Crystal structure of 1,4-dihydro-1-methyl-3′-methylsulfinyl-4-oxo-6-nitro-3,4′-diquinolinyl sulfide complex with DMF

The title compound crystallized as a complex with N,N-dimethylformamide (DMF) in a monoclinic space group P2 ₁ /c with a = 9.469(2), b = 25.168(5), c = 9.860(3) Å, and = 97.48(3)°. The two quinoline moieties are nearly perpendicular. The sulfoxide oxygen is pointed toward the H-2 proton. The S-methyl group is perpendicular to the parent pyridine ring plane.     

The structure of Wallach's compound. Single-crystal X-ray structure determination oftrans-2,5-bis(trichloromethyl)-N-(1′-hydroxy-2′,2′,2′-trichloroethyl)-4-imino-1,3-dioxolane

The structure of Wallach's compound, C₇H₄O₃NCl₉, prepared in 1874 from concentrated aqueous solutions of potassium cyanide and chloral hydrate, has long been undecided. By single crystal X-ray crystallography it has now been established astrans-2,5-bis(trichloromethyl)-N-(1-hydroxy-2,2,2-trichloroethyl)-4-imino-1,3-dioxolane, confirming the tentative assignment by¹H and¹³C NMR spectrography. The title compound is monoclinic,P2₁/c;a=8.445 (1),b=10.948(1),c=17.923(4) Å;=94.36(1)°;Z=4. The structure was solved by direct methods, from data collected at room temperature on an Enraf-Nonius CAD4 diffractometer, and refined by least squares to a finalR value of 0.041 using 2101 reflections.     

C-H⋯π(Ar)⋯Cl-C,C-Cl⋯π(Ar), Cl⋯Cl and other interactions in the crystal structure of 6-benzoyl-2,4-bis(trichloromethyl)-1,3-benzdioxin

The title compound is monoclinic,P2₁/n,Z=4,a=9.934(1),b=18.399(2),c=11.098(2)Å, =111.08(1)°. The molecule can conveniently be visualized as a benzophenone molecule with one of the aromatic rings fused to a 1,3-dioxin ring which adopts a distorted envelope conformation withcis-trichloromethyl groups substituted at positions 2 and 4. An interaction, observed for the first time, involves a hydrogen atom and a chlorine atom from opposite sides of the same aromatic ring to give C-H-(Ar)Cl-C. The parameters are Hring-centroid 2.63 A, Clring centroid 3.41 Å, Hring-centroidCl 167°, C-Hring centroid 159°, C-Clring centroid 150.2°. The (Ar) system is that of the unfused aromatic ring. A second (Ar) Cl-C interaction occurs but this time with the (Ar) system of the fused aromatic ring. The ClCl and ClO(=C) interactions form the familiar zig-zag pattern which has been noted for many chloroaromatic compounds.     

Crystal structure of the Λ-[4M] enantiomer of cis-diaqua-bis(1,3-dimethylpteridine-2,4(1H,3H)-dione-N5,O4) copper(II) perchlorate monohydrate

Single-crystal X-ray diffraction studies have been performed on the complex cis-diaqua-bis(1,3-dimethylpteridine-2,4(1H,3H)-dione-O⁴,N⁵) copper(II) perchlorate monohydrate, [Cu(DLM)₂(H₂O)₂](ClO₄)₂ · H₂O. This compound crystallizes in the orthorhombic system, P2₁2₁2₁ space group, Z = 4 with a = 8.749(1) Å, b = 14.213(1) Å, c = 21.200(2) Å, and V = 2636.2(4) ų. The metal ion is surrounded in octahedral geometry by two mutually quasi-perpendicular N5,O4-coordinated lumazine chelators with the O4 atoms trans and the N5 atoms cis. The polyhedron is completed by two cis-coordinated water molecules. The absolute configuration of the complex can be described, following Bailar's nomenclature, as the enantiomer of the stereoisomer 4M. A three-dimensional hydrogen-bond network is defined by water molecules, perchlorate anions, and the O2 of the pteridine A.     

Crystal structure and resonance Raman spectroscopic study of {1,3-bis[3-(5-amino-1,2,4-triazolyl)]triazenido-N′4,N2,N″4}chloro palladium(II)-methanol (1/1)

The crystal and molecular structure of the complex [Pd(batt)Cl]·CH₃OH, in which Hbatt is 1,3-bis[3-(5-amino-1,2,4-triazolyl)]triazene, has been determined by X-ray diffraction methods. The crystals are triclinic, space group (a = 10.1883(9) Å, b = 10.5095(8)Å, c = 13.1760(11) Å, = 94.518(6)°, = 109.040(7)°, = 113.678(7)°; Z = 4). The deprotonated batt^– ligand exhibits terdentate chelate coordination with a new nitro-type ligation mode of the triazenido group and N⁴ coordination of the two outer triazolyl substituents. The asymmetric unit contains two crystallographically independent, almost parallel Pd(batt)Cl molecules with Pd–Pd contacts of 3.4584(7)Å and two independent methanol molecules. The complexes are packed in a layer structure with numerous intermolecular H-bond connections. Raman spectra have been recorded for various excitation wavelengths along the contour of the intense triazenido -* absorption band at 465 nm and resonance profiles measured for the most important Raman bands. A comparison is made with the analog [Cu(batt)Cl] complex. Structural and spectral differences between the two molecules are emphasized and related to differences in metal-ligand bonding.     

C−Cl...π(Ar)...Cl−C,Cl...Cl and other interactions in the structures of two 6-substituted-2,4-bis(trichloromethyl)-1,3-benzdioxin's: (I) 6-carboxymethyl; (II) 6-propionyl,an antimethanogenesis food additive

C₁₂H₃Cl₆O₄, (I),M _r=428.91, triclinic, ,a=9.197(1),b=9.336(2),c=9.830(1) Å, =79.29(1), =83.33(1), =85.38(1)°,V=822.16,Z=2,D _x=1.73 Mg m^–3,F(000)=428, (MoK)=0.71069 Å, =10.62 cm^–1, room temperature, finalR=0.033 for 2573 unique counter reflections withF _o>4(F _o). C₁₃H₁₀Cl₆O₃, (II),M _r=426.94, triclinic, ,a=9.374(2),b=9.503(1),c=9.888(4) Å, =79.26(2), =82.10(3), =84.43(1)°,V=854.88,Z=2,D _c=1.66 Mg m^–3,F(000)=428, =0.71069 Å, =10.17 cm^–1, room temperature, finalR=0.030 for 2609 unique counter reflections withF _o>4(F _o). Compounds I and II are isostructural. Centrosymmetric dimers are formed by hydrogen bonds from the two methine hydrogen atoms to the carbonyl oxygen atom. The dimers are linked by Cl...(Ar)...Cl, Cl...O and Cl...Cl interactions to form a three-dimensional pattern. The geometry associated with these interactions is discussed in terms of the electrophile: nucleophile model.     

Crystal structure and vibrational spectra of two cadmium halide complexes with 1,2-Bis[2-(Diphenylphosphinylmethyl)phenoxy]ethane (L 1) and 1,3-bis[2-diphenylphosphinylmethyl)phenoxy]propane (L), CdBr2 ⋅ L 1 and CdI2 ⋅ L

Two cadmium halide complexes with 1,2-bis[2-(diphenylphosphinylmethyl)phenoxy]ethane (L ¹) and 1,3-bis[2-(diphenylphosphinylmethyl)phenoxy]propane (L), namely, CdBr₂ ? L ¹ (I) and CdI₂ ? L(II), have been synthesized. An analysis of their vibrational spectra is carried out. The structures of I and II are determined by X-ray diffraction. Crystals I are monoclinic, a = 31.562(6) Å, b = 13.548(3) Å, c = 18.733(4) Å, β = 91.28(3)°, space group C2/c, Z = 8, and R = 0.051 for 3776 reflections. Crystals II are triclinic, a = 11.803(2) Å, b = 12.554(3) Å, c = 14.686(3) Å, α = 90.30(3)°, β = 90.29(3)°, γ = 106.08(3)°, space group $P\bar 1$ , Z = 2, and R = 0.043 for 4916 reflections. Compounds I and II exhibit a polymeric chain structure. The potentially tetradentate ligands L ¹ and L are coordinated to the metal atoms only through two phosphoryl oxygen atoms and fulfill the bidentate bridging function. The environment of the Cd atom is completed to the tetrahedral coordination by two Br atoms in complex I and two I atoms in complex II. The mean distances are as follows: Cd-Br, 2.526(2) Å; Cd-I, 2.695 Å; and Cd-O, 2.243(8) Å in I and 2.210(4) Å in II. The L ¹ and L ligands in complexes I and II adopt an S-shaped conformation.