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_7005842
_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         'C66 H74 F12 Li4 N2 O26 S4, 2(C H Cl3)'
_chemical_formula_sum            'C68 H76 Cl6 F12 Li4 N2 O26 S4'
_chemical_formula_weight         1934.01
_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
_cell_angle_alpha                98.19(3)
_cell_angle_beta                 105.66(2)
_cell_angle_gamma                99.55(4)
_cell_formula_units_Z            1
_cell_length_a                   11.413(6)
_cell_length_b                   12.236(5)
_cell_length_c                   16.274(5)
_cell_measurement_reflns_used    19000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.60
_cell_volume                     2115.6(16)
_computing_cell_refinement       'SAINT (Bruker, 1994)'
_computing_data_collection       'SMART (Bruker, 1994)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL v.6.10 (Bruker, 2000)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS, Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6904
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14812
_diffrn_reflns_theta_full        24.26
_diffrn_reflns_theta_max         24.26
_diffrn_reflns_theta_min         1.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Correction applied by SADABS - note that the transmission factors are
not real since they include corrections for beam decay and possibly
crystal decay (the two cannot be distinguished).
The numbers listed in the CIF are those calculated by SHELXL.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.658
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         7350
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.1017
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1421P)^2^+7.6621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2691
_refine_ls_wR_factor_ref         0.2897
_reflns_number_gt                5584
_reflns_number_total             7350
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b706043b.txt
_cod_data_source_block           '[Li2.2.A](CF3SO3)2'
_cod_database_code               7005842