Crystal structure of bis[3-methoxy-17β-estra-1,3,5(10)-trien-17-yl] oxalate
Harrison, William T. A.; Nahar, Lutfun; Turner, Alan B.; Acta Crystallographica Section E 70 (2014) 62–64; doi:10.1107/S1600536814009349

data_2239784
_publ_section_title
;
 Crystal structure of bis[3-methoxy-17\b-estra-1,3,5(10)-trien-17-yl]
 oxalate
;
_journal_coeditor_code           SU0001
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              62
_journal_page_last               64
_journal_paper_doi               10.1107/S1600536814009349
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         'C40 H50 O6'
_chemical_formula_sum            'C40 H50 O6'
_chemical_formula_weight         626.80
_chemical_name_common
;
Bis(17-\b-estradiol 3-methyl ether) oxalate diester
;
_chemical_name_systematic
;
Bis[3-methoxy-17\b-estra-1,3,5(10)-trien-17-yl] oxalate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   7.8559(4)
_cell_length_b                   14.1579(10)
_cell_length_c                   29.888(2)
_cell_measurement_reflns_used    4069
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     3324.2(4)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997), and SORTAV (Blessing,
1995)
;
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f'
_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  0.1690
_diffrn_reflns_av_sigmaI/netI    0.1563
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            21809
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.307
_refine_ls_abs_structure_details None
_refine_ls_extinction_coef       0.0132(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         3674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1555
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                2220
_reflns_number_total             3674
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su0001sup1.cf
_cod_data_source_block           I
_cod_database_code               2239784
_cod_database_fobs_code          2239784