Molecular structure and absolute configuration of (+)-(1R, 2S, 6R, 7S, 1′R)-5-(1′-phenylethylamino)-endo-tricyclo[5.2.1.02,6]deca-4,8-dien-3-one

The crystal and molecular structure of (+)-(1R, 2S, 6R, 7S, 1R)-5-(1-phenylethylamino)-endo-tricyclo[5.2.1.0^2,6]deca-4,8-dien-3-one is described. Based on the known absolute configuration (R) of the -phenylethylamine moiety the X-ray analysis revealed the absolute configuration of the title compound. The structure was refined to R ₁ = 0.0298 for 1950 reflections (with I > 2(I)). Crystal data: C₁₈H₁₉NO, monoclinic, space group P2₁, a = 6.7406(4), b = 9.959(2), c = 11.3123(8)Å, = 102.969(5), V = 740.0(2)ų, and Z = 2.     

The crystal and molecular structure of spiro[1-(S)-Br-3-(S)-H-4-(R)-l-(1′ R,2′ S,5′R)-menthyloxy-5-oxo-6-oxa-bicyclo[3.1.0]hexane-2,3′-(R)-(4′-(R)-diphenylmethoxy-5′-l-(1′ R,2′ S,5′ R)-menthyloxy-butyrolactone)]

Crystal structure of C₄₁H₅₃O₇Br has been determined by single-crystal X-ray diffraction. The compound crystalline in the orthorhombic space group P2₁2₁2₁, with a = 11.264(2), b = 12.058(2), c = 29.337(6) Å, Z = 4. The bond angles of cyclopropane moiety in the molecule are approximate to 60° and agree with theoretic values of the internal angles in a cyclopropane, and two chiral menthyloxy groups are located above and under the whole chiral molecule, respectively. The configuration of the pentacyclic lactone is shown as envelope form.     

5-(thien-2-yl) uracil analogs: 5-(5-methylthien-2-yl)-2′-deoxyuridine, 5-(5-thien-2-yl)-2′-deoxyuridine,and 5-(5-bromothien-2-yl)-2′-deoxyuridine

Crystal structures of 5-(5-methylthien-2-yl)-2-deoxyuridine (I), 5-(5-thien-2-yl)-2-deoxyuridine (II) and 5-(5-bromothien-2-yl)-2-deoxyuridine (III) have been obtained from data collected on a four-circle Enraf-Nonius diffractometer (CAD-4 system). Space group, unit/cell parameters and finalR indices are:I, monoclinic,P2₁,a=9.105(2),b=20.819(2),c=7.932(2) Å, =98.79(2)°,R=5.7%;II, monoclinic,P2₁,a=8.720(4),b=20.793(4),c=7.884(4) Å, =95.06(2)°,R=5.8%;III, monoclinic,P2₁,a=9.260(2),b=41.655(7),c=7.926(2) Å, =97.996(13)°,R=9.4%. Structural properties of the title compounds are compared with those of 5-(5-chlorothien-2-yl)-2-deoxyuridine (IV) previously reported in order to explain their affinity for HSV-1 thymidine kinase and their eventual interaction with viral DNA polymerase. The main structural features observed are the coplanarity of the uracil and thienyl cycles stabilized by a S–O intramolecular interaction and the formation of dimeric intermolecular H bonds between two uracil moieties.     

Crystal and molecular structure of (3aR,8bS,5′R)3-[(2,5-dihydro-3-methyl-2-oxo-5-furanyl)oxymethylene]-3,3a,4,8b-tetrahydroindeno[1,2-b]furan-2-one

The stereogeometry and absolute configuration of the title compound has been proved by an X-ray diffraction analysis. Crystal data: monoclinic, C2,a=20.2528(4),b=6.7254(2),c=10.6748(2) Å, =94.699(3),Z=4. The crystal structure has been solved by vector search methods and refined toR ₁=0.053 for 2043 observed reflections.     

The molecular structure of acetato[2-(pyridin-2′-yl)phenyl]mercury(II)

The crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in the monoclinic crystal system witha=8.152(4),b=17.994(7),c=8.634(9) Å, =108.92(5)°, space group P2₁/c (N:14),V=1198.02 ų,Z=4. The mercuryl(II) atom forms two strong, almost colinear bonds (bond angle 176.1(4)°) with a carbon of the phenyl ring (Hg–C=1.99(1) Å) and one of the acetate oxygen atoms (Hg–O(1)=2.005(7) Å). These primary bonds are supplemented by secondary intramolecular interactions with the pyridine nitrogen (Hg...N=2.727(9) Å) and the other acetate oxygen (Hg...O(2)=2.925(8) Å), although the latter is very weak and the acetate anion therefore practically monodentate. Weak additional intermolecular Hg–C and Hg–O(1)interactions contribute to the lattice structure.     

Synthesis and crystal structure of 2-trifluoromethyl-1-[(2′-1H-tetrazole-5-yl-biphenyl-4-yl) methyl]benzimidazole

The crystal structure of 2-trifluoromethyl-1-[(2'-1H-tetrazle-5-yl-biphenyl-4-yl) methyl]-benzimidazole and a methylene chloride have been determined by X-ray crystallography. The compound crystallizes in the monoclinic space group, P2 ₁/n with cell dimensions a = 10.931(2) Å, b = 12.31(3) Å, c = 17.901(4) Å, = 102.45(3)°, V = 2352.9(8) ų, D _calc = 1.427 g/cm³, Z = 4, = 0.324 mm^–1, and F(000) = 1032, and its structure was refined to R ₁ = 0.0663 and wR ₂ = 0.1668 for 1910 observed reflections I > 2(I)). Intermolecular hydrogen bonds were identified between the N and H atoms of intermolecular benzimidazole group and tetrazole group.     

Synthesis and crystal structure of α,β-unsaturated ketone: 3,3′-[1,2-ethanediylbis(oxy-2,1-phenylene)]bis[1-(2-pyridyl)-2-propen-1-one]

The title compound, C₃₀H₂₄N₂O₄, 3,3′-[1,2-ethanediyl-bis(oxy-2,1-phenylene)]bis[1-(2-pyridyl)-2-propen-1-one] was synthesized and characterized by elemental analysis, FT-IR spectra, ¹H NMR, and X-ray single-crystal diffraction. In the molecule, the pyridine plane and the adjacent phenyl plane are almost coplanar with the dihedral angle of 3.07°, while the dihedral angle between the mean planes of the two asymmetric units is 67.56°. The crystal packing is stabilized by weak intermolecular C-H...N and C-H...O hydrogen bonds, C-H...π and π...π stacking interactions.     

Synthesis and crystal structure of (S, S, S, S)-N, N′-bis[N-(P-toluenesulfonamido)-1,2-diphenylethyl]ethylenediamine

(S, S, S, S)-N,N′-bis[N-(p-toluenesulfonamido)-1,2-diphenylethyl] ethylenediamine (C₄₄H₄₆N₄O₄S₂), has been synthesized and structurally characterized by elemental analysis, ¹H-NMR, MS, IR and single-crystal X-ray diffraction. The title compound contains four chiral centers with C atoms in S configuration. Molecules are connected to one another by hydrogen bonds between sulfonamide nitrogen and sulfonyl oxygen to form chains alone a axis.     

Crystal and Molecular Structure Studies of 1′-Benzyl-8-(4-fluorobenzyl)-8-azaspiro[bicyclo-[3.2.1]octane-3,4′-imidazolodine]-2′,5′-dione

Abstract  

The title compound, C₂₃H₂₃FN₃O₂ has been synthesized and the structure was investigated by X-ray diffraction studies. The compound crystallizes in the triclinic crystal class in the space group P[`1]P\overline{1} with cell parameters a = 9.345(2) ?, b = 10.940(3) ?, c = 11.986(4) ?, α = 72.349(6)°, β = 68.106(18)°, γ = 66.867(5)°, Z = 2 and V = 1027.8(5) ?³. The hydantoin ring adopts a planar conformation and is affected by the π conjugation. The pyrrolidine and piperidine rings in the bicyclo octane moiety adopt envelope and chair conformations respectively. The structure exhibits both inter and intramolecular hydrogen bonds of the type N–H···O, C–H···O and C–H···N. One of the oxygen atoms attached to the hydantoin ring simultaneously accepts two hydrogen bonds to form a three centered hydrogen bonding pattern.     

Molecular and crystal structure of two nickel(II) 1,2-dithiooxalato-S,S′ complexes using 1-(Rbenzyl)pyridinium cation (R = 4′-bromo-2′-fluoro or 4′-bromo)

[BrFPy]₂[Ni(dto)₂] (1) and [BrPy]₂[Ni(dto)₂] (2) complexes have been prepared by reaction of Na₂[Ni(S₂C₂O₂)₂] and the corresponding 1-(Rbenzyl)pyridinium bromide salt (R₁ = 4-bromo-2-fluoro, R₂ = 4-bromo). The crystallographic data for 1: monoclinic P2₁/c, a = 14.2192(1) Å, b = 14.2533(4) Å, c = 15.6535(3) Å, = 96.463(1)°, V = 3152.34(11) ų, Z = 4. Two cations, [Br₁F₁Py]⁺ and [Br₂F₂Py]⁺, both adopt a conformation where both the aromatic rings are twisted to the corresponding N(1)–C(10)–C(11) or N(2)–C(22)–C(23) reference plane. Data for 2: triclinic , a = 9.4042(3) Å, b = 9.6814(4) Å, c = 10.3357(4) Å, = 80.155(1)°, = 65.245(1)°, = 64.259(1)°, V = 769.68(5) ų, Z = 1. The [Ni(dto)₂]^2– anion exhibits a quasi-planar structure in both complexes. An extensive hydrogen bond network of C–H O is clearly observed in 1 and 2, and two complexes show similar crystal packing.     

Synthesis and crystal structure of (1R,2R)-N,N′-bis(4-toluenesulfonyl)-1, 2-di(4-methoxylphenyl)ethylenediamine

The reaction of (1R,2R)-1,2-di(4-methoxylphenyl)ethylenediamine with p-toluene sulfonyl chloride affords the title compound C₃₀H₃₂N₂O₆S₂, the structure of which is ascertained by X-ray diffraction. The title compound contains two chiral centre with each C atom in R configuration. Two adjacent molecules are linked by intermolecular hydrogen bonds through sulfonamide nitrogen and sulfonyl oxygen to form a one-dimensional chain alone a axis.     

Structure of two 1,3-dioxane derivatives from 4′, 5′-dimethylfurocoumarins: 4a, 11a-dihydro-4a, 11a-dimethyl-8H-pyrano[3′,2′∶5,6]benzofuro[3,2-e]-1, 3-dioxan-8-one and 7a,11a-dihydro-7a,11a-dimethyl-2H-pyrano[2′, 3′∶4,5]benzofuro[3,2-d] (1,3) dioxan-2-one

Treatment of dimethylated psoralen and angelicin in the 4, 5-position leads to the formation of 1,3-dioxane derivatives, resulting from the condensation of an 1,3-dioxane ring to the 4, 5-positions of the dihydrofurocoumarin moiety. The structures of these new compounds, 4a, 1 1a-dihydro-4a, 11a-dimethyl-8H-pyrano [3, 25,6]benzofuro[3,2-e]-1, 3-dioxan-8-one (C₁₅H₁₄O₅) (1) and 7a, 11a-dihydro-7a, 11a-dimethyl-2H-pyrano[2, 34, 5]benzofuro[3, 2-d](1, 3)dioxan-2-one (C₁₅H₁₄O₅) (2) have been assigned by¹H and¹³C NMR measurements, mass spectrometry results, and X-ray analysis. Compound (1): triclinic,P¯1,a=9.847(2),b=8.927(2),c=8.334(2) Å,=95.98(2),=108.81(3), =106.73(3)°; compound (2): triclinic,P¯1,a=7.296(4),b=7.481(2),c=11.812(4) Å,=91.67(2),=95.97(4), =94.20(3)°. The structures were solved by direct methods and refined by full-matrix least squares toR=0.050 (1) and 0.056 (2). In both compounds the coumarin rings can be regarded as coplanar, while the five-membered ring adopts an envelope conformation and the 1,3-dioxane ring a chair conformation.     

A quasi-layer structure of trinuclear molybdenum(IV) cluster, [Mo3S7(S2CNEt2)3]I·S8

The title compound, [Mo₃(₃-S)(-S₂)₃(S₂CNEt₂)₃]I·S₈, was obtained by solid state reaction of (NH₄)₂MoS₄, Et₂NCS₂Na, and Et₄NI at low heating temperature and crystallizes in space group P with a = 13.572(3), b = 13.813(4), c = 13.239(3) Å, = 92.63(3), = 100.15(3), = 117.89(2)°, V = 2136(2) ų, and D _calc. = 2.08 g/cm³ for Z = 2. The structure reveals that it consists of a trinuclear Mo cluster molecule, [Mo₃S₇(S₂CNEt₂)₃]I, and one S₈, which are connected to form a quasi-layer structure by the interaction between S₈ and the S atoms of the cluster molecule.     

Molecular and crystal structure of [NO2Py]2[Ni(mnt)2](NO2Py=1-(4-nitrobenzyl)pyridinium, mnt2−=maleonitriledithiolate)

The structure of [NO₂Py]₂[Ni(mnt)₂], as determined by x-ray single crystal analysis, consists of two 1-(4-nitrobenzyl)pyridinium cations and one [Ni(mnt)₂]^2– anion. The crystallographic data for the complex:monoclinic P2₁/n, a = 9.913(2) Å, b = 11.968(2) Å, c = 14.566(3) Å, = 100.36(3)°, V = 1699.9(6) ų, Z = 2. The [Ni(mnt)₂]^2– anion has a crystallographically imposed center of symmetry and exhibits a relatively planar structure. The cation, [NO₂Py]⁺, adopts a conformation where both the aromatic rings are twisted to the C11-C10-N3 reference plane. The anions (A) and the cations (C) consist of alternating layers (i.e., of type ···C₁A₁C₂A₂C₁A₁C₂···) along the c axis of the crystallographic unit cell.     

The structure of 20 oximo-5α-pregnano-16-eno[3,4-C]-1′,2′,5′-oxadiazole (HS976)

The crystal and the molecular structure of the steroidal oxadiazole 20-oximo-5-pregnano-16-eno[3,4-C]-1,2,5-oxadiazole (C₂₁H₂₈N₂O₃) has been determined by direct methods, and refined to a finalR of 0.086 for 3100 observed reflections. The compound crystallizes in space groupP2₁, with cell dimensionsa=18.284(6),b=13.992(4),c=7.370(3)Å,=96.97(3)°;V=1885 ų,Z=4,D _x =1.27 g cm^–3, =1.5418 Å, (CuK =5.95 cm^–1. The two independent molecules are related by a pseudo twofold axis. Both molecules exhibit similar overall topography, rings A, B, C, and D adopting distorted sofa, chair, chair, and distorted envelope conformations, respectively.     

Crystal and molecular structure of 2-(2′-chloro-5′-nitrostyryl)benzoselenazole

The title compound C₁₅H₉ClN₂O₂Se (nsbse) is orthorhombic, witha=6.823(2),b=7.860(2),c=26.349(5) Å,Z=4,D _x =1.709,(MoK)=28.3 cm^–1,F(000)=720,T=298K in space groupP2₁2₁2₁. The structure was solved by heavy atom and Fourier methods and refined toR=0.045 for 1095 unique observed reflections. The molecule is almost planar, with a dihedral angle of 4.8(2)° between the benzoselenazole and phenyl rings. The C-Se-C angle in the selenazole ring is very small, 84.6(4)°, while the C-N-C angle in that ring is 113.7(7)°.     

Crystal structure of 2-(1-o-xylen-4′-yl-2-hydroxy-5-oxo-benzo[c]pyrroline) carboxylic acid, C17H15NO4

The title compound crystallizes in the space group P2₁/c, with a = 8.555(2), b = 22.109(2), c = 16.768(2) Å, and = 90.25(2)°, with two independent molecules in the asymmetric unit, dissimilar only for the orientation of the xylenyl group. There is no conjugation between the pyrroline ring and the xylenyl group. The molecules in the asymmetric unit are enantiomers, thus constituting a racemic dimer. The molecules are linked in chains by hydrogen bonds.