Crystal structure of 4,6-dinitro-1-(5-tetrazolyl)-1H-indazole trihydrate

The title compound, C₈H₄N₈O₄·3H₂O, crystallizes in space groupP¯1 with cell constantsa=7.022(1),b=9.507(2),c=10.906(2) Å,=84.99(1),=71.89(1),=72.56(1)°,Z=2, andV _c =660.2 ų. The structure was solved by direct methods using diffractometer data and was refined by full-matrix least-squares methods to anR value of 0.060 for 2112 observed reflections. The molecule, consisting of a phenyl ring fused to a pyrazole ring with a tetrazole ring connected to it equatorially, is planar except for the N(7) nitro-group oxygen atoms. The structure is stabilized by a three-dimensional network of O-HO, O-HN, and N-HO hydrogen bonds through the water molecules.     

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.     

Studies of systemic acylanilide fungicides. Part IV. Crystal structure and molecular conformation ofN-(2-methoxyacetyl)-N-(2,6-xylyl)-α-amino-γ-butyrolactone

The crystal structure of the title compound (C₁₅H₁₉NO₄, MW 277.3 amu) was determined by three-dimensional X-ray analysis from diffractometer data. Crystal data are: monoclinic,P2₁/n,a=9.600(3) Å,b=11.964(6) Å,c=12.802(4) Å,=101.25(3)°,V=1442.1(16) ų,Z=4;D _x =1.277 Mg m^–3;(MoK)=0.10 mm^–1. FinalR=0.055 for 1686 observed reflections having 2 (MoK)<50° andI>2.5 (I). The compound is isostructural withN-(2-methoxyacetyl)-N-(2,6-xylyl)-3-amino-1,3-oxazolidin-2-one. The dimethylphenyl ring is almost perpendicular to the amidic plane of the molecule (dihedral angle 81.9°); the butyrolactone ring is in the typical envelope conformation.     

The crystal structure of 5-methyl-1-(octahydro-1-iodo-1H-1-inden-4-yl)-1H-tetrazole

The title compound is C₁₁H₁₇N₄I, F.W.=330.20, monoclinic, space groupP2₁/a,a=11.586(2),b=10.617(1),c=10.417(1) Å, =94.567(2)°,Z=4,F(000)=652, (MoK)=0.7107 Å, (MoK)=2.31 mm^–1,V=1277.31 Å₃,D _C=1.71 gcm^–3,D _m=1.70 gcm^–3. The structurewassolved by Patterson and Fourier methods and refined to anR value 0.031 for 1620 observed reflections. The connectivity and conformation of the addition product ofcis-1,5-cyclononadiene and iodine azide was determined by X-ray analysis. The reaction product contains a chair-conformation cyclohexane ring that iscis fused to a cyclopentane ring. The cyclopentane ring has an envelope conformation and an equatorially oriented iodine substituent. A planar tetrazole ring is axially substituted on the cyclohexane ring. The plane of the tetrazole ring makes a dihedral angle of 69.6° with the average plane of the carbon atoms of the cyclohexane ring.     

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 and crystal structure of Bi(mpo)3 (Hmpo = 2-mercaptopyridine N-oxide)

The synthesis as well as crystal and molecular structure of [Bi(C₅H₄NOS)₃] are reported. The complex crystallizes in the monoclinic system, space group P2₁/n with lattice parameters a = 9.6521(3) Å, b = 10.0659(4) Å, c = 18.4484(7) Å, = 102.13(6)°, and D _calc = 2.227 Mg · m^–3 for Z = 4. It is clear from the packing diagram that the title compound is a dimer via the secondary coordination. Surrounding Bi atom, three five-membered ring planes (Bi,O,N,C,S) make a dihedral angle of 55.91, 54.72, and 26.13° respectively. The whole crystal presents a three-dimensional network structure as each molecule produces four weak C–H O hydrogen bonds and a weak C–H S hydrogen bond.     

Structural and spectral studies of binuclear copper(II) 2-acetylpyridine 3-azacyclothiosemicarbazones with sulfato bridges

Structures of two binuclear copper(II) complexes with sulfato bridges and tridentate 2-acetylpyridine 3-azacyclothiosemicarbazone ligands have been solved. The complex-sulfato-bis{(2-acetylpyridine 3-hexamethyleneiminyl-thiosemicarbazonato)copper(II)} N,N-dimethylformamide, [Cu(Achexim)]₂SO₄·DMF, has the following structural properties: triclinic, P1¯(#2), a = 12.314(4), b = 15.885(4), c = 10.959(4) Å, = 103.25(2), = 103.60(2), = 109.94(2)°, V = 1843(2) ų, and Z = 2; for -sulfato-bis{(2-acetylpyridine 3-piperidylthiosemicarbazonato)copper(II)}chloroform, [Cu(Acpip)]₂SO₄·CHCl₃: triclinic, P1¯(#2), a = 11.657(1), b = 17.101(2), c = 10.338(1) Å, = 98.51(1), = 109.294(7), = 107.016(9)°, V = 1790.3(4) ų, and Z = 2. The size of the azacyclo ring significantly affects the stereochemistry of these binuclear complexes.     

Crystal structure of triphenylphosphine-(1-(di(trifluoromethyl)-hydroxymethyl)-cyclopentadienyl)-(1,2-di(carboxymethyl) ethylene-1-yl) ruthenium (0)

The structure of triphenylphosphine — (1 — (di(trifluoromethyl) — hydroxymethyl) — cyclopentadienyl) — (1,2 — di(carboxymethyl)ethylene — 1 — yl) — ruthenium (0) has been studied by single-crystal X-ray diffraction techniques. This compound, [C₅ H₄(CF₃)2 COH] Ru(PPh₃)C2(CO₂Me)₂H, crystallizes in the triclinic space groupP¯1 witha =10.131,b= 15.107,c= 10.798 Å, = 102.14, = 107.04, = 89.64° andZ = 2. The structure was refined by block-diagonal least-squares methods to a finalR value of 0.042, including hydrogen atoms. The compound contains a dicarboxymethylethylene ligand coordinated to ruthenium both through a ketonic oxygen and through a metal--carbon -bond. An intramolecular hydrogen bond is observed. Details of the structure are reported, and the structures of several Ru(0) complexes are compared.     

Synthesis and crystal structure of 4,5-(cis-cyclohexylenedithio)-1,3-dithiole-2-one

The x-ray crystal structure of 4,5-(cis-cyclohexylenedithio)-1,3-dithiole-2-one has been determined. Yellow block shaped crystals of C₉H₁₀OS₄ crystallize in the space group P with cell dimensions a = 8.872(4), b = 9.330(8), c = 14.333(12) Å, = 95.23(7), = 91.09(5), = 107.60(5)°, V = 1124.8(14) ų, and Z = 4. This compound has two S---S contacts [3.574, 3.610 Å] shorter than 3.70 Å and the usual disordered ethylene moiety [C(3)—C(8)] of the six-membered ring is fixed by the cis-cyclohexylene subsitituent. This means that it may be a new precursor for conducting and strong near-IR absorbing nickel-dithiolenes. Also, it provides the first example of polymorphism of the dmit derivatives and contains two independent molecules I and II in the asymmetric unit.     

Conformations of barbiturates related to pentobarbitone. II. Crystal structure oftrans-5-ethyl-5-(1′,3′-dimethylbut-1′-enyl) barbituric acid

Crystals oftrans-5-ethyl-5-(1,3-dimethylbut-1-enyl) barbituric acid (13M1TB), mp 183° C, are triclinic witha = 7.677(2),b = 10.393(3),c = 9.176(3) Å, = 104.331(1), = 106.919(1), = 96.494(1)°, space group P, with two molecules in the unit cell. The structure was solved by direct methods and refined by least-squares procedures toR = 0.050 for 2809 observed diffraction maxima. The 5-ethyl group is oriented under the barbiturate ring with the orientation of the but-1-enyl group directed away from the ring. This orientation is determined by the 1-methyl substituent. The molecules are linked together by N-H ... O=C hydrogen bonds across inversion centers, thus forming single ribbons alongb. Adjacent ribbons are held together in theac plane by van der Waals interactions between alternating ethyl and l,3-dimethylbut-l-enyl groups.     

Synthesis and X-ray structure of 3-(4-methyl phenyl)-2-(4-biphenyl)-1,3-thiazolidin-4-one

The title compound (C₂₂H₁₉NOS) was synthesized, characterized and structure was determined by X-ray diffraction method. It crystallizes in the monoclinic space group P2₁/c with cell parameters a = 22.181(2) Å, b = 6.0760(4) Å, c = 13.349(3) Å, = 95.615(3)^, and {Z = 4}. The final residual factor is 0.0625 for 1724 reflections with I > 2(I). 4-thiazolidinone ring moiety shows twisted conformation.     

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 oftrans-tetrachlorobis[2-(2-1H-imidazolyl)-1H-imidazolium]cadmium(II), [Cd(H3biim)2Cl4]

The reaction between cadmium(II) chloride and 2,2'-bi-1H-imidazole (H₂biim) in an acidic solution affords [Cd(H₃biim)₂Cl₄] (H₃biim=2-(2-1H-imidazolyl)-1H-imidazolium) in 63% yield. The compound crystallizes in the triclinic space groupP1, wherea=8.072(2),b=8.100(2),c=8.593(2) Å, =75.89(2), =62.94(2), =63.29(1)°,V=446.4(2) ų, andZ=1. The central Cd atom exhibits an octahedral geometry composed of a Cl₄N₂ core. The Cd-N bond distance is 2.392(2) Å. Cd–Cl distances are 2.5919(9) and 2.671(1) Å.     

4-(<Emphasis Type="Italic">E</Emphasis>)-2-[3-(3-[(<Emphasis Type="Italic">E</Emphasis>)-2-(4-cyanophenyl)-1-diazenyl]hexahydro-1-pyrimidinylmethyl)hexahydro-1-pyrimidinyl]-1diazenylbenzonitrile: X-ray crystal structure

4-(E)-2-[3-(3-[(E)-2-(4-cyanophenyl)-1-diazenyl]hexahydro-1-pyrimidinylmethyl)hexahydro-1-pyrimidinyl]-1-diazenylbenzonitrile (1) has been synthesized by reaction of p-cyanobenzene diazonium chloride with a mixture of formaldehyde and 1,3-propanediamine. The crystal structure has been determined by single crystal X-ray diffraction analysis. The bis-triazene (1) adopts a folded conformation, similar to previously studied ethylenediamine analogues, and there is evidence of -stacking in the crystal packing. The two planar phenyltriazenyl groups are almost parallel, forming an angle of 6.6(1), and display weak intermolecular s interactions between molecules. This result establishes the structure of the product of this diazonium coupling reaction as the 1-(1-hexahydropyimidinylmethyl)hexahydropyrimidine derivative and not the alternate tetraazabicyclo[5.5.1]tridecane derivative. Crystal data: 1C₂₃H₂₆N₁₀, monoclinic, space group P2₁/c, a = 10.717(1) Å, b = 7.749(1) Å, c = 28.252(2) Å, = 97.223(2), V = 2327.5(5) ų, for Z = 4.     

Crystal structure of dinitratotris(pyridine)nickel(II), Ni(NC5H5)3(NO3)2

Ni(NC₅H₅)₃(NO₃)₂ crystallizes in the triclinic space group P¯1 witha=8.432(2),b=9.993(2),c=12.181(3)Å, =69.78(2),=83.16(2), =67.73(1), andD _c =1.57 g cm^–3 forZ=2. The Ni²⁺ ion is six-coordinate with one bidentate and one monodentate nitrato ligand.     

Crystal structure of (diphenyl)(morpholino)phosphiniminocyclotrithiazene

The title compound (C₆H₅)₂(OC₄H₈N)P=N–S₃N₃ crystallizes in the space group with unit cell parametersa=9.3900(2),b=9.4747(1),c=11.3850(3) Å, =95.73(4), =96.85(6), =104.26(2)^o, and Z=2. The tricoordinated sulfur of the cyclotrithiazene ring deviates from the mean plane of other skeletal atoms by 0.683(4) Å. The angle at this atom is the smallest in the ring and is enclosed by the longest S–N bonds observed in the ring.     

The structure of 2-amino-3-cyano-4-(4-methylphenyl)-6-methoxyl-1,4,9,10-tetrahydrobenzo[<Emphasis Type="Italic">f</Emphasis>]chromene

The X-ray crystal structure of 2-amino-3-cyano-4-(4-methylphenyl)-6-methoxyl-1,4,9,10-tetrahydrobenzo [f]chromene 1, C₂₂H₂₀N₂O₂, is determined. The crystals of compound 1 are triclinic, space group P-1, a = 10.120(1), b = 13.127(1), c = 15.203(2) Å, = 67.841(9), = 80.81(1), = 77.58(1), Z = 4, V = 1819.7(4) ų. It is interesting that all the atoms of the pyran ring are coplanar, which is different from other similar compounds. The structure is stabilized by intermolecular hydrogen bonds.     

Synthesis, characterization, and crystal structure of 1-(4-chloro-benzoyl)-3-naphthalen-1-yl-thiourea

1-(4-Chloro-benzoyl)-3-naphthalen-1-yl-thiourea has been synthesized and characterized by elemental analysis, IR spectroscopy, and mass spectrometry. The crystal and molecular structure of the title compound has been determined from single crystal X-ray diffraction data. It crystallizes in the triclinic space group P-1, with a = 6.962(1) Å, b = 10.770(3) Å, c = 11.738(2) Å, = 65.76(2)°, = 80.03(1)°, = 84.86(2)°, and D _calc= 1.432 g cm^–1 for Z = 2. The thermal behavior of the compound has been studied by DTA and TG. The antibacterial activities of the title compound were investigated for three Gram (+) and two Gram (–) bacteria by employing broth microdilution method and subsequently, inhibitory activity against yeast-like fungi was also determined.     

Structure of bis(2-amino-5-methylpyridinium) tetrachlorozincate at 298 and 150 K

Reaction of 2-amino-5-methylpyridine with zinc chloride and HCl in aqueous solution yields bis(2-amino-5-methylpyridinium) tetrachlorozincate. The complex crystallizes in the monoclinic space group P2₁/c, with minimal tetrahedral distortion of the ZnCl₄ ^2– ion at both 298 and 150 K; at 298 K, a = 8.090(2) Å, b = 14.795(6) Å, c = 15.850(4) Å, = 101.93 (2); at 150 K, a = 8.0986(2) Å, b = 14.7190(5) Å, c = 15.7684(7) Å, = 102.862(2). The anisotropic cell contraction results in significant changes in nonbonding Cl Cl contacts.     

Structure of 2-{2-[3-methyl-3-(2,4,6-trimethylphenyl) cyclobutyl]-2-oxoethyl}isoindole-1,3-dione

2-{2-[3-Methyl-3-(2,4,6-trimethylphenyl)cyclobutyl]-2-oxoethyl}isoindole-1,3-dione (C₂₄ H₂₅NO₃) was synthesized, and its crystal structure was determined by X-ray crystallographic techniques. The compound crystallizes in the triclinic space group P-1, with unit cell parameters: a = 14.109(9) Å, b = 14.130(8) Å, c = 12.152(6) Å, = 105.62(5)°, = 113.75(4)°, = 98.78(5)°, V = 2039.8(19) ų, D _c= 1.223 g/cm³, and Z = 4. The crystal structure has two crystallographically independent molecules, I and II. These molecules are held together by weak intermolecular C—H···O interactions, forming a continuous chain. The dihedral angles between the N-substituted phthalimide moiety and cyclobutane ring in molecules I and II are 60.37(14) and 68.18(18)°, respectively.