Crystal and molecular structure of the (−)-N-hydroxyimide of (10-pinene-2-yl) succinimic acid

Two independent molecules in the unit cell are the same enantiomer of the title compound but possess slightly different conformations. Both conformers are joined by H-bonds to one water molecule. The configuration at C11 was established asR.Crystal data: C₁₄H₁₉O₃N×1/2H₂O; trigonal,P3₂;a=17.486(2),b=17.486(2),c=8.024(1)Å;V=2124.72(6)ų;Z=6; (CuK)=1.54178 Å;F(000)=834; finalR=0.0495 for 2376 reflections (of 2747 unique data).     

Crystal and molecular structures of three 2,2′-thio- and 2,2′-sulfonyl-bis(1,3-diarylprop-2-en-1-ones)

The X-ray crystal structures of 2,2-thio- and 2,2-sulfonylbis(1,3-diarylprop-2-en-1-ones) are determined [1: 2,2-thiobis(3-(p-chlorophenyl)-1-phenylprop-2-en-1-one), C₃₀H₂₀Cl₂O₂S, space group C2/c, a = 14.275(3), b = 6.280(1), c = 26.533(5) Å, = 94.55(3)°, Z = 1/2; 2: 2,2-sulfonylbis(1,3-diphenylprop-2-en-1-one), C₃₀H₂₂O₄S, space group P , a = 9.652(1), b = 12.044(1), c = 12.182(1) Å, = 61.985(6), = 77.511(5), = 74.340(6)°, Z = 1; 3: 2,2-sulfonylbis(3-(p-chlorophenyl)-1-phenylprop-2-en-1-one), C₃₀H₂₀Cl₂O₄S, space group P , a = 8.294(1), b = 13.175(2), c = 13.470(1) Å, = 62.870(9), = 83.796(7), = 85.282(8)°, Z = 1]. The C=C double bonds are all clearly defined. The sulfide 1 crystallizes on a crystallographic twofold axis, leading to a symmetric molecular conformation. The sulfones 2 and 3 crystallize on general positions, with different and irregular conformations.     

Crystal and molecular structure of (±)-1-phenyl-2-amino-1-propanol,C9H13NO

The crystal structure of (±)-phenylpropanolamine has been determined by single-crystal X-ray diffraction methods. The structure was solved by direct methods and refined by least-squares toR=0.055 andR _w=0.045 for 2000 reflections (I2 (I)). The molecule was found to adoptgauche geometry. Inter- and intramolecular N-HO and O-HN hydrogen bonds were observed in the crystal structure.     

Crystal and molecular structures of 11,12-epoxydrim-8(9)-en-11β-ol-7-one

The crystal structure of 11,12-epoxydrim-8(9)-en-11β-ol-7-one is determined by X-ray diffraction. The crystal data for the C₁₅H₂₂O₃ composition are as follows: a = 6.646(1) Å, b = 7.242(1) Å, c = 7.635(2) Å, α = 84.34(3)°, β = 84.50(3)°, γ = 69.84(3)°, space group P1, and Z = 1. The structure is solved by the direct method and refined in the anisotropic approximation to R = 0.043 and R _w = 0.110. The stereochemical formula of the compound is determined. It is shown that the hydroxyl group at the C(11) atom is situated at the β position. In the crystal, the molecules related by the translation along the a-b direction of the unit cell are linked into infinite chains by intermolecular hydrogen bonds between the hydrohyl group and the carbonyl oxygen atom [O-H?O, 2.867(4) Å].     

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 and molecular structure of calcium L(–)-malate trihydrate

The new crystal and molecular structures of a less common hydrated calcium L(–)-malate (calcium (2S) 2-hydroxybutanedioate trihydrate) Ca(C₄H₄O₅)3H₂O, are reported. X-ray crystallographic data are as follows: a = 6.6460(3) Å, b = 8.3795(3) Å, c = 8.2707(4) Å, = 112.640(2)°, V = 425.1(4) ų, space group P2₁ (No. 4), Z = 2, D _calc = 1.767 g cm^–3. The calcium ion coordination number is seven. One of the three water molecules present in the unit cell is less strongly bound, only interacting with a calcium ion. In aqueous or hydroalcoholic solution, both di- and trihydrated species crystallize simultaneously.     

Crystal and molecular structure of the H-bonded complex between 1-chloro-2-hydroxynaphthalene-3-carboxylic acid and dimethylformamide (1∶1)

Crystal structure determination of the title complex reveals that the dimethylformamide solvent is bound to the carboxylic function of the hydroxy acid, in the form of a 7-membered hydrogen-bonded loop involving both the expected O-HO and an apparently weak C-HO interaction between host and guest. There is a strong intramolecular hydrogen bond between the phenolic OH and the carbonyl oxygen. Close packing of the complex units is afforded by a herringbone type alignment of host molecules.     

Crystal and molecular structure of 2′,4′-dimethoxyflavone

C₁₇H₁₄O₄,M _r =282.3, triclinic,P-1,a=8.469(3),b=8.516(2),c=20.425(8)Å,=84.95(3),=81.98(3), =70.47(2)°,V=1373(13)ų,Z=4,D _x =1.365 g cm^–3, (MoK )=0.71069 Å,=0.91 cm^–1,F(000)=592,T=294K,R=0.038 for 3577 observed reflections (F>3 (F)). The asymmetric unit is composed of two molecules. These two molecules, which are in planar conformations, differ in 4-methoxyl group orientation. Short intramolecular contacts are found between the -benzopyran portion and the dimethoxyphenyl ring.     

Crystal and molecular structure of aN(2)-benzyl-1,3-disubstituted-1,2,3,4-tetrahydro-β-carboline

(1R,3S)-2-Benzyl-3-methoxycarbonyl-1-methylcarboxymethyl-1,2,3,4-tetrahydro-9H-pyrido [3,4-b] indole, C₂₃H₂₄N₂O₄, was synthesized by a modified Pictet-Spengler reaction, and its crystal and molecular structure determined by single crystal X-ray diffraction methods. The crystals are monoclinic:P2₁ (No. 4),a=11.336(1),b=8.919(1),c=10.314(1)Å,=100.81(1)°,Z=2. The structure has been solved by direct methods, and refined toR=0.041 for 2203 observed reflections. The six-membered heterocyclic ring is in a half-chair conformation, and the substituents at C(3) and C(5) occupy axial and equatorial positions respectively. The CH₂Ph group attached to N(4) is in the generally less favoured axial position. The nitrogen atom of the indole system forms an intermolecular hydrogen bond with the carbonyl oxygen of the CH₂CO₂ Me group, the NO distance being 2.995(3)Å.     

Crystal and molecular structure of β-resorcylidene aminoguanidine copper(II) complex

The tridentate Schiff base, -resorcylidene aminoguanidine (RAG)1 was synthesized from 2,4-dihydroxybenzaldehyde and aminoguanidine and complexed with copper(II) to form a copper(II)--resorcylidene aminoguanidine (Cu-RAG)2 complex. X-ray diffraction analysis of compound2 (orthorhombic, Pnma,a=11.674(1);b=6.7198(7);c=17.836(2) ) revealed a square-planar copper(II) cation with a tridentate·ligand bound through two nitrogen atoms (N1 and N3) of the aminoguanidine moiety and an oxygen (O1) of the monodeprotonated dihydroxybenzaldehyde function. The remaining coordination site was occupied by chloride and the structure was rigidly planar as demanded by the restrictions of the crystallographic space group. The unit cell contents exhibited an extended sheet-like structure constructed via hydrogen bonds both intermolecularly and involving two water molecules (O3 and O4) also restricted by the same mirror symmetry. The remaining water (O5) provided for interlayer hydrogen bonding.     

Crystal and molecular structure of 1-chloro-1,2-benziodoxolin-3(1H)-one·tetra-n-butylammonium chloride

The title compound,6, a novel 11 complex of 1-chloro-1,2-benziodoxolin-3(1H)-one (5) andtetra-n-butylammonium chloride, was prepared from tetra-n-butylammoniumo-iodoxybenzoate (7) and acetyl chloride. A single crystal of6 was subjected to X-ray analysis: triclinic, space group a=10.239(2),b=11.518(2),c=11.523(3)Å; =73.20(2); =87.85(2), =87.72(2)°; R1=0.0326. The most notable structural feature of crystalline6 is the existence of a secondary bond [I· ·Cl(2), 2.943(1)Å] between the chloride ion and the iodine atom of the chlorobenziodoxolinone moiety. Further coordination at iodine includes three primary bonds: I–C [2.115(4) Å], I–O [2.145(3) Å], I–Cl(1) [2.454(1) Å]. The entire 1-chlorobenziodoxolinone-chloride sub-structure is planar and exhibits iodine-centered bond angles of 78.8(1)° [C–I–O], 92.0(1)° [C–I–Cl(1)], 97.6(1)° [Cl(2)–I–O] and 91.6(1)° [Cl(2)–I–Cl(1)]. The unit cell of6 contains two loosely packed formula units. The chlorobenziodoxolinone-chloride sub-structures occupy a common plane and exhibit a centrosymmetric relationship, while the tetra-n-butylammonium ions are situated one above and one below the plane. Bonding at the iodine atom in6 is more consistent with a 10-I-3 species electrostatically associated with the chloride ion than a 12-I-4 species such as the tetrachloroiodate ion.     

Crystal and molecular structure of [Cu2(3,5-dihydroxybenzoate)4 (acetonitrile)2] ⋅ 8H2O

The crystal and molecular structure of the title compound, [Cu₂(3,5-dihydroxybenzoate)₄ (acetonitrile)₂] 8H₂O 1, is reported. Crystal data for 1: tetragonal, space group I 4/m, a = 11.720(2) Å, c = 15.304(3) Å, V = 2102.4(6), and D _c = 1.53 g/cm³, for Z = 2. The metal and organic components crystallize to form a Cu paddle-wheel complex, of idealized D_4h symmetry, that assembles in the solid-state, along with eight equivalents of water, to form a 3D hydrogen-bonded network held together by O–H O hydrogens bonds. The metal complexes pack to form a 2D layered structure.     

Crystal and molecular structure of 1,1′-ferrocene-dicarbaldehyde

The crystal and molecular structure of 1,1-ferrocene-dicarbaldehyde 1 is reported. Crystal data for 1: monoclinic, space group P2₁/n, a = 5.876(1), b = 11.349(1), c = 29.460(3) Å, = 95.067(2)°, V = 1956.9(3) ų, and D _c = 1.64 g/cm³, for Z = 8. The complex crystallizes such that two molecules are located in the asymmetric unit in which the complexes display different degrees of twisting of the cyclopentadienyl (Cp) rings and formyl substituents about the Cp—Fe—Cp and Cp—COH axes, respectively. The molecule self-assembles in the solid state to form a 2D layered structure held together by - interactions and C—H···O hydrogen bonds.     

Crystal and molecular structure of aquabis(2,2′-bipyridine)nitratomanganese(II) nitrate monohydrate

A new monomeric manganese(II) nitrate complex with 2,2-bipyridine (bpy), [Mn(bpy)₂(NO₃)(H₂O)](NO₃)·H₂O, has been prepared and characterized by X-ray crystallography. The complex crystallizes in the triclinic space group witha=9.721(3),b=14.691(5),c=8.578(3) Å, =106.79(3), =96.05(3), =82.55(3)°,V=1159.9 ų andZ=2. The structure comprises discrete cation [Mn(bpy)₂(NO₃)(H₂O)]⁺ in which the metal atom is coordinated by a pair of bidentate bpy ligands [Mn–N=2.261(4)–2.299(4) Å], a unidentate nitrato [Mn–O=2.284(4) Å] and aqua [Mn–O=2.160(3) Å] ligands in a highly distorted octahedral arrangement.     

Crystal and molecular structure of 4-(3-indolyl)butyric acid-picric acid 2/2 π complex

The title compound, IBA-PIC, is 2C₁₂H₁₃NO₂·2C₆H₃N₃O₇, triclinic,P¯1,a=7.137(1),b=15.355(4),c=18.282(5) Å,=79.72(2),=79.85(2), =76.87(2)°. The structure was solved by direct methods and refined by least-squares techniques to anR factor of 0.068 for 3395 observed reflections. The IBA-PIC complex occurs as two independent molecules with different conformations. The crystallographic evidence for a prominent overlapping between the phenyl and indole rings corroborates earlier conclusions from UV spectroscopy. Molecules of both IBA and picric acid lie approximately parallel to (100) in layers and -bonding interactions across the 3.55 Å spacing. The angles between the indole ring and carboxyl-group planes are 82.9 and 86.9° for the A and B molecules, respectively.     

Crystal and molecular structure of dipotassium-aquapentachlororhodate (III): (K2)++ [RhCl5(H2O)]2−

The structure of K₂[RhCl₅(H₂O)] has been established by X-ray crystallography. It crystallizes in the orthorhombic space groupPcmn, with cell dimensionsa=7.065(1),b=9.453(1),c=13.567(1) Å,V=906.1(3) ų,Z=4,M _r =376.4,D _x =2.76 g cm^–3,F(000)=712,T=293 K. The final wasR=0.046. The rhodium atom has a distorted octahedral coordination involving five chlorine atoms and an oxygen of the water molecule with Rh, O, and three chlorine atoms on the mirror plane. Rh-Cl distances range from 2.284(7) Å to 2.345(7) Å. The Cl(4)O intermolecular distance, 3.140(12) Å indicates strong hydrogen bonding between oxygen and chlorine atoms of the neighboring octahedra.N. C. L. Communication No. 5353.     

Crystal and molecular structures of the 4-(1H)-pyridone (=L) lanthanide complexes {[GdL(NO3)3(H2O)]·CH3OH}2 and [DyL4(NO3)2](NO3) and of L2HNO3

The crystal structures of the title compounds have been determined by single crystal diffraction methods. Crystals of the dysprosium compound are monoclinic, space groupP2₁/c witha=14.133(4),b=13.438(5),c=14.401 (4)Å,=103.98(2)°,V=2654(1)ų,Z=4,D _c =1.82 g cm^–3, finalR=0.035. The Dy atom is eight-coordinate with a distorted dodecahedral coordination geometry involving two bidentate nitrate groups and four pyridone oxygen atoms. An erbium complex with analogous stoichiometry was also prepared but not structurally characterized. Crystals of the Gd compound are monoclinic, space groupP2₁/n, witha=11.226(2),b=9.075(2),c=16.737(3)Å,=93.88(3)°,V=1701(1)ų,Z=2,D _c =1.91 g cm^–3, finalR=0.042. Each Gd atom is bonded to one pyridone oxygen atom, a water molecule and three bidentate nitrate groups. An oxygen atom of one of the bidentate nitrates additionally serves to bridge pairs of Gd atoms so as to form a dinuclear complex in which each Gd atom is nine-coordinate with a tricapped trigonal prismatic geometry. Crystals of L₂HNO₃ are monoclinic, space groupI2/a witha=12.479(4),b=6.535(2),c=14.297(6)Å,=96.07(3)°,V=1159(1)ų,Z=4,D _c =1.45 g cm^–3, finalR=0.057. The pyridones are linked in pairs by very short (2.44 Å) symmetrical OHO hydrogen bonds. Each pair is further linked via a nitrate ion by means of N-HO(nitrate)H-N hydrogen bonds, so as to form an extended chevron-like pyridone-pyridone-nitrate-pyridone-pyridone array. Adjacent chains are linked via weak C-HO(NO₃) interactions.     

Crystal and molecular structures of 1,4-dihydro-6-methyl-5-N,N-diethylcarbamoyl-4-phenyl-2(3H)-pyrimidinethione (1) and 1,4-dihydro-6-methyl-5-N-methyl carbamoyl-4-(2′-nitrophenyl)-2(3H)-pyrimidinethione hemihydrate (2)

The crystal structure of 1,4-dihydro-6-methyl-5-N,N-diethylcarbamoyl-4-phenyl-2(3H)-pyrimidinethione, C₁₆ H ₂₁ N ₃OS (1), is monoclinic, space group P2₁/n, a = 6.818(1), b = 13.211(2), c = 18.807(3) Å, = 99.53(1)°, V = 1670.6(4) ų, Z = 4 and d _cal = 1.206 Mg/m³, R = 0.042 (wR = 0.119) for 190 parameters and 2560 observations with I 2(I) and 1,4-dihydro-6-methyl-5-N-methyl carbamoyl-4-(2-nitrophenyl)-2(3H)-pyrimidinethione hemihydrate, C₁₃ H ₁₄N₄O₃S 0.5H₂O, (2), is triclinic, space group P1, a = 7.513(1), b = 14.381(2), c = 15.506(2)Å, = 114.95(2), = 98.11(1), = 93.55(1)°, V = 1490.0(3) ų, Z = 4 and d _cal = 1.406 Mg/m³, R = 0.062 (wR = 0.165) for 388 parameters and 3094 observations with I 2(I).The compound 2 crystallized having two molecules in the asymmetric unit, which can be regarded as monohydrated dimers, and forming a hydrate. The conformation of the central heterocyclic ring (1,4-dihydropyrimidine) in both compounds was found to be close to a half-chair conformation. The 2-nitrophenyl substituent in 2 is in the axial synperiplanar orientation. In both compounds, the conformation of the 3-substituted carbamoyl group appears to be influenced by hydrogen bonding with anticlinal orientation observed for carbonyl groups serving as hydrogen bonding acceptors.     

Crystal and molecular structure of the photocatalyst tris(2,2′-bipyrazine)ruthenium(II) hexafluorophosphate

The X-ray structure determination of the complex tris(2,2-bipyrazine)ruthenium(II) hexafluorophosphate, [Ru(C₈N₄H₆)₃](PF₆)₂, has shown that the compound crystallizes in the monoclinic space group P2₁/c witha=13.459(5),b=23.486(8),c=17.913(10) Å,=139.85(1)°, andZ=4. Each asymmetric unit also contains one dimethylformamide and one water molecule. Least-squares refinement led to an R factor of 0.074 based on 3463 reflections for which I>2(I). The [Ru(C₈N₄H₆)₃]²⁺ cation has no crystallographic symmetry, but the requirements for point symmetry 32 are nearly met. The six Ru-N bond lengths agree within experimental error and have an average length of 2.05(1) Å.     

Crystal and molecular structure of 17-β-methyllupanineN(16)-oxide perchlorate hemihydrate

[C₁₆H₂₇N₂O₂]⁺·C1O ₄ ^– ·1/2H₂O,M _r =387.86, is monoclinic:P2₁,a=8.934(1),b=14.625(1),c=14.449(1) Å, =103.03(1)°,V _c =1839.3(2) ų,Z=4,D _x =1.40(1) g cm^–3, (CuK)=1.54178 Å,(CuK)=20.29 cm^–1,F(000)=808 e,T=292K,R=0.057 for 3428 observed reflections. Two independent cations are connected into chains along [101] by short hydrogen bonds between their oxygen atoms O(C2) and O(N16); distances, 2.607(5) and 2.625(5) Å. The water molecule has short contacts with the two independent perchlorate anions, which indicates that the anions are linked by weak hydrogen bonds utilizing the water molecule. The conformations of the two independent cations are similar and can be described as distorted half-chair, chair, distorted boat, and chair for ringsA, B, C, andD, respectively. Except for the flexible ringA, few changes in conformation of the cations are observed in comparison to the cations of lupanineN(16)-oxide perchlorate or 17--meth-yllupanine perchlorate.