Crystal Structure od mono[3-(2-imidazolylthio)]-altro-β-cyclodextrin: Elliptical distortion of the cavity and unique 'Yin-Yang' stacking
Lindner, Hans J.; Yuan, De-Qi; Fukudome, Makoto; Fujita, Kahee; Lichtenthaler, Frieder W.; Chemical communications (Cambridge, England)  (2003) –; doi:10.1039/b303788f

data_7103762
_publ_section_title
; 
Crystal Structure od mono[3-(2-imidazolylthio)]-altro-\b-cyclodextrin:
Elliptical distortion of the cavity and unique 'Yin-Yang' stacking
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b303788f
_journal_year                    2003
_chemical_absolute_configuration syn
_chemical_compound_source        'synthesized by Fujita et al. see text'
_chemical_formula_moiety         'C45 H72 N2 O34 S1, 15.5(H2 O1)'
_chemical_formula_sum            'C45 H103 N2 O49.5 S'
_chemical_formula_weight         1496.35
_chemical_name_common
;
mono-[3-(2-imidazolylthio)]-altro-\b-cyclodextrin
;
_chemical_name_systematic
; 
cyclo[(1\\rightarrow4)-(3-dexoy-3-(2-imidazolylthio))-
\a-D-altropyranosyl-hexakis(1\\rightarrow4)-\a-D-glucopyranosyl]
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.7589(8)
_cell_length_b                   15.7589(8)
_cell_length_c                   53.461(5)
_cell_measurement_reflns_used    11892
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      1.35
_cell_volume                     13276.7(17)
_computing_cell_refinement       'STOE X-AREA (STOE, 2001)'
_computing_data_collection       'STOE X-AREA (STOE, 2001)'
_computing_data_reduction        'STOE X_RED (STOE, 2001)'
_computing_molecular_graphics    'PLATON (Spek, 1999)'
_computing_publication_material  'SHELXL97 CIF and IUCr SHELXL97-template'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source
'sealed tube X-ray tube 12 x 0.4mm long-fine-focus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.1423
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11892
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6392
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.00220(14)
_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   0.831
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     917
_refine_ls_number_reflns         6735
_refine_ls_number_restraints     685
_refine_ls_restrained_S_all      0.815
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                2521
_reflns_number_total             6735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303788f.txt
_cod_data_source_block           ld691
_cod_original_formula_sum        'C45 H103 N2 O49.50 S1'
_cod_database_code               7103762