Determination of the Absolute Configuration of Aegelinol by Crystallization of Its Inclusion Complex with beta-Cyclodextrin
Elasaad, Kossay; Alkhatib, Racha; Hennebelle, Thierry; Norberg, Bernadette; Wouters, Johan; Crystals 2 (2012) 1441–1454; doi:10.3390/cryst2041441

data_1508399
_publ_section_title
;
 Determination of the Absolute Configuration of Aegelinol by
 Crystallization of Its Inclusion Complex with beta-Cyclodextrin
;
_journal_issue                   4
_journal_name_full               Crystals
_journal_page_first              1441
_journal_page_last               1454
_journal_paper_doi               10.3390/cryst2041441
_journal_volume                  2
_journal_year                    2012
_chemical_absolute_configuration rm
_chemical_formula_moiety
; 
 C42 H70 O35, C14 H14 O4, 0.25(O2), 9.25(H2 O), 2(O)
;
_chemical_formula_sum            'C56 H102.5 O50.75'
_chemical_formula_weight         1587.88
_chemical_melting_point          ?
_chemical_name_common
; 
 beta-cyclodextrin Aegelinol clathrate hydrate 
;
_chemical_name_systematic
; 
 cyclomaltoheptaose pyranocoumarin clathrate hydrate 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                99.6620(10)
_cell_angle_beta                 113.4230(10)
_cell_angle_gamma                102.4810(10)
_cell_formula_units_Z            2
_cell_length_a                   15.4039(12)
_cell_length_b                   15.2813(12)
_cell_length_c                   17.8904(14)
_cell_measurement_reflns_used    19702
_cell_measurement_temperature    149.8(5)
_cell_measurement_theta_max      67.4424
_cell_measurement_theta_min      2.7674
_cell_volume                     3618.4(5)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 and SHELXH (Sheldrick, 1997) '
_computing_structure_solution    'atomic coordination replacement methods'
_diffrn_ambient_temperature      149.8(5)
_diffrn_detector_area_resol_mean 10.3712
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54179
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36967
_diffrn_reflns_theta_full        69.59
_diffrn_reflns_theta_max         69.59
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.8660
_exptl_absorpt_correction_T_min  0.6779
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1689.0
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.279
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.5(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2068
_refine_ls_number_reflns         15938
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.356
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1359P)^2^+3.1177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1900
_refine_ls_wR_factor_ref         0.1966
_reflns_number_gt                14762
_reflns_number_total             15938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file
C56H102.5O50.75_P1_crystals-02-01441-s002_DC144.cif
_cod_data_source_block           new4_chateigner_1508400
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' according to the built-in table
from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_Hall     P1
_cod_original_sg_symbol_H-M      P1
_cod_database_code               1508399