Macromolecular ensembles of cyclodextrin crystallohydrates and clathrates ‒ experimental and theoretical gas ‒ and condense phase study
Ivanova, Bojidarka; Spiteller, Michael; International Journal of Biological Macromolecules 64 (2014) 383–391; doi:10.1016/j.ijbiomac.2013.12.026

data_1513211
_publ_section_title
;
 Macromolecular ensembles of cyclodextrin crystallohydrates and clathrates
 -- experimental and theoretical gas -- and condense phase study
;
_journal_name_full
'International Journal of Biological Macromolecules'
_journal_page_first              383
_journal_page_last               391
_journal_paper_doi               10.1016/j.ijbiomac.2013.12.026
_journal_volume                  64
_journal_year                    2014
_chemical_formula_sum            'C43 H70 O39'
_chemical_formula_weight         1210.98
_space_group_IT_number           4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 110.479(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1625(12)
_cell_length_b                   10.2550(8)
_cell_length_c                   20.9687(17)
_cell_measurement_temperature    200(2)
_cell_volume                     3054.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker GIS'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker APEX2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART X2S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'doubly curved silicon crystal'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19256
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.9802
_exptl_absorpt_correction_T_min  0.9476
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.936
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2.2(15)
_refine_ls_extinction_coef       0.017(3)
_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   1.188
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         8766
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0957
_refine_ls_shift/su_max          5.257
_refine_ls_shift/su_mean         0.103
_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          0.2600
_refine_ls_wR_factor_ref         0.2790
_reflns_number_gt                7141
_reflns_number_total             8766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            CD2.CIF
_cod_data_source_block           cd2
_cod_original_formula_sum        'C21.50 H35 O19.50'
_cod_database_code               1513211