Ring-through-ring molecular shuttling in a saturated [3]rotaxane
Kelong Zhu; Giorgio Baggi; Stephen J. Loeb; Nature Chemistry 10 (2018) 625–630; doi:10.1038/s41557-018-0040-9

data_1551887
_publ_section_title
;
 Ring-through-ring molecular shuttling in a saturated [3]rotaxane
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              625
_journal_page_last               630
_journal_paper_doi               10.1038/s41557-018-0040-9
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         'C50 H30 Br4 N4, C16 H32 O8, 1.5(C4 H8 O2)'
_chemical_formula_sum            'C72 H74 Br4 N4 O11'
_chemical_formula_weight         1490.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 126.4052(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.466(2)
_cell_length_b                   18.3593(12)
_cell_length_c                   29.875(2)
_cell_measurement_reflns_used    3870
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      58.52
_cell_measurement_theta_min      14.85
_cell_volume                     13890.4(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      170.0
_diffrn_measured_fraction_theta_full 0.774
_diffrn_measured_fraction_theta_max 0.774
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1206
_diffrn_reflns_av_unetI/netI     0.1822
_diffrn_reflns_Laue_measured_fraction_full 0.774
_diffrn_reflns_Laue_measured_fraction_max 0.774
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13500
_diffrn_reflns_point_group_measured_fraction_full 0.774
_diffrn_reflns_point_group_measured_fraction_max 0.774
_diffrn_reflns_theta_full        58.861
_diffrn_reflns_theta_max         58.861
_diffrn_reflns_theta_min         14.848
_exptl_absorpt_coefficient_mu    3.326
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.0996 before and 0.0587 after correction. 
The Ratio of minimum to maximum transmission is 0.8288. 
The \l/2 correction factor is 0.00150.'
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       plates
_exptl_crystal_F_000             6096
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.471
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         7718
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.2035
_refine_ls_R_factor_gt           0.1067
_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^)+(0.1296P)^2^+78.1473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2366
_refine_ls_wR_factor_ref         0.2919
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3819
_reflns_number_total             7718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            41557_2018_40_MOESM31_ESM.cif
_cod_data_source_block           kz036b
_cod_original_cell_volume        13890.3(17)
_cod_database_code               1551887
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.689
_shelx_res_checksum              9630
_shelx_hkl_checksum              49126