Photoregulated "Breathing" Vesicle with Inversed Supramolecular Chirality.
Cheng, Qiuhong; Duan, Hongdong; Hao, Aiyou; Xing, Pengyao; ACS applied materials & interfaces  (2020) –; doi:10.1021/acsami.0c20211

data_4518389
_publ_section_title
;
 Photoregulated &quot;Breathing&quot; Vesicle with Inversed Supramolecular
 Chirality.
;
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_paper_doi               10.1021/acsami.0c20211
_journal_year                    2020
_chemical_formula_moiety         'C44 H64 N4 O3'
_chemical_formula_sum            'C44 H64 N4 O3'
_chemical_formula_weight         696.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.129(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3703(4)
_cell_length_b                   8.78618(17)
_cell_length_c                   27.0121(5)
_cell_measurement_reflns_used    16139
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.7070
_cell_measurement_theta_min      2.5760
_cell_volume                     4166.49(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.962
_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    -53.00  24.00   1.00    0.25    --  -48.45  56.00 -40.00   77
  2  \w    -43.00 -13.00   1.00    5.00    --  -86.25  38.00-180.00   30
  3  \w    -64.00 -18.00   1.00    5.00    --  -86.25  56.00 -40.00   46
  4  \w    -43.00 -13.00   1.00    5.00    --  -86.25  38.00 120.00   30
  5  \w    -99.00 -73.00   1.00    5.00    --  -86.25 -56.00 177.00   26
  6  \w   -103.00 -63.00   1.00    5.00    --  -86.25 -77.00  90.00   40
  7  \w   -119.00 -43.00   1.00    0.25    --  -48.45 -56.00 177.00   76
  8  \w    -16.00  38.00   1.00    0.25    --   48.45 -56.00 177.00   54
  9  \w     34.00  64.00   1.00    5.00    --  106.49 -56.00 177.00   30
 10  \w     34.00  62.00   1.00    5.00    --  106.49 -57.00 150.00   28
 11  \w     34.00 105.00   1.00    5.00    --  106.49 -77.00 150.00   71
 12  \w     34.00  66.00   1.00    5.00    --  106.49 -57.00   0.00   32
 13  \w     41.00  66.00   1.00    5.00    --  106.49 -57.00 -60.00   25
 14  \w     35.00 105.00   1.00    5.00    --  106.49 -77.00 -90.00   70
 15  \w     38.00 111.00   1.00    5.00    --  106.49-125.00 -90.00   73
 16  \w     34.00 105.00   1.00    5.00    --  106.49 -77.00  60.00   71
 17  \w     34.00  65.00   1.00    5.00    --  106.49 -57.00 -30.00   31
 18  \w     98.00 178.00   1.00    5.00    --  106.49  19.00-120.00   80
 19  \w     92.00 169.00   1.00    5.00    --  106.49  56.00 -40.00   77
 20  \w     93.00 169.00   1.00    5.00    --  106.49  57.00   0.00   76
 21  \w     92.00 176.00   1.00    5.00    --  106.49  57.00  60.00   84
 22  \w     92.00 176.00   1.00    5.00    --  106.49  57.00  30.00   84
 23  \w     48.00  75.00   1.00    0.25    --   48.45  56.00 -40.00   27
 24  \w     34.00  99.00   1.00    0.25    --   48.45  57.00  60.00   65
 25  \w   -109.00 -75.00   1.00    0.25    --  -48.45-125.00 -30.00   34
 26  \w   -145.00-119.00   1.00    5.00    --  -86.25 -77.00  90.00   26
 27  \w   -118.00 -63.00   1.00    5.00    --  -86.25 -77.00 120.00   55
 28  \w   -153.00 -73.00   1.00    5.00    --  -86.25 -57.00 150.00   80
 29  \w   -159.00-133.00   1.00    5.00    --  -86.25 -77.00 120.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0657750000
_diffrn_orient_matrix_UB_12      0.0431373000
_diffrn_orient_matrix_UB_13      0.0218670000
_diffrn_orient_matrix_UB_21      0.0533150000
_diffrn_orient_matrix_UB_22      0.1094512000
_diffrn_orient_matrix_UB_23      0.0387139000
_diffrn_orient_matrix_UB_31      -0.0230256000
_diffrn_orient_matrix_UB_32      0.1301097000
_diffrn_orient_matrix_UB_33      -0.0397812000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            44557
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.859
_diffrn_reflns_theta_min         2.594
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_F_000             1520
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 3959 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.09(10)
_refine_ls_extinction_coef       0.00015(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         16231
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0896
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1717P)^2^+0.9401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2769
_refine_ls_wR_factor_ref         0.2985
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.881
_reflns_number_gt                11927
_reflns_number_total             16231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c20211_si_001.cif
_cod_data_source_block           200523a
_cod_original_cell_volume        4166.51(15)
_cod_database_code               4518389
_shelx_shelxl_version_number     2014/7
_diffrn_oxdiff_digest_frames
;
017b6ff1e3ff1c302dbdf50b01aab7894601524471a
;
_diffrn_oxdiff_digest_hkl
;
0155a0a604b91b3458c6c458c28d2f353f93a8
;
_reflns_odcompleteness_completeness 99.84
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N51-C67 = N38-C23
 2.35 with sigma of 0.02
 N51-C23 = N38-C67
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C23 \\sim C38 \\sim C4AA \\sim C9CA \\sim C75 \\sim C15 \\sim N51 \\sim N38:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a Ternary CH refined with riding coordinates:
 C8BA(H8BA), C5CA(H5CA), C9BA(H9BA), C8AA(H8AA), C9AA(H9AA), C7CA(H7CA),
 C3CA(H3CA), C2(H2), C5(H5), C45(H45), C12(H12), C20(H20), C44(H44), C64(H64)
4.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C31(H31A,H31B), C58(H58A,H58B), C59(H59A,H59B), C61(H61A,
 H61B), C77(H77A,H77B), C6(H6A,H6B), C11(H11A,H11B), C0AA(H0AA,H0AB), C16(H16A,
 H16B), C7(H7A,H7B), C9(H9A,H9B), C37(H37A,H37B), C48(H48A,H48B), C7AA(H7AA,
 H7AB), C14(H14A,H14B), C19(H19A,H19B), C5BA(H5BA,H5BB), C26(H26A,H26B),
 C28(H28A,H28B), C33(H33A,H33B), C35(H35A,H35B), C0DA(H0DA,H0DB), C65(H65A,
 H65B), C69(H69A,H69B), C2DA(H2DA,H2DB)
4.c Aromatic/amide H refined with riding coordinates:
 N16(H16), N22(H22), C32(H32), C52(H52), C1DA(H1DA), C75(H75), C4(H4),
 C1BA(H1BA), C22(H22A), C41(H41), C10(H10), C13(H13), C15(H15), C17(H17),
 C18(H18), C4AA(H4AA), C38(H38), C7BA(H7BA), C3(H3), C66(H66)
4.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C2CA(H2CA,H2CB,H2CC), C(HA,HB,HC), C8(H8A,H8B,H8C),
 C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AB,H3AC), C5AA(H5AA,H5AB,H5AC), C43(H43A,
 H43B,H43C), C1CA(H1CA,H1CB,H1CC), C56(H56A,H56B,H56C), C6AA(H6AA,H6AB,H6AC),
 C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C8CA(H8CA,H8CB,H8CC)
;
_shelx_res_checksum              41089
_shelx_hkl_checksum              67683
_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 1.798
_oxdiff_exptl_absorpt_empirical_full_min 0.541