.00 185.00   1.00    2.00    --   95.80  77.00-120.00   58
 59  \w     65.00  91.00   1.00    2.00    --   95.80  77.00  30.00   26
 60  \w     63.00  89.00   1.00    2.00    --   95.80  82.00 -90.00   26
 61  \w     65.00  93.00   1.00    2.00    --   95.80  77.00 120.00   28
 62  \w     65.00  90.00   1.00    2.00    --   95.80  77.00-180.00   25
 63  \w    140.00 166.00   1.00    2.00    --   95.80  74.00  89.04   26
 64  \w     68.00 127.00   1.00    2.00    --   95.80 -82.00   0.00   59
 65  \w      7.00 119.00   1.00    2.00    --   95.80 -82.00-180.00  112
 66  \w     75.00 101.00   1.00    2.00    --   95.80  45.00 120.00   26
 67  \w     94.00 124.00   1.00    2.00    --   95.80 -82.00  30.00   30
 68  \w    152.00 183.00   1.00    2.00    --   95.80  80.00 127.42   31
 69  \w     53.00  79.00   1.00    2.00    --   95.80 -82.00  30.00   26
 70  \w     65.00  94.00   1.00    2.00    --   95.80  77.00 -60.00   29
 71  \w      8.00  34.00   1.00    2.00    --   95.80 -82.00  30.00   26
 72  \w     64.00 149.00   1.00    2.00    --   95.80  80.00 127.42   85
 73  \w     66.00  91.00   1.00    2.00    --   95.80  74.00  89.04   25
 74  \w     76.00 103.00   1.00    2.00    --   95.80  32.00 124.44   27
 75  \w     73.00  98.00   1.00    2.00    --   95.80  54.00 -69.79   25
 76  \w     74.00 177.00   1.00    2.00    --   95.80  49.00  58.97  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1351181000
_diffrn_orient_matrix_UB_12      0.0057281000
_diffrn_orient_matrix_UB_13      0.0195512000
_diffrn_orient_matrix_UB_21      -0.0157472000
_diffrn_orient_matrix_UB_22      0.0154113000
_diffrn_orient_matrix_UB_23      0.0611215000
_diffrn_orient_matrix_UB_31      0.0068529000
_diffrn_orient_matrix_UB_32      -0.0774630000
_diffrn_orient_matrix_UB_33      0.0135932000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            143580
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.482
_diffrn_reflns_theta_min         3.764
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.00062(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         10739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0610P)^2^+0.9970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9069
_reflns_number_total             10739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ob00156a2.cif
_cod_data_source_block           exp_16
_cod_depositor_comments
'Adding full bibliography for 7156117--7156122.cif.'
_cod_database_code               7156122
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.97
_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 Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C39(H39A,H39B), C41(H41A,H41B), C43(H43A,H43B), C49(H49A,
 H49B), C42(H42A,H42B), C50(H50A,H50B), C47(H47A,H47B), C48(H48A,H48B),
 C51(H51A,H51B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C17(H17), C12(H12), C2(H2), C14(H14), C21(H21), C28(H28), C36(H36),
 C5(H5), C25(H25), C24(H24), C37(H37), C32(H32), C33(H33)
2.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C), C59(H59A,H59B,H59C), C53(H53A,H53B,H53C), C57(H57A,H57B,H57C), C58(H58A,
 H58B,H58C)
;
_shelx_res_checksum              74587
_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 5.651
_oxdiff_exptl_absorpt_empirical_full_min 0.471