Applications of Low Temperature Gradient Sublimation in Vacuo: Rapid Production of High Quality Crystals. The First Solvent-Free Crystals of Ethinyl Estradiol
Karpinska, Jolanta; Erxleben, Andrea; McArdle, Patrick; Crystal Growth & Design 13 (2013) 1122–; doi:10.1021/cg301479c

data_4507481
_publ_section_title
;
 Applications of Low Temperature Gradient Sublimation in Vacuo: Rapid
 Production of High Quality Crystals. The First Solvent-Free Crystals of
 Ethinyl Estradiol
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1122
_journal_paper_doi               10.1021/cg301479c
_journal_volume                  13
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_sum            'C20 H24 O2'
_chemical_formula_weight         296.39
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_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            8
_cell_length_a                   6.8664(3)
_cell_length_b                   20.9003(11)
_cell_length_c                   22.0448(8)
_cell_measurement_reflns_used    2754
_cell_measurement_temperature    150.1
_cell_measurement_theta_max      29.1217
_cell_measurement_theta_min      2.9325
_cell_volume                     3163.6(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_molecular_graphics
;
 ORTEX, McArdle, P. (1995) J.Appl.Cryst.,28,65-65
;
_computing_publication_material
;
 Ciftab, G.M. Sheldrick, G.M. (2008) Acta Crystallogr.,D64,112-122
;
_computing_structure_refinement
;
 SHELXL-97/2, G.M. Sheldrick, G.M. (2008) Acta Crystallogr.,D64,112-122
;
_computing_structure_solution
;
 SHELXS-97, Sheldrick, G.M. (2008) Acta Crystallogr.,D64,112-122
;
_diffrn_ambient_temperature      150.1
_diffrn_detector_area_resol_mean 16.1048
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -69.00    9.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.3278  -77.0000   60.0000 78
  
  2 omega   14.00   48.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7966   37.0000 -180.0000 34
  
  3 omega   -7.00   25.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7966   91.0000 -160.0000 32
  
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0279935000
_diffrn_orient_matrix_UB_12      0.0246862000
_diffrn_orient_matrix_UB_21      -0.0305585000
_diffrn_orient_matrix_UB_22      0.0190316000
_diffrn_orient_matrix_UB_23      0.0248881000
_diffrn_orient_matrix_UB_31      0.0945780000
_diffrn_orient_matrix_UB_32      0.0134573000
_diffrn_orient_matrix_UB_33      0.0020323000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9428
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.7(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5434
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                3926
_reflns_number_total             5434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301479c_si_002.cif
_cod_data_source_block           EE
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4507481