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_4518155
_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         'C25 H26 Fe N3, C24 H32 O8, 0.5(H2 O), F6 P'
_chemical_formula_sum            'C49 H59 F6 Fe N3 O8.5 P'
_chemical_formula_weight         1026.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-12-09
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                78.972(3)
_cell_angle_beta                 78.823(3)
_cell_angle_gamma                87.279(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1238(10)
_cell_length_b                   11.4618(12)
_cell_length_c                   21.607(2)
_cell_measurement_reflns_used    7372
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      2.41
_cell_volume                     2414.1(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      199.99
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       multi-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_av_unetI/netI     0.1011
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35751
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.212
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       prism
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         8460
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0733
_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^)+(0.0159P)^2^+4.6823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5025
_reflns_number_total             8460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c15171_si_004.cif
_cod_data_source_block           d18553
_cod_original_formula_sum        'C49 H59 F6 Fe N3 O8.50 P'
_cod_database_code               4518155
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.749
_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, All Fe(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
3. Rigid body (RIGU) restrains
 C16, N2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N3, C19
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Others
 Sof(N2A)=Sof(N3A)=1-FVAR(1)
 Sof(N2)=Sof(N3)=FVAR(1)
 Fixed Sof: O9(0.5) H9A(0.5) H9B(0.5)
5.a Riding coordinates:
 Fe1(H9A,H9B)
5.b Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9)
5.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,
 H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
  N1(H1A,H1B)
5.d Me refined with riding coordinates:
 C25(H25A,H25B,H25C)
5.e Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23),
 C24(H24), C33(H33), C34(H34), C35(H35), C36(H36), C45(H45), C46(H46), C47(H47),
  C48(H48)
;
_olex2_submission_special_instructions 'No special instructions were received'