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_1508400
_publ_section_title
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 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 unk
_chemical_formula_moiety         'C14 H14 O4'
_chemical_formula_sum            'C14 H14 O4'
_chemical_formula_weight         246.25
_chemical_name_common
;
Aegelinol
;
_chemical_name_systematic
;
 pyranocoumarin
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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            12
_cell_length_a                   6.8921(3)
_cell_length_b                   11.4302(9)
_cell_length_c                   44.964(3)
_cell_measurement_reflns_used    2837
_cell_measurement_temperature    150.05(10)
_cell_measurement_theta_max      28.0954
_cell_measurement_theta_min      3.2468
_cell_volume                     3542.2(4)
_computing_cell_refinement
;
'Sat Apr 21 20:58:11 2012'
;
_computing_data_collection
;
'Sat Apr 21 20:58:11 2012'
;
_computing_data_reduction
;
'Sat Apr 21 20:58:11 2012'
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150.05(10)
_diffrn_detector_area_resol_mean 10.3712
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            11272
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.0954
_diffrn_reflns_theta_min         3.2468
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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'Sat Apr 21 20:58:11 2012'
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rod like'
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(9)
_refine_ls_extinction_coef       0.0010(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   1.097
_refine_ls_hydrogen_treatment
;
all Hydrogen atoms have been refined in
 the riding mode on their carrier atom
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         5883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+0.7867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                5198
_reflns_number_total             5883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file
C14H14O4_P21P21P21_crystals-02-01441-s003_DC145.cif
_cod_data_source_block           shelxl_chateigner_1508400
_cod_depositor_comments
;
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 
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_cod_database_code               1508400