Processive Rotaxane Systems. Studies on the Mechanism and Control of the Threading Process
Pilar Hidalgo Ramos; Ruud G. E. Coumans; Alexander B. C. Deutman; Jan M. M. Smits; Rene de Gelder; Johannes A. A. W. Elemans; Roeland J. M. Nolte; Alan E. Rowan; Journal of the American Chemical Society 129 (2007) 5699–5702; doi:10.1021/ja068714i

data_4109346
_publ_contact_author
;
        Prof.dr. R.J.M. Nolte
        Institute for Molecules and Materials
        Radboud University Nijmegen
        Toernooiveld 1
        6525 ED  Nijmegen
        The Netherlands
;
_publ_contact_author_email       r.nolte@science.ru.nl
_publ_contact_author_fax         '031 024 3553393'
_publ_contact_author_phone       '031 024 3652143'
_publ_section_title
;
 Processive Rotaxane Systems. Studies on the Mechanism and Control of the
 Threading Process
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5699
_journal_page_last               5702
_journal_paper_doi               10.1021/ja068714i
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C173 H135 Cl3 N18 O20'
_chemical_formula_weight         2892.34
_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             2006-07-27
_audit_creation_method           'SHELXL, adapted and expanded'
_cell_angle_alpha                90.00
_cell_angle_beta                 105.160(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.5934(11)
_cell_length_b                   32.0613(18)
_cell_length_c                   16.2353(13)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      22.500
_cell_measurement_theta_min      2.050
_cell_volume                     7834.3(10)
_computing_data_collection
;
Nonius "Collect" program suite (Nonius, 1999)
;
_computing_data_reduction
;
Nonius "EvalCCD" program suite (Duisenberg, 1998)
;
_computing_molecular_graphics
;
PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
CRUNCH (de Gelder et al., 1993),
;
_diffrn_ambient_temperature      208(2)
_diffrn_detector_area_resol_mean 18.4
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       'area detector \f and \w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1733
_diffrn_reflns_av_sigmaI/netI    0.1576
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            80914
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0.000
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS multiscan (Sheldrick, 1996)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       'rather regular thin needle'
_exptl_crystal_F_000             3020
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.109
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         10212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.2060
_refine_ls_R_factor_gt           0.1286
_refine_ls_R_factor_obs          0.1286
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_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^)+(0.1016P)^2^+34.9055P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2939
_refine_ls_wR_factor_gt          0.2577
_refine_ls_wR_factor_obs         0.2577
_refine_ls_wR_factor_ref         0.2939
_reflns_number_gt                6011
_reflns_number_observed          6011
_reflns_number_total             10212
_reflns_observed_criterion       >2sigma(I)
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja068714isi20070308_083825.cif
_cod_data_source_block           PILI01
_cod_original_cell_volume        7834.3(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4109346