Chelate Cooperativity and Spacer Length Effects on the Assembly Thermodynamics and Kinetics of Divalent Pseudorotaxanes
Wei Jiang; Karol Nowosinski; Nora L. Löw; Egor V. Dzyuba; Fabian Klautzsch; Andreas Schäfer; Juhani Huuskonen; Kari Rissanen; Christoph A. Schalley; Journal of the American Chemical Society 134 (2012) 1860–1868; doi:10.1021/ja2107096

data_4117345
_publ_contact_author_address
;Department of Chemistry
University of Jyvaskyla
P.O. Box 35
FIN-40014 Jyvaskyla, Finland
;
_publ_contact_author_email       juhani.s-p.huuskonen@jyu.fi
_publ_contact_author_fax         358(14)2602501
_publ_contact_author_name        'Rissanen, Kari'
_publ_contact_author_phone       358(50)5623721
_publ_section_title
;
 Chelate Cooperativity and Spacer Length Effects on the Assembly
 Thermodynamics and Kinetics of Divalent Pseudorotaxanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1860
_journal_page_last               1868
_journal_paper_doi               10.1021/ja2107096
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C95 H115 Cl3 F12 N8 O19 P2'
_chemical_formula_weight         2069.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-10-17T09:06:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.43(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.484(3)
_cell_length_b                   32.495(7)
_cell_length_c                   22.293(5)
_cell_measurement_reflns_used    22870
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      63.57
_cell_measurement_theta_min      5.63
_cell_volume                     10351(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      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_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      0.0332729
_diffrn_orient_matrix_UB_12      0.0116901
_diffrn_orient_matrix_UB_13      0.0391388
_diffrn_orient_matrix_UB_21      0.0600356
_diffrn_orient_matrix_UB_22      0
_diffrn_orient_matrix_UB_23      -0.0166595
_diffrn_orient_matrix_UB_31      -0.0136638
_diffrn_orient_matrix_UB_32      0.0284669
_diffrn_orient_matrix_UB_33      -0.0160726
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1503
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73922
_diffrn_reflns_theta_full        63.57
_diffrn_reflns_theta_max         63.57
_diffrn_reflns_theta_min         5.63
_exptl_absorpt_coefficient_mu    1.864
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS - Bruker/Siemens area detector absorption 
and other correction - V2.03
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       block
_exptl_crystal_F_000             4328
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.00041(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1319
_refine_ls_number_reflns         15565
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.1933
_refine_ls_R_factor_gt           0.1132
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3079
_refine_ls_wR_factor_ref         0.3648
_reflns_number_gt                7767
_reflns_number_total             15565
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja2107096_si_002.cif
_cod_data_source_block           kn148
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4117345