Biotransformation, spectroscopic investigation, crystal structure and electrostatic properties of 3,7α-dihydroxyestra-1,3,5(10)-trien-17-one monohydrate studied using transferred electron-density parameters
Shahid, Ammara; Aziz, Ambreen; Noureen, Sajida; Ahmed, Maqsood; Yousuf, Sammer; Choudhary, Muhammad Iqbal; Acta Crystallographica Section C 74 (2018) 534–541; doi:10.1107/S2053229618004953

data_2021115
_publ_section_title
;
 Biotransformation, spectroscopic investigation, crystal structure and
 electrostatic properties of 3,7\a-dihydroxyestra-1,3,5(10)-trien-17-one
 monohydrate studied using transferred electron-density parameters
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              534
_journal_page_last               541
_journal_paper_doi               10.1107/S2053229618004953
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C18 H22 O3, H2 O'
_chemical_formula_moiety         'C18 H22 O3, H2 O'
_chemical_formula_sum            'C18 H24 O4'
_chemical_formula_weight         304.368
_chemical_name_systematic
;
3,7\a-Dihydroxyestra-1,3,5(10)-trien-17-one monohydrate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'MoPro v16'
_cell_angle_alpha                90.
_cell_angle_beta                 91.94(2)
_cell_angle_gamma                90.
_cell_formula_units_Z            2
_cell_length_a                   6.143(3)
_cell_length_b                   8.4833(17)
_cell_length_c                   14.767(3)
_cell_measurement_reflns_used    2931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.166
_cell_measurement_theta_min      2.994
_cell_volume                     769.1(4)
_computing_cell_refinement
;
APEX2 (Bruker, 2014)
;
_computing_data_collection       'Bruker D8 Venture PHOTON II Detector'
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008) and <i>MoProViewer</i> (Guillot,
2011)
;
_computing_publication_material
;
pubCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>MoPro</i> (Jelsch <i>et al.</i>,  2005)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>,  1993)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON II Detector'
_diffrn_measurement_method       'omega and phi scan'
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_source         Microfocus
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.07014
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9196
_diffrn_reflns_theta_full        72.17
_diffrn_reflns_theta_max         72.17
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.28068
_refine_diff_density_min         -0.2634
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.000
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0316
_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^)+(0.06P)^2^+0.05P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                2905
_reflns_number_total             2931
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ly3062sup1.cif
_cod_data_source_block           ELMAM2_MoPro
_cod_original_cell_volume        769.2(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2021115
_cod_database_fobs_code          2021115