pH-Gated photoresponsive shuttling in a water-soluble pseudorotaxane.
Zubillaga, A.; Ferreira, P.; Parola, A. J.; Gago, S.; Basílio, N; Chemical communications (Cambridge, England) 54 (2018) 2743–2746; doi:10.1039/c8cc00688a

data_7121296
_publ_section_title
;
 pH-Gated photoresponsive shuttling in a water-soluble pseudorotaxane.
;
_journal_issue                   22
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2743
_journal_page_last               2746
_journal_paper_doi               10.1039/c8cc00688a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C24 H32 N O3, Br'
_chemical_formula_sum            'C24 H32 Br N O3'
_chemical_formula_weight         462.41
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-02-14 deposited with the CCDC.
2018-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.315(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.980(3)
_cell_length_b                   10.7749(16)
_cell_length_c                   11.4258(18)
_cell_measurement_reflns_used    2664
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.17
_cell_measurement_theta_min      2.85
_cell_volume                     2332.8(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2595
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            41450
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.083
_diffrn_reflns_theta_max         25.083
_diffrn_reflns_theta_min         2.174
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.786
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       Plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
The final refinement showed a disordered co-crystallized H2O molecule and therefore, the SQUEEZE utility in PLATON was used to remove its contribution to the overall intensity data. The electron density modelled by SQUEEZE is consistent with around 2.8 water molecules per unit cell (ca. 28 electrons for a volume of ca. 102 \%A3), corresponding to about 0.7 water molecules per molecule of C24H32NO3Br.
;
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0536P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2075
_reflns_number_total             4118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00688a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7121296.cif.'
_cod_database_code               7121296
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.616
_shelx_estimated_absorpt_t_max   0.948
_shelx_res_checksum              74794
_shelx_fab_checksum              79933