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_1513212
_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            'C40 H70 N0 O40'
_chemical_formula_weight         1190.96
_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                 110.926(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1417(13)
_cell_length_b                   10.1840(10)
_cell_length_c                   20.937(2)
_cell_measurement_temperature    198(2)
_cell_volume                     3015.6(5)
_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      198(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19044
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.9684
_exptl_absorpt_correction_T_min  0.9515
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.497
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         10219
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0852
_refine_ls_shift/su_max          1.792
_refine_ls_shift/su_mean         0.111
_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          0.2413
_refine_ls_wR_factor_ref         0.2555
_reflns_number_gt                8655
_reflns_number_total             10219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            CD3.CIF
_cod_data_source_block           cd3
_cod_original_cell_volume        3015.5(5)
_cod_database_code               1513212