Crystal structure of (8S*,9S*,13S*,14R*,17S*)-estra-1(10),2,4,6-tetraene- 14,17-diol monohydrate, C~18~H~22~O~2~ · H~2~O
Wefelscheid, Ulrike K.; Brüdgam, Irene; Hartl, Hans; Reißig, Hans-Ulrich; Zeitschrift für Kristallographie - New Crystal Structures 222 (2007) 467–468; doi:

data_8102222
_publ_section_title
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Crystal structure of (8S*,9S*,13S*,14R*,17S*)-estra-1(10),2,4,6-tetraene-
14,17-diol monohydrate, C~18~H~22~O~2~ &#x00B7; H~2~O
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_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              467
_journal_page_last               468
_journal_volume                  222
_journal_year                    2007
_chemical_formula_structural     'C18H22O2 &#x00B7; H2O'
_chemical_formula_sum            'C18 H24 O3'
_chemical_formula_weight         288.38
_chemical_melting_point          441.0(10)
_chemical_name_systematic
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(8S*,9S*,13S*,14R*,17S*)-estra-1(10),2,4,6-tetraene-14,17-diol monohydrate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 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            4
_cell_length_a                   11.9945(19)
_cell_length_b                   17.309(3)
_cell_length_c                   7.4999(12)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      3.41
_cell_volume                     1557.1(4)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'phi/omega, \d\w = 0.3&#x00B0;'
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17353
_diffrn_reflns_theta_full        30.59
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         2.07
_diffrn_standards_interval_time  '5 sec/frame'
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          .6
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.3(9)
_refine_ls_extinction_coef       0.0000(14)
_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   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         4725
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          4.579
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                3691
_reflns_number_total             4725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2158.cff
_cod_data_source_block           org3wef
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '440 - 442K' was changed to
'441.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               8102222