A highly hydrated α-cyclodextrin/1-undecanol inclusion complex: crystal structure and hydrogen-bond network from high-resolution neutron diffraction at 20K
Gallois-Montbrun, Delphine; Le Bas, Geneviève; Mason, Sax A.; Prangé, Thierry; Lesieur, Sylviane; Acta Crystallographica Section B 69 (2013) 214–227; doi:10.1107/S2052519213001772

data_2105942
_publ_section_title
;
 A highly hydrated \a-cyclodextrin/1-undecanol inclusion complex: crystal
 structure and hydrogen-bond network from high-resolution neutron
 diffraction at 20K
;
_journal_coeditor_code           EB5023
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              214
_journal_page_last               227
_journal_paper_doi               10.1107/S2052519213001772
_journal_volume                  69
_journal_year                    2013
_chemical_formula_sum            'C80.75 H175.5 O82.25'
_chemical_formula_weight         2464
_chemical_name_common            'alpha-cyclodextrin 1-undecanol hydrate'
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 95.8270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.7452(4)
_cell_length_b                   27.0276(4)
_cell_length_c                   15.72520(10)
_cell_measurement_reflns_used    7800
_cell_measurement_temperature    20
_cell_measurement_theta_max      62.40
_cell_measurement_theta_min      4.26
_cell_volume                     12154.0(3)
_computing_cell_refinement       'ILL RAFD19'
_computing_data_collection       'ILL HKLGEN, MAD'
_computing_data_reduction        'ILL RETREAT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      20
_diffrn_detector_area_resol_mean '1.56mm vert., 2.5 mm hor,'
_diffrn_measured_fraction_theta_full 0.830
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_device_type  'D19 position sensitive detector dif'
_diffrn_measurement_method       'omega steps-scans'
_diffrn_radiation_monochromator  'copper 331'
_diffrn_radiation_source         'ILL high flux reactor, beam H11'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.46160
_diffrn_reflns_av_R_equivalents  0.1211
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47610
_diffrn_reflns_theta_full        80.46
_diffrn_reflns_theta_max         80.46
_diffrn_reflns_theta_min         10.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '2 hours'
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.277
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1431
_exptl_crystal_size_max          3.40
_exptl_crystal_size_mid          1.48
_exptl_crystal_size_min          1.27
_refine_diff_density_max         1.495
_refine_diff_density_min         -1.030
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2382
_refine_ls_number_reflns         13268
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1486
_refine_ls_R_factor_gt           0.1237
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1429P)^2^+556.9357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2876
_refine_ls_wR_factor_ref         0.3089
_reflns_number_gt                10550
_reflns_number_total             13268
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            eb5023sup1.cif
_cod_data_source_block           C11neutron
_cod_original_sg_symbol_H-M      C2
_cod_original_formula_sum        'C80.75 H175.50 O82.25'
_cod_database_code               2105942
_cod_database_fobs_code          2105942