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_1513210
_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            'C72 H114 N0 O73'
_chemical_formula_weight         2147.63
_space_group_IT_number           19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            2
_cell_length_a                   9.4126(14)
_cell_length_b                   14.233(2)
_cell_length_c                   37.401(5)
_cell_measurement_temperature    291(2)
_cell_volume                     5010.6(12)
_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      291(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0781
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            25749
_diffrn_reflns_theta_full        22.78
_diffrn_reflns_theta_max         22.78
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.9871
_exptl_absorpt_correction_T_min  0.9582
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         6698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          2.415
_refine_ls_shift/su_mean         0.040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1695
_reflns_number_gt                5133
_reflns_number_total             6698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            CD1.CIF
_cod_data_source_block           cd1
_cod_original_cell_volume        5010.6(13)
_cod_database_code               1513210