Structure of Equilenin at 100K: an estrone-related steroid
Frampton, Christopher S.; MacNicol, David D.; Acta Crystallographica Section E 73 (2017) 1223–1226; doi:10.1107/S2056989017010532

data_2242124
_publ_section_title
;
 Structure of Equilenin at 100K: an estrone-related steroid
;
_journal_coeditor_code           SU5383
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1223
_journal_page_last               1226
_journal_paper_doi               10.1107/S2056989017010532
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C18 H18 O2'
_chemical_formula_sum            'C18 H18 O2'
_chemical_formula_weight         266.32
_chemical_melting_point          531
_chemical_name_common
;
Equilenin
;
_chemical_name_systematic
3-Hydroxy-13-methyl-11,12,13,14,15,16-hexahydrocyclopenta[<i>a</i>]phenanthren-17-one
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.27709(7)
_cell_length_b                   7.32686(6)
_cell_length_c                   25.5179(2)
_cell_measurement_reflns_used    13177
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      76.3890
_cell_measurement_theta_min      3.4610
_cell_volume                     1360.57(2)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and <i>Mercury</i> (Macrae <i>et al</i>.,
2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXD2014 (Sheldrick, 2010)
;
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 5.2921
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction SuperNova Dualflex AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16660
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.465
_diffrn_reflns_theta_min         3.464
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku Oxford Diffraction, 2015)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       rod
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.173
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1130 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0525P)^2^+0.3100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                2754
_reflns_number_total             2769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5383sup1.cif
_cod_data_source_block           I
_cod_database_code               2242124
_cod_database_fobs_code          2242124
_shelx_estimated_absorpt_t_min   0.776
_shelx_estimated_absorpt_t_max   0.955
_shelx_hkl_checksum              23793
_shelx_res_checksum              69464
_shelxl_version_number           2014/6