Substituent effects on axle binding in amide pseudorotaxanes: comparison of NMR titration and ITC data with DFT calculations.
Kaufmann, Lena; Dzyuba, Egor V.; Malberg, Friedrich; Löw, Nora L; Groschke, Matthias; Brusilowskij, Boris; Huuskonen, Juhani; Rissanen, Kari; Kirchner, Barbara; Schalley, Christoph A.; Organic & biomolecular chemistry 10 (2012) 5954–5964; doi:10.1039/c2ob25196e

data_7152467
_publ_section_title
;
 Substituent effects on axle binding in amide pseudorotaxanes: comparison
 of NMR titration and ITC data with DFT calculations.
;
_journal_issue                   30
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5954
_journal_page_last               5964
_journal_paper_doi               10.1039/c2ob25196e
_journal_volume                  10
_journal_year                    2012
_chemical_formula_moiety         'C68 H80 N4 O4, C10 H16 N2 O2, 4(C H Cl3)'
_chemical_formula_sum            'C82 H100 Cl12 N6 O6'
_chemical_formula_weight         1691.08
_chemical_name_common            'Compound X'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-11-02T13:20:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                103.23(2)
_cell_angle_beta                 107.21(3)
_cell_angle_gamma                108.81(2)
_cell_formula_units_Z            1
_cell_length_a                   13.087(3)
_cell_length_b                   13.192(2)
_cell_length_c                   14.620(3)
_cell_measurement_reflns_used    6843
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      63.31
_cell_measurement_theta_min      5.8
_cell_volume                     2130.5(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0143722
_diffrn_orient_matrix_UB_12      -0.0420361
_diffrn_orient_matrix_UB_13      0.0478804
_diffrn_orient_matrix_UB_21      0.0851353
_diffrn_orient_matrix_UB_22      0.0301667
_diffrn_orient_matrix_UB_23      0.011579
_diffrn_orient_matrix_UB_31      0.0176486
_diffrn_orient_matrix_UB_32      0.0684226
_diffrn_orient_matrix_UB_33      0.0587955
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1111
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9544
_diffrn_reflns_theta_full        63.31
_diffrn_reflns_theta_max         63.31
_diffrn_reflns_theta_min         5.8
_exptl_absorpt_coefficient_mu    3.998
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         6843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1038P)^2^+3.5602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1974
_refine_ls_wR_factor_ref         0.216
_reflns_number_gt                5265
_reflns_number_total             6843
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2ob25196e.txt
_cod_data_source_block           2@1b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7152467