Paweł Grochulski

Crystal structures of 4,11-pregnadiene-3,20-dione and 21-methyl-20-oxa-4-pregnene-3,20-dione

The structures of the title compounds were solved by direct methods and refined by anisotropic full-matrix least-squares methods. 4,11-Pregnadiene-3,20-dione, C21H28O2(1) crystallizes in the monoclinic space groupP21 (Z=2). The unit cell parametersa, b, c (Å), and β (°) were: 12.319(2), 7.700(2), 9.717(2), 109.41(2). TheA- andC-rings exhibit intermediate sofa-halfchair conformations. TheB-ring has a chair conformation and theD-ring assumes an intermediate envelope-half-chair conformation. The progesterone side chain has a typical conformation; the C16−C17−C20−O20 torsion angle is −15.1(4)°. 21-Methyl-20-oxa-4-pregnene-3,20-dione, C21H30O3 (2) crystallizes in the orthorhombic space groupP212121 (Z=4). The unit cell parametersa, b, c (Å) were: 12.926(2), 19.447(4), 7.313(1). The progesterone side chain has an unusual conformation; the C16−C17−C20−O20 torsion angle is 174.6(4)°. TheA-ring has a 1α, 2β-half-chair conformation, ringsB andC exhibit chair conformations and ringD is in a 13β,14α-half-chair conformation.

Structure of 6β-hydroxy-4-androsten-3,17-dione monohydrate, C19H27O3·H2O

The structure of the title compound was determined by X-rays:Mr=319.4,P212121,a=7.753(3),b=10.566(8),c=20.997(10) Å,Z=4 andDx=1.171 M gm−3. FinalR=0.042 (Rw=0.041) for 1814 unique reflections. The water molecule is the hydrogen donor to O3 and O17 and an hydrogen acceptor from the O17 hydroxyl group.

Structure of 17β-hydroxy-4-pregnen-20-yn-3-one, C21H28O2

The crystal structure of 17β-hydroxy-4-pregnen-20-yn-3-one, C21H28O2, was determined by means of X-ray diffraction methods.Mr=312.5, space groupP21,a=6.493(1),b=21.065(3),c=6.478(1) Å,β=105.97(1)°,Vc=851.9(3) Å3,Z=2,Dx=1.22 Mg m−3, CuKα radiation (λ=1.54184 Å),μ(CuKα)=5.5 cm−1,F(000)=340. The structure was solved withMultan; final conventionalR=0.032 (Rw=0.032) for 1803 reflections. The molecule studied (I) has an overall conformation almost identical to 19-norethindrone (II), although ringA of molecule (I) is slightly more bent toward theα direction of the steroid skeleton in comparison with molecule (II).

Structure of 1-[ethyl(phenyl)phosphinyl]-1-phenylethanol, C16H19O2P

M r = 274.3, monoclinic, space group P2~/c, Z=4, a=15.960(4), b=5.614(2), c= 16.418(4)A, fl= 110.06(2) ° , V= 1381.7A 3, Din= 1.303, Dx=l.318Mgm -3, MoKa, 2=0-7107/k, /t = 0.20 mm -~, F(000) = 584, room temperature, m.p. 410-412 K, final R = 0.078 for 2973 reflections. There are no unusual bond distances and angles. The conformation about C(10)-P is such that the two phenyl groups are in antiperiplanar orientation. The molecules form chains along the (010) direction by means of hydrogen bonding with O...O 2.758 (3), H...O 1.94 (6)/~ and O...H-O 144 (6) °.

Structure of 17α-methyl-testosterone semihydrate, C20H30O2.1/2 H2O

AbstractThe crystal structure of 17α-methyltestosterone hemihydrate, C20H30O2·1/2H2O, has been determined:Mr=312.5, space groupP21212121,a=6.374(2),b=12.807(2),c=43.398(5)Å,Vc=3543(2)Å3,Z=8,Dx=1.172 mg−3, CuKα radiation (

Structure of 6-methyl-3,20-dioxo-4,6-pregnadien-17α-yl acetate, C24H32O4

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Structure of 4-methoxy-4-cholesten-3-one, C28H46O2

= 1.54184 Å),μ(CuKα)=5.5 cm−1,F(000)=1376. The structure was solved usingMultan. The final conventionalR=0.053 (Rw=0.052) for 3634 reflections. The structure contains two crystallographically independent molecules in the asymmetric part of the unit cell that have almost identical geometry.

Structure of 11α-hydroxy-progesterone, C21H30O3

AbstractThe crystal and molecular structure of 3α,12β-dihydroxy-2β-morpholino-5α-pregnan-20-one, C25H41O4N, has been determined:Mr=419.6,P21,a=13.5778(8),b=14.4340(8),c=5.8943(5) Å,β=94.32(1)°,Vc=1151.9(3) Å3,Z=2,Dx=1.21 g cm−3,