Photoinduced Mechanical Motions of Pseudorotaxane Crystals Composed of Azobenzene and Ferrocenyl Groups on an Axle and a Crown Ether Ring
Cheng, Shao-Chi; Wang, Chi-Hsien; Lin, Yi-Chia; Tsuchido, Yoshitaka; Suzaki, Yuji; Sei, Yoshihisa; Kuo, Ting-Shen; Horie, Masaki; ACS Applied Materials & Interfaces  (2020) –; doi:10.1021/acsami.0c15171

data_4518158
_publ_section_title
;
 Photoinduced Mechanical Motions of Pseudorotaxane Crystals Composed of
 Azobenzene and Ferrocenyl Groups on an Axle and a Crown Ether Ring
;
_journal_name_full               'ACS Applied Materials &amp; Interfaces'
_journal_paper_doi               10.1021/acsami.0c15171
_journal_year                    2020
_chemical_formula_moiety
'C24 H28 Br4 O8, C24 H15 Fe N3, F6 P, C4 H10 O'
_chemical_formula_sum            'C52 H53 Br4 F6 Fe N3 O9 P'
_chemical_formula_weight         1384.43
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.478(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1045(3)
_cell_length_b                   11.8380(4)
_cell_length_c                   39.6515(16)
_cell_measurement_reflns_used    10157
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      73.0820
_cell_measurement_theta_min      3.5790
_cell_volume                     5676.5(3)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90
_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 0.957
_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  38.00   0.50   15.00    --  -41.80  19.00 -60.00  122
  2  \w    -23.00  36.00   0.50   15.00    --  -41.80  19.00-120.00  118
  3  \w    -36.00  43.00   0.50   15.00    --   41.80 -37.00 -90.00  158
  4  \w     11.00  61.00   0.50   15.00    --   41.80-115.00  38.00  100
  5  \w     35.00  62.00   0.50   41.62    --  106.13-115.00  38.00   54
  6  \w     80.00 105.00   0.50   41.62    --  106.13 -94.00  60.00   50
  7  \w     35.00  71.00   0.50   41.62    --  106.13 -94.00  60.00   72
  8  \w     40.00  73.00   0.50   41.62    --  106.13 -61.00  60.00   66
  9  \w     33.00  71.00   0.50   41.62    --  106.13 -61.00  30.00   76
 10  \w     34.00 112.00   0.50   41.62    --  106.13-125.00  30.00  156
 11  \w     80.00 121.00   0.50   15.00    --   41.80-165.00-108.00   82
 12  \w    101.00 133.00   0.50   41.62    --  106.13-165.00-108.00   64
 13  \w     33.00  72.00   0.50   41.62    --  106.13 -61.00-180.00   78
 14  \w     99.00 160.00   0.50   41.62    --  106.13  77.00  90.00  122
 15  \w    145.00 170.00   0.50   41.62    --  106.13 115.00 127.00   50
 16  \w     58.00 106.00   0.50   15.00    --   41.80 165.00 -85.00   96
 17  \w    -68.00 -38.00   0.50   41.62    -- -102.00 115.00 127.00   60
 18  \w   -102.00 -28.00   0.50   41.62    -- -102.00  77.00 150.00  148
 19  \w   -109.00 -84.00   0.50   41.62    -- -102.00 115.00 127.00   50
 20  \w    -67.00 -28.00   0.50   41.62    -- -102.00  61.00 -60.00   78
 21  \w    -63.00 -38.00   0.50   15.00    --  -41.80 165.00 -85.00   50
 22  \w   -103.00 -78.00   0.50   41.62    -- -102.00 -30.00-150.00   50
 23  \w   -149.00-105.00   0.50   41.62    -- -102.00 -94.00 -60.00   88
 24  \w    -93.00 -66.00   0.50   41.62    -- -102.00-165.00-108.00   54
 25  \w   -106.00 -81.00   0.50   15.00    --  -41.80-165.00-108.00   50
 26  \w   -133.00 -87.00   0.50   41.62    -- -102.00-115.00  38.00   92
 27  \w   -173.00 -84.00   0.50   41.62    -- -102.00 -94.00 -90.00  178
 28  \w   -166.00-129.00   0.50   41.62    -- -102.00 -30.00-150.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0061371000
_diffrn_orient_matrix_UB_12      0.0155807000
_diffrn_orient_matrix_UB_13      -0.0384718000
_diffrn_orient_matrix_UB_21      0.0197995000
_diffrn_orient_matrix_UB_22      0.1275201000
_diffrn_orient_matrix_UB_23      0.0051696000
_diffrn_orient_matrix_UB_31      0.1255879000
_diffrn_orient_matrix_UB_32      -0.0208514000
_diffrn_orient_matrix_UB_33      0.0027852000
_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  0.1003
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            39030
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.889
_diffrn_reflns_theta_min         3.655
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.344
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55656
_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_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       plate
_exptl_crystal_F_000             2772
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.250
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         11172
_refine_ls_number_restraints     918
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0926
_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^)+(0.1553P)^2^+16.0891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2691
_refine_ls_wR_factor_ref         0.2965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7132
_reflns_number_total             11172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c15171_si_007.cif
_cod_data_source_block           a17743_2
_cod_database_code               4518158
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.785
_reflns_odcompleteness_completeness 99.58
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 N67(H67A,H67B), C6(H6A,H6B), C44(H44A,H44B), C13(H13A,H13B), C46(H46A,H46B),
 C29(H29A,H29B), C12(H12A,H12B), C22(H22A,H22B), C7(H7A,H7B), C9(H9A,H9B),
 C23(H23A,H23B), C10(H10A,H10B), C28(H28A,H28B), C26(H26A,H26B), C73(H73A,H73B),
  C75(H75A,H75B), C25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C3(H3), C19(H19), C16(H16), C52(H52), C51(H51), C49(H49), C48(H48),
 C63(H63), C64(H64), C62(H62), C60(H60), C61(H61)
3.c Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C(HA,HB,HC)
;
_shelx_res_checksum              71621
_shelx_hkl_checksum              23891
_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 2.681
_oxdiff_exptl_absorpt_empirical_full_min 0.322