Thermodynamic and electrochemical study of tailor-made crown ethers for redox-switchable (pseudo)rotaxanes
Hupatz, Henrik; Gaedke, Marius; Schröder, Hendrik V; Beerhues, Julia; Valkonen, Arto; Klautzsch, Fabian; Müller, Sebastian; Witte, Felix; Rissanen, Kari; Sarkar, Biprajit; Schalley, Christoph A.; Beilstein Journal of Organic Chemistry 16 (2020) 2576–2588; doi:10.3762/bjoc.16.209

data_4038901
_publ_section_title
;
 Thermodynamic and electrochemical study of tailor-made crown ethers for
 redox-switchable (pseudo)rotaxanes
;
_journal_name_full               'Beilstein Journal of Organic Chemistry'
_journal_page_first              2576
_journal_page_last               2588
_journal_paper_doi               10.3762/bjoc.16.209
_journal_volume                  16
_journal_year                    2020
_chemical_formula_sum            'C44 H50 N4 O10'
_chemical_formula_weight         794.88
_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
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90.657(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6717(13)
_cell_length_b                   9.8821(10)
_cell_length_c                   28.639(3)
_cell_measurement_reflns_used    5843
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.405
_cell_measurement_theta_min      2.180
_cell_volume                     3869.0(7)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT+ (Bruker, 2009)'
_computing_molecular_graphics    'Diamond 3D, Version 4.0 (Brandenburg, 2014)'
_computing_publication_material  shelxle
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega + phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            134093
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.405
_diffrn_reflns_theta_min         2.180
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         7104
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0481P)^2^+4.0429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1254
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5843
_reflns_number_total             7104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NDIC7.cif
_cod_data_source_block           bip387_p21c_a
_cod_original_cell_volume        3869.1(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4038901
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              2649
_shelx_hkl_checksum              45609