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_2021113
_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         304.37
_chemical_name_systematic
;
3,7\a-Dihydroxyestra-1,3,5(10)-trien-17-one monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_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)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>,  1993) in WinGX (Farrugia, 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON II Detector'
_diffrn_measurement_method       'omega and phi scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_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        67.679
_diffrn_reflns_theta_max         72.166
_diffrn_reflns_theta_min         2.994
_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    1.314
_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         0.338
_refine_diff_density_min         -0.268
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1292 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2931
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+0.2090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                2905
_reflns_number_total             2931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ly3062sup1.cif
_cod_data_source_block           IAM_SHELXL
_cod_original_cell_volume        769.2(4)
_cod_database_code               2021113
_cod_database_fobs_code          2021113
_shelx_estimated_absorpt_t_min   0.727
_shelx_estimated_absorpt_t_max   0.916
_shelx_hkl_checksum              76476
_shelx_res_checksum              70025
_shelxl_version_number           2014/6