Solvent-resolved self-assemblies of cholesteryl-cyanostilbene conjugates with photo- and thermo-responsiveness.
Zhang, Shuqing; Hao, Aiyou; Xing, Pengyao; Nanoscale 15 (2023) 9567–9576; doi:10.1039/d3nr01056b

data_1569018
_publ_section_title
;
 Solvent-resolved self-assemblies of cholesteryl-cyanostilbene conjugates
 with photo- and thermo-responsiveness.
;
_journal_issue                   21
_journal_name_full               Nanoscale
_journal_page_first              9567
_journal_page_last               9576
_journal_paper_doi               10.1039/d3nr01056b
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'C42 H55 N3 O2'
_chemical_formula_sum            'C42 H55 N3 O2'
_chemical_formula_weight         633.88
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-12-13 deposited with the CCDC.	2023-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.170(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0358(4)
_cell_length_b                   6.2586(2)
_cell_length_c                   36.1603(12)
_cell_measurement_reflns_used    5572
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.0640
_cell_measurement_theta_min      4.8810
_cell_volume                     3626.51(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.963
_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     68.00 119.00   1.00    0.25    --   48.42-163.00  85.00   51
  2  \w     34.00 111.00   1.00    1.19    --  106.65-125.00 120.00   77
  3  \w     55.00 138.00   1.00    1.19    --  106.65-163.00  85.00   83
  4  \w     36.00  78.00   1.00    0.25    --   48.42-117.00-124.00   42
  5  \w     74.00 109.00   1.00    1.19    --  106.65-117.00-124.00   35
  6  \w     35.00  93.00   1.00    1.19    --  106.65 -77.00-120.00   58
  7  \w     39.00 104.00   1.00    1.19    --  106.65 -77.00 -90.00   65
  8  \w     94.00 120.00   1.00    1.19    --  106.65  38.00  60.00   26
  9  \w    128.00 178.00   1.00    1.19    --  106.65  38.00  60.00   50
 10  \w     92.00 178.00   1.00    1.19    --  106.65  57.00  30.00   86
 11  \w     27.00 121.00   1.00    0.25    --   48.42  77.00 150.00   94
 12  \w     71.00  96.00   1.00    0.25    --   48.42 163.00 112.00   25
 13  \w     88.00 113.00   1.00    1.19    --  106.65 163.00 112.00   25
 14  \w     95.00 178.00   1.00    1.19    --  106.65 125.00 150.00   83
 15  \w    100.00 178.00   1.00    1.19    --  106.65 125.00 -90.00   78
 16  \w    101.00 163.00   1.00    1.19    --  106.65 117.00 -37.00   62
 17  \w    -75.00 -50.00   1.00    1.19    --  -91.75 117.00 -37.00   25
 18  \w    -96.00 -70.00   1.00    1.19    --  -91.75 163.00 112.00   26
 19  \w    -96.00 -71.00   1.00    0.25    --  -48.42 163.00 112.00   25
 20  \w    -51.00  -9.00   1.00    0.25    --  -48.42 117.00 -37.00   42
 21  \w    -66.00 -19.00   1.00    1.19    --  -91.75  57.00 120.00   47
 22  \w    -44.00 -19.00   1.00    1.19    --  -91.75  77.00 150.00   25
 23  \w   -105.00 -48.00   1.00    1.19    --  -91.75  77.00 150.00   57
 24  \w    -65.00 -19.00   1.00    1.19    --  -91.75  57.00 -30.00   46
 25  \w    -44.00 -19.00   1.00    1.19    --  -91.75  57.00-120.00   25
 26  \w   -121.00 -27.00   1.00    0.25    --  -48.42 -77.00-120.00   94
 27  \w   -113.00 -78.00   1.00    1.19    --  -91.75-117.00-124.00   35
 28  \w   -154.00 -98.00   1.00    1.19    --  -91.75 -99.00   0.00   56
 29  \w   -126.00 -98.00   1.00    1.19    --  -91.75-163.00  85.00   28
 30  \w   -105.00 -48.00   1.00    0.25    --  -48.42-163.00  85.00   57
;
_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      -0.0069514000
_diffrn_orient_matrix_UB_12      -0.0379580000
_diffrn_orient_matrix_UB_13      -0.0420948000
_diffrn_orient_matrix_UB_21      -0.0151264000
_diffrn_orient_matrix_UB_22      0.2405412000
_diffrn_orient_matrix_UB_23      -0.0062912000
_diffrn_orient_matrix_UB_31      0.0946969000
_diffrn_orient_matrix_UB_32      0.0358605000
_diffrn_orient_matrix_UB_33      -0.0024571000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1079
_diffrn_reflns_av_unetI/netI     0.1216
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            39202
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.491
_diffrn_reflns_theta_min         2.446
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 2384 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         14098
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1603
_refine_ls_R_factor_gt           0.1032
_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^)+(0.1973P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2496
_refine_ls_wR_factor_ref         0.3157
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.879
_reflns_number_gt                7970
_reflns_number_total             14098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr01056b2.cif
_cod_data_source_block           20220916zsq_auto
_cod_depositor_comments
;
          Adding full bibliography for 1569018.cif.

2025-06-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C84 H110 N6 O4'
_cod_original_formula_weight         1267.77
_cod_original_formula_moiety         '2(C42 H55 N3 O2)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        3626.50(19)
_cod_database_code               1569018
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CNO
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.984
_reflns_odcompleteness_completeness 99.76
_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.a Ternary CH refined with riding coordinates:
 C2(H2), C49(H49), C48(H48), C17(H17), C54(H54), C7(H7), C1(H1), C64(H64),
 C14(H14), C61(H61), C65(H65), C18(H18), C69(H69), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C6(H6A,H6B), C8(H8A,H8B), C50(H50A,H50B), C55(H55A,H55B),
 C53(H53A,H53B), C56(H56A,H56B), C58(H58A,H58B), C9(H9A,H9B), C11(H11A,H11B),
 C63(H63A,H63B), C59(H59A,H59B), C12(H12A,H12B), C62(H62A,H62B), C16(H16A,H16B),
  C68(H68A,H68B), C15(H15A,H15B), C66(H66A,H66B), C21(H21A,H21B), C19(H19A,
 H19B), C20(H20A,H20B), C67(H67A,H67B)
2.c Aromatic/amide H refined with riding coordinates:
 N77(H77), N30(H30), C83(H83), C37(H37), C81(H81), C36(H36), C90(H90),
 C80(H80), C84(H84), C33(H33), C34(H34), C43(H43), C88(H88), C41(H41), C45(H45),
  C92(H92), C46(H46), C94(H94), C93(H93), C47(H47), C51(H51), C4(H4)
2.d Idealised Me refined as rotating group:
 C78(H78A,H78B,H78C), C31(H31A,H31B,H31C), C26(H26A,H26B,H26C), C73(H73A,H73B,
 H73C), C72(H72A,H72B,H72C), C25(H25A,H25B,H25C), C71(H71A,H71B,H71C), C70(H70A,
 H70B,H70C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              30551
_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 1.368
_oxdiff_exptl_absorpt_empirical_full_min 0.517