A new estra-1,3,5(10)-triene-3,17β-diol solvate: estradiol‒methanol‒water (3/2/1)
Parrish, Damon A.; Pinkerton, A. Alan; Acta Crystallographica Section C 59 (2003) o80–o82; doi:10.1107/S0108270102021637

data_2013218
_publ_section_title
;
 A new estra-1,3,5(10)-triene-3,17\b-diol solvate:
 estradiol--methanol--water (3/2/1)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o80
_journal_page_last               o82
_journal_paper_doi               10.1107/S0108270102021637
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         'C18 H24 O2 , 0.67C H4 O , 0.33H2 O'
_chemical_formula_sum            'C18.67 H27.33 O3'
_chemical_formula_weight         299.74
_chemical_name_common            estradiol
_chemical_name_systematic
;
estra-1,3,5(10)-triene-3,17\b-diol-methanol-water (3/2/1)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 117.9780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   11.7152(4)
_cell_length_b                   19.6270(6)
_cell_length_c                   12.1310(4)
_cell_measurement_reflns_used    7309
_cell_measurement_temperature    298.0(10)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.25
_cell_volume                     2463.34(14)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART Platform CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56085
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_av_sigmaI/netI    0.067
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44195
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.051
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'multipole expansion (Blessing, 1995) using SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         21122
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.085
_refine_ls_R_factor_gt           0.058
_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^)+(0.0812P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.134
_refine_ls_wR_factor_ref         0.145
_reflns_number_gt                15597
_reflns_number_total             21122
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq1003.cif
_cod_data_source_block           I
_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 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2013218
_cod_database_fobs_code          2013218