Rigid Duplex α-Cyclodextrin Reversibly Connected With Disulfide Bonds. Synthesis and Inclusion Complexes
Lukáš Kumprecht; Miloš Buděsínský; Jiří Vondrášek; Jiří Vymětal; Jiří Čěrný; Ivana Císařová; Jiří Brynda; Vladimír Herzig; Petr Koutník; Jiří Závada; Tomáš Kraus; Journal of Organic Chemistry 74 (2009) 1082–1092; doi:10.1021/jo802139s

data_4024284
_publ_section_title
;
Rigid Duplex \a-Cyclodextrin Reversibly Connected With Disulfide Bonds.
Synthesis and Inclusion Complexes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1082
_journal_page_last               1092
_journal_paper_doi               10.1021/jo802139s
_journal_volume                  74
_journal_year                    2009
_chemical_absolute_configuration syn
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C72 H116 O56 S4, 6(H2 O)'
_chemical_formula_sum            'C72 H128 O62 S4'
_chemical_formula_weight         2113.98
_chemical_name_systematic        ?
_space_group_IT_number           79
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      79
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Jul 10 11:16:08 2008'
_audit_creation_method           'PLATON <TABLE ACC> option'
_audit_update_record
;
2008-07-24 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3680(7)
_cell_length_b                   22.3680(7)
_cell_length_c                   23.1510(4)
_cell_measurement_reflns_used    4627
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.00
_cell_measurement_theta_min      1.00
_cell_volume                     11583.1(6)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30096
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        24.10
_diffrn_reflns_theta_max         24.10
_diffrn_reflns_theta_min         3.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.784
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         8758
_refine_ls_number_restraints     990
_refine_ls_restrained_S_all      2.726
_refine_ls_R_factor_all          0.1610
_refine_ls_R_factor_gt           0.1343
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3430
_refine_ls_wR_factor_ref         0.3687
_reflns_number_gt                6791
_reflns_number_total             8758
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            jo802139s_si_002.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:
'_chemical_absolute_configuration' value 'SYN' changed to 'syn' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_symmetry_cell_setting'
value 'Tetragonal' changed to 'tetragonal' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value ' none' changed to
'none' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4024284