Crystal and molecular structure of 4-p-hydroxyphenyl-2,2,4-trimethylthiachroman-1,1-dioxide

The title compound1 crystallizes as colorless polyhedra in the monoclinic polar space groupCc, witha=8.107(2),b=21.577(3),c=9.542(2)Å,=103.58(2)°, by contrast with its thioether precursor3, crystals of which have the trigonal space groupR¯3. The structure comprises infinite chains of molecules linked head-to-tail by S=OHO hydrogen bonds of length 2.723(2)Å, with HO contact 1.97(4)Å and O-HO 177(3)°; HÔ=S 146(1)°.     

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.     

Structure of dichloro[(2,4-dimethyl-5-oxo-2,3,4,5-tetrahydro-2-furyl)methyl]-(4-methoxyphenyl)tellurium(IV)

The crystal structure of TeCl₂(C₇H₇O)(C₇H₁₁O₂) has been determined from three dimensional, single crystal X-ray diffraction data. It crystallizes in the monoclinic space group C2/c with the lattice constantsa=24.551(5),b=11.435(2),c=12.368(2)Å,=97.33(1)° andZ=8,D _X=1.67 g cm^–3. Final least-squares refinement based on 3023 independent observed reflections yieldedR=0.026. The Te^iv ion is in a trigonal bipyramidal configuration with its lone pair of electrons at one of the equatorial positions. Distances and angles are: Te-Cl=2.495(1), 2.517(1); Te-C=2.134(3), 2.106(3)(aryl)Å; Cl-Te-Cl=173.45(4), Cl-Te-C=88.11(9), 88.60(9), 88.72(9), 86.06(9); C-Te-C=96.5(1)°. There are two secondary bonds to the tellurium: TeCl=3.824(1) and TeO(2)=3.006(1)Å. The methyl group to the carbonyl oxygen and the aryltelluro moiety exhibit atrans 2,4 relationship.     

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.     

Synthesis and structure of (H2O·HBF4)2(18-crown-6)

The title compound has been prepared by the addition of fluoroboric acid to 18-crown-6 in toluene. The compound crystallizes in the triclinic space group P¯1 witha=7.341(2),b=8.364(2),c=10.631(3)Å,=71.48(2),=67.91(2), =67.94(2)°, andD _c =1.44 g cm^–3 forZ=1. The final conventionalR value was 0.079 based on 1575 observed reflections. The molecule resides on a center of inversion. The (H₂O·HBF₄) moieties are best viewed as fluoroboric acid monohydrate molecules hydrogen bonded to the crown ether, one above and one below the plane of the crown. The FO(water) hydrogen bond separation is 2.474(5)Å, and the O(crown)O(water) separations are 2.834(5) and 2.841(6) Å. The oxygen atoms of the crown ether are planar to 0.23 Å.     

Crystal and molecular structure of (+)-6,7∶8,9∶10,11-tri-O-isopropylidene-2,3-dideoxy-d-arabino-l-allo-undec-2-enono-1,4-lactone,C20H30O9

The crystal structure of the title lactone, C₂₀H₃₀O₉, a potential precursor of uncommon 11-carbon sugar derivatives, has been determined by single-crystal diffraction methods. The compound crystallizes in the orthorhombic space groupP2₁2₁2₁ witha=15.581(3),b=14.047(2),c=9.888(2) Å, andZ=4. The structure was solved by direct methods and refined by full-matrix least-squares toR=0.054. The absolute configuration of the seven stereogenic carbon atoms was deduced as 4R, 5R, 6R, 7R, 8S, 9R, 10R, being (R)-(+)-glyceraldehyde its progenitor. An intramolecular O-HO hydrogen bond is present. Weak interaction C-HO links the molecules in sheets parallel to the (100) plane.     

Crystal and molecular structure of glycinehydroxamic acid

Glycinehydroxamic acid, C₂H₆N₂O₂ (NH₂CH₂C(O)NHOH), was synthesized and its crystal and molecular structure determined by single-crystal X-ray diffraction methods. The crystals are monoclinic:P2 ₁/c C _2h ⁵ , No. 14),a=5.682(2),b=7.133(2),c=9.540(3) Å,=104.38(4)°,Z=4. The structure has been solved by direct phase determination methods, and refined to anR value of 0.042 for 633 nonzero independent amplitudes. The molecule of the title compound exists in the structure as a zwitterion, NH ₃ ⁺ -CH₂-C(O)-N-OH. The hydroxamate group is planar and the N (amino) atom, from the glycine part of the molecule, deviates by 1.43 Å from the best molecular plane defined by O(1), N(1), C(1), and O(2) atoms, respectively.The molecules are held together by a network of N⁺-HO, N⁺-H¯N, and O-HO hydrogen bonds.     

Crystal structure of hexa(3,5-dicarboxypyridine)potassium tetrabromoaurate(III)

The title complex has been prepared, and characterized by X-ray crystallography. The crystals are rhombohedral, space groupR32, witha=20.954(5),c=9.753(1) Å,Z=3, andR _F =0.070 for 680 observed MoK reflections. The structure consists of a packing of hexa(3,5-dicarboxypyridine) potassium cations and tetrabromoaurate(III) anions. The potassium atom is surrounded by equivalent oxygen atoms to form a KO₆ octahedron with a very short K-O distance of 2.56(1) Å. The AuBr ₄ ^– group exhibits orientational disorder with a mean bond length of 2.38(1) Å. Two symmetric strong hydrogen bonds (linear OHO and bent NHN) are found in the crystal structure. The nearly planar organic ligands are interlinked by hydrogen bonds to form parallel sheets which approximately correspond to the (003) family of planes. The potassium atoms lying in between these sheets connect them into a three-dimensional network.On leave from Central Laboratory, Nankai University, Tianjin, China.     

Crystal structure and spectroscopic properties of glycinium monophenylphosphate

The crystal structure of glycinium monophenylphosphate [NHsk3/+CH₂COOH·C₆H₅OPO₃H^– has been determined. The crystals are orthorhohombic:Pbca (NO. 61),a=26.001(3),b=7.423(2),c=11.273(2) Å,Z=8. The structure was solved by direct methods, are refined toR=0.035 for 1499 independent reflections. The crystal structure is stabilized by a three-dimensional network of hydrogen bonds. The phosphate group is involved in five H bonds: three NO and two OO bonds, with the shortest distances 2.745(3) and 2.608(2) Å, respectively. The glycine cation is entirely planar, and a cationo-anionic form of the title compound has also been confirmed in solution byIR studies.     

Structure of fruticuline B: A new natural anthracene quinodimethide of abietanoid origin

The title compound is C₁₉H₁₈O₄·1/2 CH₃OH, triclinic,P¯1,a=9.891(2),b=13.273(4),c=13.860(4) Å,a=66.47(2),=86.91(2), and =85.59(2)°. The structure was solved by direct methods and refined by least-squares techniques to anR factor of 0.082 for 2282 observed reflections. The X-ray structure uniquely resolves the one remaining ambiguity, namely the assignment of the correct structure4. There are two crystallographically independent molecules (A and B) and one disordered methanol molecule. Both molecular skeletons show small distortions from planarity with inclinations of 1.7 and 4.0° between the outermost rings A/C in molecules A and B, respectively. Intramolecular hydrogen bonds of the form O(3A)-HO(2A) and O(3B)-HO(2B) are observed in molecules A and B, respectively. The molecules are linked by pairs of O(3A)-HO(2B) and O(3B)-HO(2A) hydrogen bonds. The dimerlike structures are stabilized by intermolecular C-HO interactions and van der Waals forces.     

Crystal and molecular structure of glycinium diphenylphosphate

The crystal and molecular structure of glycinium diphenylphosphate, C₁₄H₁₆NO₆P, has been determined by X-ray methods. The crystals are orthorhombic:Pbca (No. 61),a=11.412(3),b=24.624(7),c=10.775(3) Å,Z=8. The structure was solved by direct methods and refined to anR value of 0.043 for 1289 nonzero independent amplitudes. The molecule exists in the structure as⁺NH₃CH₂CO₂H,(C₆H₅O)₂PO ₂ ^– and is planar except for the N atom, which deviates by 0.49 Å from the plane defined by C(1), C(2), O(5), and O(6) atoms, respectively. The conformation of the diphenylphosphate anion isgauche with respect to both P-O ester bonds. There are four crystallographically independent hydrogen bonds, three of the N-HO type and one of the O-HO type.     

Crystal structure of a nucleoside analog: 1-(R)-[6-(R)-hydroxymethyl-1,4-dioxan-2-yl] uracil

The title compound (C₉H₁₂N₂O₅,M _r =228.2) crystallizes in the trigonal space groupP3₁,21 witha=b=9.438(3) andc=19.775(3) Å,V=1525.5 ų,D _x =1.490 gm cm^–3,Z=6,=0.12 mm^–1,F(000)=720.0,T=293 K. The structure was solved by direct methods and refined by full-matrix least-squares calculations to anR value of 0.044 on 843 unique observed reflections. The dioxane ring adopts a chair conformation. The crystal structure is stabilized by N-HO hydrogen bonds and C-HO close contacts.     

Aquadifluoro(1,10-phenanthroline)copper(II) dihydrate: X-ray crystal structure reveals strong hydrogen bonds between ligand fluoride and lattice water molecules

C₁₂H₁₄CuF₂N₂O₃,M=335.797, monoclinic, space groupP2₁/n,a=6.985(2),b=17.406(2),c=10.581(2) Å,=92.41(2)°,V=1285(1) ų,D _c =1.736 g cm^–3,Z=4,F(000)=684,(CuK)=27.0 cm^–1, =1.5418 Å,T=20°C, crystal dimensions=0.75×0.45×0.30 mm. The structure of the title compound shows it to be [Cu(phen)F₂(H₂O)]·2H₂O with pentacoordinate-square pyramidal Cu(II), short Cu-F bonds [1.890(4) and 1.891(4) Å], and short FH-O hydrogen bonds (ca. 2.68 Å) between the complex and lattice water molecule.     

Molecular structure and some reactivity aspects of 2,6-diamino-4(3H)-pyrimidinone monohydrate

Crystals of C₄H₆N₄O·H₂O are orthorhombic:Pbca,a=16.721(2),b=4.242(1),c=18.293(2)Å,Z=8. The structure has been solved by direct methods and refined by full-matrix least-squares techniques toR=0.046 for 1252 unique reflections. The structure consists of approximately planar molecules of the 3(H)4-one tautomer. Delocalization of the ring and the C=O-electrons, and conjugation of the lone-pair electrons of the amine groups with the pyrimidinone nucleus are observed. The molecules are connected by O-HO, N-HN, and N-HO hydrogen bonds. The molecular structure clarifies the chemical properties of the compound.     

Structure and spectroscopic properties of the 1∶2 complex of 3,5-dimethylpyridine with 3,5-dinitrobenzoic acid and its deuterated analog

The structure of the nondeuterated and deuterated complexes of 3,5-dimethylpyridine with 3,5-dinitrobenzoic acid in a stoichiometric ratio 12 have been determined by X-ray diffraction methods. The crystals of the nondeuterated complex are triclinic, space groupP¯1 witha=9.409(9),b=10.813(7),c=12.310(7)Å,a=95.75(5),=108.17(7), =91.46(7)° andZ=2. The crystals of the deuterated complex are monoclinic, space groupP2₁/c, witha=11.680(6),b=8.451(4),c=24.382(9)Å,=102.94(4)° andZ=4. Both structures have been solved by direct methods and refined toR=0.035 for 2235 and toR=0.044 for 1938 independent reflections for nondeuterated and deuterated crystal, respectively. The structures consist of 3,5-dimethylpyridinium cations and hydrogen (or deuterium) bis(3,5-dinitrobenzoate) anions. The N(1)⁺-H(N1)O(1)^–, O(7)-H(7)O(2), N(1)⁺-D(1)O(l)^– and O(7)-D(7)O(2) bond lengths are 2.644(4), 2.499(3), 2.739(5), and 2.526(5)Å, respectively. The IR spectra of both complexes within the proton (or deuteron) absorption range have been studied.     

Structure and IR spectroscopic properties ofN-methylmorpholinium pentachlorophenolate-pentachlorophenol

The crystal structure of C₅H₁₁OND⁺C₆Cl₅O^–·C₆Cl₅OD has been determined by X-ray diffraction. The crystals are triclinic:P¯1,a=9.443(7),b=7.534(6),c=18.05(2) Å,=91.23(7),=95.83(6), =110.67(6)°,Z=2. The structure was solved by direct methods, and refined toR=0.033 for 2779 non-zero reflections. The structure consists of theN-methylmorpholinium cations and deuterium bis(pentachlorophenolate) homoconjugated anions. The N⁺-D(1)O(l)^– and O(2)-D(2)O(1)^– bond lengths and angles are 2.654(4), 2.557(4) Å, and 171(4), 158(5)°, respectively.     

Synthesis,infrared and Mössbauer characterization and X-ray crystal structure of 1,10-phenanthrolinium tetrachloromethoxy phenylantimonate(V)

The compound has been characterized by X-ray crystal structure determination, Mössbauer and i.r. spectroscopy. It crystallizes in the monoclinic space groupP2 ₁ /c (No. 14) witha=24.228(4),b=8.335(2),c=23.975(4) Å,=117.83(3)° andZ=8. Least-squares refinement on 3749 observed reflections gave finalR=0.034 (R _w=0.037). The compound is constituted by [(C₆H₅)SbCl₄OMe]^– anions andphenH⁺cations. The coordination polyhedron about Sb is an octahedron (Sb-Cl 2.416(3), Sb-O 1.962(7) and Sb-C 2.138(9) Å). The whole structure is characterized by two short contacts (O(1)N(2) 2.76(1) O(2)N(4) 2.75(1) Å) involving the methoxy oxygens of the two independent anionic units [(C₆H₅)SbCl₄OMe]^– and two nitrogens of the two independent phenanthrolinium moieties.     

Crystal and molecular structure of 3-dimethylaminobenzoic acid

The title compound C₉H₁₁NO₂ is triclinic, space group P¯1, with the cell dimensionsa=7.022(1),b=7.476(2),c=8.957 (1) Å,=87.02(2),=110.88(1),=99.10(1)°,V=433.8(4) ų,Z=2,M _r =165.2,Do=1.27,Dx=1.26 mg/m³,F(000)=176,T=293 K,R=0.057 for 939 observed reflections. The molecules are packed as centrosymmetric hydrogen bonded dimers with an O-HO distance of 2.626(3) Å. The COOH group is rotated by 1.7(1)° about the exocyclic C(1)-C(7) bond out of the benzene ring plane. The molecules lie on (0 2-1) plane for which thed value is found to be 3.378 Å which is very close to the mean separation between the parallel packed benezene rings [3.347(4) Å]. The entire molecule is planar except for the two methyl groups attached to the nitrogen atom. The N atom is free from any binding of either type C-HN or O-HN.N. C. L. Communication No. 4699.     

Crystal and molecular structure of an anchored catechol ligand: 2,3-dihydroxy benzenemethanimine α-(2-hydroxymethyl)phenyl

The structure of the new tetranucleating ligand 2,3,-dihydroxy benzenemethanimine -(2-hydroxymethyl)phenyl has been determined by X-ray diffraction techniques. C₁₄H₁₃NO₃ is monoclinic, space groupP2₁/a, with cell dimensionsa=10.382(2),b=19.147(1),c=12.799(1) Å,=113.08(1)°,V=2340.6(3) ų,Z=8,M=243.04,D _o=1.36,D _x=1.38 mg/m³,F(000)=1024,T=293 K,R=0.041 for 2640 observed reflections. There are two molecules in the asymmetric unit and both have a similar geometry. The molecules are parallel to each other, the distance between them being 3.7 Å and the dihedral angle between mean planes 7.8°. There is a pseudocenter between molecule A and (1–x, 1–y, 1–z) of molecule B. The structure is stabilized by intramolecular O-HN and intermolecular O-HO as well as by C-HO hydrogen bonds.NCL Communication No. 5332.     

Crystal structure of 1-(2-hydroxyphenyl)-3-(2-thiomethoxyphenyl)-1,3-propanedione,C16H14O3S

The crystal structure of the enol tautomer of 1-(2-hydroxphenyl)-3-(2-thiomethoxyphenyl)-1,3-propanedione C₁₆H₁₄O₃S, was determined from X-ray crystallography. The finalR value was 5.99% based on 1945 unique observed reflections. The crystals are monoclinic,P2₁/c, witha=7.406(6),b=8.585(6),c=21.992(4) Å,=93.42(2),D _c =1.36 g cm^–3 forz=4. The compound is present in the solid state as a unique enol tautomer.There are two short, intramolecular OO contacts of 2.553(4) and 2.577(4) Å. Both the phenol and the enol H atoms are asymmetrically located with respect to the O atoms.