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_7152468
_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, C18 H20 N2 O2, 2(C H Cl3)'
_chemical_formula_sum            'C88 H102 Cl6 N6 O6'
_chemical_formula_weight         1552.46
_chemical_name_common            'Compound X'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-11-03T08:35:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 126.21(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.976(5)
_cell_length_b                   19.610(4)
_cell_length_c                   19.930(4)
_cell_measurement_reflns_used    20775
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.94
_cell_volume                     8191(4)
_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      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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      0.004048
_diffrn_orient_matrix_UB_12      -0.0577389
_diffrn_orient_matrix_UB_13      0.0072101
_diffrn_orient_matrix_UB_21      -0.0633976
_diffrn_orient_matrix_UB_22      -0.0170981
_diffrn_orient_matrix_UB_23      0.0008935
_diffrn_orient_matrix_UB_31      -0.034676
_diffrn_orient_matrix_UB_32      -0.0353644
_diffrn_orient_matrix_UB_33      -0.0617634
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1122
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54437
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3.94
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         7156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0695
_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^)+(0.0674P)^2^+16.6562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1742
_reflns_number_gt                4611
_reflns_number_total             7156
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2ob25196e.txt
_cod_data_source_block           8@1b
_cod_original_cell_volume        8191(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7152468