1-(Ethoxymethyl)-6-(phenylselenyl)-5-ethyl uracil: a nucleoside analog

The compound, 1-(ethoxymethyl)-6-(phenylselenyl)-5-ethyl uracil, crystallizes in the monoclinic space group P2₁/n with unit cell parameters a = 5.304(1), b = 21.261(4), c = 13.996(4) Å, = 94.30(2)°, and Z = 4. The acyclic chain C1, O4, C4, C5 is in fully extended form and nearly perpendicular to the uracil base. The molecules are held together by van der Waal's forces.     

Synthesis and crystal structure of [ReOCl<Subscript>2</Subscript>(L)] (HL = 2-(1-ethanolaminomethyl)-1-methylimidazole)

The title compound was prepared from the reaction of (n-Bu₄N)[ReOCl₄] with the ligand HL in acetonitrile. The chelate L is coordinated as a terdentate uninegative N, N,O^–-donor ligand in a distorted octahedral coordination geometry around the rhenium(V) ion. The structure has a triclinic space group P-1 with a = 6.9796(3), b = 7.1530(3), c = 12.0416(6) Å, = 73.742(2), = 86.458(2), = 73.928(3), V = 554.50(4) ų, and Z = 2.     

Crystal structures of 1-(2-hydroxyphenyl)-3-phenyl-1,3-propanedione and 1-(1,3-benzodioxol-5-yl)-3-(2,4-dimethoxyphenyl)-1,3-propanedione

1-(2-Hydroxyphenyl)-3-phenyl-1,3-propanedione crystallizes in the triclinic space group (a=5.4233(5),b=13.910(1),c=17.036(1) Å, =68.311(6), =80.854(7), =78.760(8)°) as two independent enolic tautomers in which the hydroxyl and phenolic protons are hydrogen bonded to the ketonic oxygen atom. The structure was refined toR=0.039 for 2085I3(I) reflections. 1-(1,3-Benzodioxol-5-yl)-3-(2,4-dimethoxyphenyl)-1,3-propanedione, which belongs to the triclinic space group (a=7.3990(7),b=8.1239(5),c=14.004(1) Å, =86.673(6). =88.574(7), =64.885(7)°) also exists in the enolic form. The structure was refined toR=0.040 for 1564I3(I) reflections.     

Synthesis,characterization and crystal structure of oxovanadium(IV) complex with tridentate o-van-gly and bidentate phenanthroline

A novel oxovanadium(IV) complex with tridentate schiff base and bidentate phenanthroline ligands, VO(o-van)(phen) 2H₂O[o-van-gly: o-vanillin-glycine; phen: phenanthroline], was synthesized and characterized by elemental analysis, IR and UV-vis spectra. The crystal structure was determined by X-ray single crystal diffraction analysis. The crystal of title complex (C₂₂H₂₁N₃O₇V, M_w = 490.36) belongs to triclinic, space group P-1 with the following crystallographic parameters: a = 9.247(3) Å, b = 10.125(4) Å, c = 13.100(5) Å, = 106.343(6), = 96.042(7), = 101.726(7), V = 1135.0(7) ų, Z = 2, D_c = 1.435 Mg m^–3, (MoK = 0.485 mm^–1, F(000) = 506, and final R₁ = 0.0779, wR₂ = 0.1598 for observed reflections 1606 (I > 2(I)). V(IV) is six-coordinate with three oxygen atoms and three nitrogen atoms in a distorted octahedral geometry. The complex forms a 3-D network via – stacking and hydrogen bonds.     

Synthesis and structure of 4-R,5-R-[5-(hydroxy-diphenyl-methyl)-2, 2-dimethyl-[1,3]dioxolan-4-yl]-phenyl-methanone, a chiral ligand building block

A triphenyl analog of taddol, 4-R,5-R-[5-(hydroxy-diphenyl-methyl)-2,2-dimethyl-[1,3]dioxolan-4-yl]-phenyl-methanone, has been synthesized and structurally characterized. This molecule could act as a chiral ligand building block in the creation of tuned taddol analogs. Structural analysis of the title compound reveals that the hydroxyl group is involved in an intramolecular hydrogen bond and does not take part in any intermolecular interaction. Crystal packing is influenced by C–H O hydrogen bonding and phenyl phenyl interactions. Crystal data: Triclinic, P1 (No. 1), a = 5.9343(4) Å, b = 8.2367(17) Å, c = 10.987(2) Å, = 88.290(6), = 75.442(4), = 80.655(6), V = 512.86(15) ų, Z = 1, D _calc = 1.258 mg/m³. Final residual values were R ₁ = 0.0407 for 3022 observed data (I > 2s(I) ) and wR ₂ = 0.0941 for all 3524 unique data.     

Structure of (Z)-1-p-methoxyphenyltelluro-1,4-diphenyl but-1-en-3-yne

C₂₃H₁₈TeO,M _r=437.97, ,a=9.940(2),b=13.664(3),c=7.895(2) Å, =80.60(1), =69.71(2), =75.95(1)°,V=972.0(4) ų,Z=2,R=0.041 for 2668 observed reflections. The Te–C bond distances are 2.109(5)Å and the C–Te–C angle is 96.0(2)°. The phenyl rings are planar to within experimental accuracy, making dihedral angles of 64.6(2), 65.3(2) and 31.1(3)°.     

A comparison of the coordination preferences of Zn, Co, and Cd(II) with the heteroscorpionate ligand (2-hydroxy-3-t-butyl-methylphenyl)bis (3,5-dimethylpyrazolyl)methane

Reaction of the Zn, Cd, or Co nitrate salts with the deprotonated ligand (2-hydroxy-3-t-butyl-methylphenyl)bis(3,5-dimethylpyrazolyl)methane (L1O^–) in methanol produced the following complexes: [(L1OH)Zn(NO₃)₂] in two isomorphs, a = 40.983(8) Å, b = 9.571(2) Å, c = 15.667(8) Å, = 90, = 106.38(1), = 90, C2/c, and a = 13.027(3) Å, b = 14.781(4) Å, c = 16.107(3) Å, = 90, = 105.30(1), = 90, P2₁/n; [(L1OH)Cd(pz)(NO₃)₂] a = 14.7476(2) Å, b = 13.5411(2) Å, c = 16.7223(2) Å, = 90, = 110.3840(10), = 90, P2₁/c; and [(L1O)Co(pz)(NO₃)] a = 11.4240(2) Å, b = 13.4498(2) Å, c = 13.8056(2) Å, = 105.2080(10), = 105.8130(10), = 112.7470(10), P . The Zn adopts a pseudotetrahedral four-coordinate geometry where the potentially tridentate ligand is actually bidentate with a protonated and uncoordinated phenoxy arm. The Co complex is pseudooctahedral six-coordinate where the phenoxy arm is deprotonated and coordinated. Finally the Cd complex is seven-coordinate but the metal is not coordinated through the phenoxy group that is again protonated.     

Crystal structure ofcatena-O,O′-diethylphosphonoacetatotriphenyltin

Triphenyltin diethylphosphonoacetate, which crystallizes in the monoclinc space groupP2₁/c (a=15.154(4),b=9.159(3),c=17.685(4) Å, =91.410(8)°), adopts a polymeric structure in which planar triphenyltin cations (_C—Sn—C=357.3(6)°) are axially linked by the diethylphosphonoacetato anions (Sn–O_esteryl=2.129(3), SnO_phosphoryl=2.420(3) Å; O–SnO=171.9(1)° into chains that propagate by translations along theb-axis. The structure has been erfined toR=0.037 for 3384I3(I) reflections.     

Structural characterization and photophysical properties of a luminescent trinuclear zinc(II) complex exhibiting multiple coordination geometries

A luminescent trinuclear zinc(II) complex, tris(-2,3-toluenedithiolato)-1:2²S¹;1:2²S¹, 2:3²S²;3S², 1:3²S³;3S³-bis(2,2-bypyridine)-1²N,N,2²N,N-trizinc, containing 3,4-dimercaptotoluene (tdt) and 2,2-bipyridine (bpy) has been synthesized and found to have the trinuclear formulation Zn₃(tdt)₃(bpy)₂ (I). The complex crystallizes in the monoclinic space group P2₁/n with a = 11.7247(12), b = 20.134(2), c = 17.7376(18) Å and = 103.743(2). The complex has two heteroleptic zinc(II) centers exhibiting similar distorted trigonal bipyramidal geometries with the third homoleptic zinc(II) center displaying a flattened tetrahedral geometry. Present in the solid state are both intra- and intermolecular – interactions. The complex is emissive at 77 K in the solid state with an emission maximum at 574± 2 nm with a luminescence lifetime of 7.4± 0.4 ns. The unstructured emission is assigned as a metal-mediated ligand-to-ligand –^* charge transfer transition.     

Crystal and molecular structure of 1,1′,3,3′-tetraphenyloxaldiamidrazone

1,1,3,3-Tetraphenyloxaldiamidrazone, C₂₆H₂₄N₆, crystallizes in the monoclinic system: space groupP2₁/c,a= 13.946(1) Å,b= 5.706(1) Å,c= 17.109(1) Å, = 125.31(1) °,D _m = 1.254,D _c = 1.259 gcm^–3 andZ= 2. Intensities were obtained from –2 scans with a Syntex automated diffractometer using graphite-monochromated MoK radiation. The structure was solved by direct methods. Full-matrix least-squares refinement of all positional and thermal (anisotropic for the nonhydrogen atoms and isotropic for the hydrogen atoms) parameters using 2022 reflections [I>2(itI)] converged at a conventionalR of 0.041. The molecule is characterized by a conjugated pi system which includes the central N=C–C=N moiety and two of the four aniline groups. No intermolecular and only weak intramolecular hydrogen bonds are present.     

Caging the mercurous ion: a tetradentate tripodal nitrogen ligand enhances stability and J(1H199Hg)

The dimeric mercurous ion has been encapsulated by a pair of the tetradentate tripodal nitrogen ligands tris[(2-(6-methylpyridyl))methyl]amine (TLA). The complex [Hg₂(TLA)₂](ClO₄)₂ (1) was isolated directly from an acetonitrile solution of Hg(ClO₄)₂ 3H₂O and TLA. Complex 1 crystallizes in the triclinic space group with a = 10.537(2) Å, b = 10.751(2) Å, c = 10.907(2) Å, = 75.20(3), = 73.73(3), = 75.73(3), and Z = 1. The cation is located an inversion center. The Hg–Hg and Hg–N_amine bond distances are 2.5469(8) and 2.297(6) Å, respectively, and the average Hg–N_pyridyl bond length is 2.75(7) Å. Complex 1 was stable indefinitely in acetonitrile-d ₃ solution, permitting detection of 13 and 22 Hz heteronuclear couplings between the Hg(I) ions and the methylene protons of the ligand. Comparisons with the structures and spectroscopic properties of related mercuric and mercurous complexes are made.     

Crystal and molecular structure of rac(1R,5S,6S,7R)-1-oxy-7-benzoyl-5-methyl-8-azabicyclo-[4.3.0]nonane-4,9-dione,C16H17NO4 (perhydroindole)

The structure of the title compound (perhydroindole) was determined by X-rays, using CuK radiation (graphite-crystal monochromator,=1.54184 Å): T=290 K., C₁₆H₁₇NO₄,M _r =287.31 monoclinic, space groupC2/c,a= 14.471(1),b=6.169(2),c=32.065(2) Å,=92.192(6)V _c =2860,6 ų,Z=8,D inx=1.338 Mg m^–3, (CuK)=7.54 cm^–1. Final conventionalR-factor=0.048, (R _w =0.072) for 2513 unique reflections and 258 variables. The structure was solved usingMultan. The six-membered ring of the molecule is in the chair configuration. The molecules are connected by hydrogen bonds.     

Choline sodium 4-amino-1-β-d-ribofuranosyl-2-(1H)-pyrimidionone diphosphate tetrahydrate (Sodium cytidine diphosphocholine,C14H33N4NaO15P2)

This communication presents a preliminary report on the crystal structure of this important nucleotide, involved in lecithin synthesis in animal tissues. The crystallographic data were recorded using a four-circle diffractometer with Cu-K x-radiation. Crystal data: orthorhombic, space groupP2₁2₁2₁ (No. 19),Z = 4,a = 6.98 pm,b = 123.6 pm,c = 292.3 pm,U = 2.522 nm³. The structure was solved by means of a Patterson and electron-density maps and refined by several cycles of least-squares using isotropic temperature factors toR = 0.14.The torsion angles associated with the furanosyl ring are, in general, at the very extreme of the range commonly observed for C(2) endopuckering (Altona and Sundaralingam, 1972); their values are 1 = 319 °, 2 = 47 °, 3 = 326 °, 4 = 13 °, 5 = 18 °. The phase angle of pseudorotation, calculated from these values using the formula given by Altona and Sundaralingam (1972) is 139 °. This shows the ribose ring to be slightly nearer to the C(1) exopuckering than the C(2) endopuckering conformation, but remote from being a C(3) endo-conformer. The sugar ring, in fact, is very close to being an idealized twist conformer. This is supported by a four-atom least-squares planes study, and is consistent with the high value of 237 ° (Sundaralingam, 1973).Backbone torsion angles associated with the structure are = 57 °, = 133 °, = 174 °, and = 291 °. is some 7 ° less than the preferred minimum value for C(2) endopuckering.     

Crystal structure of 6-nitrobenzo(a)pyrene

In 6-nitrobenzo(a)pyrene, an environmental pollutant, the nitro substituent lies at 69.5(1) to the mean plane of the aromatic moiety. The C–C bond distances range from 1.341(3) to 1.443(3) Å. The crystal is in the monoclinic space group, P2₁/c, with a = 8.3239(3) Å, b = 8.9530(3) Å, c = 18.0678(5) Å, = 99.264(2) and Z = 4. Molecules are assembled in sheets in the unit cell through stacking and alternating C–H O interactions.     

Synthesis and crystal structure of a cobalt(II) complex with tris(1-pyrazolylmethyl)amine

The synthesis of a cobalt(II) complex of tris(1-pyrazolylmethyl)amine (amtp) is reported. The complex [Co(amtp)Cl](BPh₄) crystallizes in the space group P-1, with a = 8.979(2), b = 19.329(3), c = 20.251(3) Å, = 93.321(2), = 93.685(3), = 98.930(2)°, and Z = 4. The Co(II) atom is nearly tetrahedrally coordinated by three pyrazole N-atoms and one Cl^–. The tertiary amine N-atom of amtp is only weakly coordinated to Co(II) atom at a Co—N(amine) distance of ca 2.40 Å.     

Crystal and molecular structure of pyridinium di-μ-oxo-bis(oxodichloroaquomolybdate(V)) monohydrate, (pyh)2[Mo2O4Cl4(H2O)2] · H2O

The crystal and molecular structure of pyridinium di--oxo-bis(oxodichloroaquomolybdate(V)) monohydrate has been determined from MoK diffractometer data. The compound crystallizes in the monoclinic space groupP2 ₁/m witha = 7.544(1),b= 17.046(3),c = 7.894(1) Å, = 106.00(1) ° andZ = 2. The structure was solved by the heavy-atom technique and refined by full-matrix least-squares method toR = 0.046, using 1800 reflections for whichF> 4(F). Molybdenum atoms are linked by the double oxygen bridge with an Mo—O distance of 1.943(4) Å and an Mo—O—Mo angle of 83.4(2) °. The Mo—Mo distance is 2.584(1) Å, indicating direct Mo—Mo bonding. The pyridinium and [Mo₂O₄C1₄(H₂O)₂]^2- ions are hydrogen bonded through N—H ... O bonds. The N ... O contact is 2.656(8) Å.     

Synthesis and X-ray structure analysis of 2-acetylamino-benzoic acid

The title compound crystallizes in the orthorhombic space group Fdd2 with unit cell parameters a = 10.848(1) Å, b = 30.264(1) Å and c = 10.577(1) Å, V = 3472.47(2) ų, and Z = 4. The final reliability index is 0.030 for 700 observed reflections. Nitrogen of the amide group and carbon atom of the acid group deviate significantly below and above the plane of the phenyl ring. The crystal cohesion is accentuated by N—HO and O—HO hydrogen bonds.     

Structural characterization of 2,6-bis(N-methylenepiperidino)-4-nitrophenol (MPN) and 2,6-bis-(N-methylenemorpholino)-4-nitrophenol (MMN)3

MPN: C₁₈H₂₇N₃O₃,M _r=333.43, monoclinic,P2₁/n. a=6.207(2),b=21.893(6),c=13.693(3) Å; =96.12(2)^o,V=1850.1(8) ų.,Z=4,D _cal=1.20 mg/m³,F(000)=720, (CuK)=1.5418 Å, andT=298K.R=0.042 andwR=0.049 for 1675 observed reflections. MMN: C₁₆H₂₃N₃O₅,M _r=337.38, triclinic,P,a=9.642(1) Å,b=10.123(5) Å,c=9.341(2) Å, =93.00(3)^o, =90.96(1)^o, =110.46(1)^o, V=852.5(5) ų,D _cal=1.31 mg m^–3.F(000)=360,Z=2, (CuK)=1.5418 Å,R=0.054 andwR=0.074 for 2804 observed reflections. The piperidine and morpholino rings assumechair conformation and orient each other at an angle of 44.8(1)^o (MPN) and 47.1(1)^o (MMN), respectively.Contribution No. 827 from DCB.     

Crystal structure of 751-1751-1751-1751-2751-2751-2

The title compound crystallizes in the centrosymmetric triclinic space group (No. 2) witha=10.818(1)Å,b=10.876(1)Å,c=11.072(2)Å, =98.74(1)°, =98.83(1)°, =96.61(1)°,V=125906(3)ų andZ=2. Interatomic distances include Fe–P=2.243(2)Å, Fe–CO=1.771(6)–1.781(5)Å, Fe–C(C₅H₅)=2.074(6)–2.103(5)Å and P–F=1.511(6)–1.571(4)Å.     

Low-temperature,high-resolution crystal structure study of tricyclo[3.3.1.13,7]decan-2-ol (adamantanol-2)

The structure of the title compound (C₁₀H₁₅OH) was determined by X-ray diffraction at liquid nitrogen temperature. The crystals are triclinic, spacegroupP¯1 witha=11.3686(5),b=11.3990(5),c=11.4353(6) Å,=82.193(4),=70.211(4) and =62.279(4)°,V _c =1233.9(1) ų,Z=6,F(000)=504,D _x =1.229 g cm^–3; MoK radiation, =0.71073 Å,(MoK)=0.7 cm^–1. FinalR factor=0.046 andwR=0.062 for 8162 reflections withI>2.5(I). The asymmetric unit consists of three independent adamantanol-2 molecules which together with the three symmetry-related molecules form a cluster having pseudo ¯3 symmetry. The six molecules in the cluster are connected by six O-HO hydrogen bonds, the oxygens of which constitute an almost ideal chair conformation.