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/S0108768113001778

data_2105444
_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_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              214
_journal_page_last               227
_journal_paper_doi               10.1107/S0108768113001778
_journal_volume                  69
_journal_year                    2013
_chemical_formula_sum            'C79.46 H120.12 O73.55'
_chemical_formula_weight         2255.22
_chemical_name_common
;
 alpha-cyclodextrin undecanol complex
 (water solvate)
;
_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                90.00000
_cell_angle_beta                 95.920(10)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   28.725(3)
_cell_length_b                   27.195(3)
_cell_length_c                   15.838(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    277(2)
_cell_volume                     12306(2)
_computing_data_reduction        'DENZO SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      277(2)
_diffrn_measured_fraction_theta_full 0.471
_diffrn_measured_fraction_theta_max 0.471
_diffrn_measurement_device_type  'MAR 345 image plate'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'LURE DW32 beam line'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.97260
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11213
_diffrn_reflns_theta_full        28.57
_diffrn_reflns_theta_max         28.57
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         5000
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4741
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.282
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.237
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1410
_refine_ls_number_reflns         5941
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.244
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2237
_refine_ls_wR_factor_ref         0.2264
_reflns_number_gt                5806
_reflns_number_total             5941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            eb5023.cif
_cod_data_source_block           c11Xray
_cod_original_sg_symbol_H-M      C2
_cod_database_code               2105444
_cod_database_fobs_code          2105444