Structures and solution dynamics of pseudorotaxanes mediated by alkali-metal cations.
Pascu, Sofia I.; Naumann, Christoph; Kaiser, Guido; Bond, Andrew D.; Sanders, Jeremy K. M.; Jarrosson, Thibaut; Dalton transactions (Cambridge, England : 2003)  (2007) 3874–3884; doi:10.1039/b706043b

data_7005840
_publ_section_title
;
 Structures and solution dynamics of pseudorotaxanes mediated by
 alkali-metal cations.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3874
_journal_page_last               3884
_journal_paper_doi               10.1039/b706043b
_journal_year                    2007
_chemical_formula_moiety         'C62 H78 I2 N2 Na2 O16, 2(C H Cl3)'
_chemical_formula_sum            'C64 H80 Cl6 I2 N2 Na2 O16'
_chemical_formula_weight         1645.78
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.281(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7604(5)
_cell_length_b                   23.6245(6)
_cell_length_c                   15.4728(6)
_cell_measurement_reflns_used    20952
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     3755.8(2)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction        Denzo/Scalepack
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL v6.10 (Bruker, 2000)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'thin-slice /w and /f scans'
_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  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21958
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.72
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6586
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+12.7893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                4404
_reflns_number_total             6586
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b706043b.txt
_cod_data_source_block           '[Na2.1.A]I2'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7005840