Chiroptical inversion of a planar chiral redox-switchable rotaxane
Gaedke, Marius; Witte, Felix; Anhäuser, Jana; Hupatz, Henrik; Schröder, Hendrik V.; Valkonen, Arto; Rissanen, Kari; Lützen, Arne; Paulus, Beate; Schalley, Christoph A.; Chemical Science  (2019) –; doi:10.1039/C9SC03694F

data_1552283
_publ_section_title
;
 Chiroptical inversion of a planar chiral redox-switchable rotaxane
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC03694F
_journal_year                    2019
_chemical_formula_moiety         'C30 H36 O6 S8 [+ solvent]'
_chemical_formula_sum            'C30 H36 O6 S8'
_chemical_formula_weight         749.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-04-17 deposited with the CCDC.    2019-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.649(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.1361(6)
_cell_length_b                   5.09490(10)
_cell_length_c                   30.6018(9)
_cell_measurement_reflns_used    15644
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.700
_cell_measurement_theta_min      0.407
_cell_volume                     3690.84(16)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker, 2008)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    SHELXL-2018/3
_computing_publication_material  SHELXL-2018/3
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD with APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1129
_diffrn_reflns_av_unetI/netI     0.1418
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            14025
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.823
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker, 2012)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       needle
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7554
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1606
_refine_ls_R_factor_gt           0.0734
_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^)+(0.0689P)^2^+4.0234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3856
_reflns_number_total             7554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03694f2.cif
_cod_data_source_block           dTTFC8
_cod_database_code               1552283
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              79206
_shelx_fab_checksum              47950