A solid-state study of the inclusion of endosulfan in native and derivatised cyclodextrins using X-ray diffraction and thermoanalytical methods
Cruickshank, Dyanne L.; Bourne, Susan A.; Caira, Mino R.; New Journal of Chemistry 36 (2012) 2007–; doi:10.1039/c2nj40364a

data_7052936
_publ_section_title
;
 A solid-state study of the inclusion of endosulfan in native and
 derivatised cyclodextrins using X-ray diffraction and thermoanalytical
 methods
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2007
_journal_paper_doi               10.1039/c2nj40364a
_journal_volume                  36
_journal_year                    2012
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C56 H98 O35, C9 H6 Cl6 O3 S, 1.04(H2O)'
_chemical_formula_sum            'C65 H106.08 Cl6 O39.04 S'
_chemical_formula_weight         1757.01
_chemical_melting_point          523
_chemical_name_common
;
heptakis(2,6-di-O-methyl)-beta-cyclodextrin.6,7,8,9,10,10 -
hexachloro-1,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin
3-oxide
;
_chemical_name_systematic
;
heptakis(2,6-di-O-methyl)-beta-cyclodextrin.6,7,8,9,10,10
-hexachloro-1,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-
benzodioxathiepin 3-oxide
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.907(4)
_cell_length_b                   29.784(4)
_cell_length_c                   20.352(3)
_cell_measurement_reflns_used    417
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      3.41
_cell_volume                     16310(4)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT 2000'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXD (TR Schneider & GM Sheldrick, 2002)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Kappa Apex II Duo diffractometer'
_diffrn_measurement_method       'phi- and omega-scans of 0.5 deg.'
_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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.1244
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62632
_diffrn_reflns_theta_full        25.82
_diffrn_reflns_theta_max         25.82
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.9806
_exptl_absorpt_correction_T_min  0.8828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             7411
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1790
_refine_ls_number_reflns         30518
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1850
_refine_ls_R_factor_gt           0.1023
_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^)+(0.1550P)^2^+39.9039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2548
_refine_ls_wR_factor_ref         0.3065
_reflns_number_gt                16217
_reflns_number_total             30518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2nj40364a.txt
_cod_data_source_block           d:\dyanne\2012\endosu~1\dmbbend\merg2\dmbbend
_cod_original_formula_sum        'C65 H106.08 Cl6 O39.04 S1'
_cod_database_code               7052936