Crystal and molecular structure of nickel(II) dicyanothiosemicarbazide monohydrate

The structure of the title compound (Ni(CN)₂(CH₅N₃S)·H₂O) has been determined, from X-ray diffractometer data, by the heavy-atom method and refined by least-squares. The finalR-values, based on 3109 observed reflections, areR=0.035 andR _w =0.039. The complex has square-planar geometry with two adjacent cyano carbon atoms (Ni-C, 1.838(2) Å and 1.862(2) Å)and thiosemicarbazide sulfur and nitrogen atoms (Ni-S, 2.169(1) Å and Ni-N, 1.923(2) Å). The water molecule does not enter the inner coordination sphere of the nickel atom; however, it plays a very important role in the crystal structure. Water is coordinated by hydrogen bonds to four adjacent complex units.     

Crystal and molecular structure of bis(acetylacetonato) nickel(II)diethanol

The title compound, Ni(C₅H₇O₂)₂· (C₂H₅OH)₂, crystallizes in the triclinic system with unit cell dimensionsa = 8·923,b = 5·283,c = 9·522 Å, = 81·4, = 106·1 and = 103·3 °;Z= 1, space groupP¯1. The structure was solved by Fourier methods, and the 1557 three-dimensional counter diffraction intensity data (CuK) were used in a least-squares refinement to a conventional unweightedR of 0·053. The nickel atom is surrounded by the four oxygen atoms of the two acetylacetone ligands and the two oxygen atoms of the ethanol molecules, forming a tetragonally-distorted octahedron with acetylacetone oxygen atoms at 1·997 and 2·026 Å and ethanol oxygen atoms at 2·140 Å. Parallel molecules are linked into columns along theb-axis by hydrogen bonds between the ethanol oxygen atom of one molecule and an acetylacetone oxygen atom of a neighboring molecule.Presented at the Amer. Cryst. Ass'n. Summer Meeting, Ames, Iowa, Aug. 1971.Taken in part from the M.S. Thesis in Physics of T. S. Burke, Syracuse University, 1971.     

Crystal and molecular structure of nitrito-bis(1,3-propanediamine) nickel(II) tetraphenylborate

The title compound is orthorhombic,M _r =590.2,P2₁2₁2₁ (No. 19),a=9.865(2),b=9.924(2),c=31.202(7) Å,V=3055(2) ų,Z=4,D _x =1.283 g cm^–3, (MoK );F(000)=1256; (MoK )=6.76 cm^–1, finalR=0.052 for 1441 reflections I2.5(I). The nitrite group is chelated via the two oxygen atoms; the two six-membered rings resulting from the coordination of the 1,3-propanediamine ligands to the nickel(II) atom are in the chair conformation. The Ni-N and Ni-O distances average 2.07(1) and 2.14(2) Å respectively. The two Ni-O distances are nearly equivalent.     

Crystal and molecular structure of tetrakis(N,N′-diallylthiourea)nickel(II) iodide

Summary The crystal structure of tetrakis(N,N-diallylthiourea)nickel(II) iodide [Ni(C₇H₁₂N₂S)₄I₂] has been determined by a three-dimensional X-ray analysis. FinalR, after anisotropic least-squares refinement, is 8·8%. The crystals are tetragonal (P4/n):a = 11·24(1),c = 15·43(1) Å,Z = 2. Ni(II) is on a 4-fold axis; the coordination around it is flattened pyramidal and involves four sulphur atoms from four diallylthiourea molecules (Ni-S = 2·221 Å). Ni(II) is out of the plane through the sulphur atoms by 0·40 Å. Two I^- ions lie on opposite sides with respect to the nickel atom along the 4-fold axis, at distances Ni...I(1) = 3·74 Å, Ni...I(2) = 6·64 Å. The orientation of the allylthiourea molecules is determined mainly by a hydrogen bond formed by one nitrogen (N(1)) with the iodine which is nearer to the nickel.The authors are indebted to Prof. C. Furlani who kindly supplied the crystals of the compound.     

Crystal and molecular structure of bis(2,2,6,6-tetramethylheptane-5-thiolo-3-onato)nickel(II)

The crystal structure of the nickel(II) chelate of the monothio derivative of 2,2,6,6-tetramethyl-heptane-3, 5-dione has been studied at room temperature by X-ray diffraction methods. The space group isP2₁/c and the crystal data area = 19·96(2),b = 10·25(1),c = 12·45(1) Å, = 102·17(5) °Z = 4,D _m = 1·22,D _c = 1·23 g cm^–3. Full-matrix least-squares refinement of atomic and anisotropic thermal parameters, using 2109 non-zero intensities obtained by counter methods, terminated with a conventionalR of 0·105. The nickel was found to be surrounded by acis arrangement of two oxygen and two sulphur atoms which is almost planar, but slightly distorted towards a tetrahedron. All the evidence obtained supports extensive delocalization in the chelate rings, and the entire molecule has pseudomm symmetry. Thecis, rather thantrans relationship of the ligand atoms may indicate weak S-S interaction.     

Cobalt(II) and nickel(II) complexes ofN-protected amino acids. Crystal and molecular structure of bis (N-acetylglycinato)tetraaquocobalt(II)

Binary complexes of formula [M(II)(acgly)₂(H₂O)₄] (M(II)=Co(II), Ni(II), acgly=N-acetylglycinate ion) were synthesized, and for the Co(II) complex the crystal and molecular structure was determined. The crystals are monoclinic, space groupP2₁/c,a=4.838(1),b=10.785(2),c=14.340(6) Å,=96.96(2)°,Z=2. The structure was solved by the heavy-atom method and refined through full-matrix least-squares calculations toR=0.0394 for 1069 observed reflections. The coordination around the cobalt atom is slightly elongated octahedral arising from one carboxylate oxygen of each of the two centrosymmetrically related monodentateN-acetylglycinate anions and four water molecules.     

Crystal and molecular structure of (±)-cyclomethylenomycinA

The structure of (±)-cyclomethylenomycinA, a penultimate synthetic precursor of the antibiotic methylenomycinA, was determined by direct methods from MoK diffractometer data. The crystals of (±)-cyclomethylen-omycinA are orthorhombic, space groupPbca, a=15.5724(1),b=11.4415(1),c=9.5454(1)Å, andZ=8. The structure was refined toR=0.077. The chemically determined structure was confirmed. Bond distances and angles are normal and there are no unusual C-H | | | O intermolecular contacts.IUPAC name: 3-(Hydroxymethyl)-1,5-dimethyl-4-oxo-6-oxabicyclo[3.1.0]hexane-2-carboxylic acid -lactone.     

Crystal and molecular structure ofcis-mesityl(phenylsulphonyl)sulphine

Cis-mesityl(phenylsulphonyl)sulphine, C₁₆H₁₆O₃S₂, crystallizes in the tri-clinic system: space groupP¯1,a = 9.209(2),b = 11.106(2),c = 7.626(1) Å, α = 92.53(1), β = 98.53(3), γ = 89.82(2) °. The structure has been determined by Patterson and direct methods and refined by full-matrix least squares toR = 0.057 for 2724 observed reflections. The sulphine moiety has bond lengths 1.622(2) Å for C-S, 1.466(3) Å for S-O and a C-S-O angle of 115.2(2) °, indicating sp² hybridization on the sulphur atom. All other bond distances and angles are close to normal values. The molecules are held together by van der Waals forces.     

Crystal and molecular structure ofE-mesityl(phenylsulphinyl)sulphine

E-mesityl(phenylsulphinyl)sulphine, C₁₆H₁₆O₂S₂, crystallizes in the monoclinic system: space groupP2₁/c,a = 8.310(2),b = 14.141(3),c = 14.873(4)Å, = 116.67(4) ° andz = 4.The structure has been determined by direct methods and refined by full-matrix least squares toR = 0.060 for 1834 non-zero reflections. The sulphine moiety has bond lengths 1.628(5)Å for C-S, 1.470(5)Å for S-O and a C-S-O angle of 113.8(2) °, values which are consistent with a cumulated double-bond system and sp² hybridization on the sulphur atom. All other bond distances and angles are close to those usually found for such functional groups.     

Crystal and molecular structure ofS-methyl(pentafluorosulfanyl)thiocarbamate

The X-ray structure of S-methyl(pentafluorosulfanyl)thiocarbamate, SF₅NHC(O)SCH₃, has been determined from three-dimensional diffractometer data and refined by full-matrix least-squares techniques. The crystals are monoclinic:P2₁/m,a=5.008 (5),b=7.811 (2),c=9.348 (4) Å, =99.08 (7)°, andZ=2; finalR=0.046 for 517 observed reflections. The structure comprises hydrogen-bonded (NHO) chains with the component monomers in thecis, cis-conformation, i.e., the arrangement of the nonhydrogen and nonfluorine atoms is nearly planar, the SF₅ group and the O are in acis position with respect to the C-NH bond, and the O and the CH₃ group are in acis position with respect to the C(O)-S bond. Theoretical methods including MNDO and molecular modeling were used to study the relative stabilities of the four possible conformations of SF₅NHC(O)SCH₃.     

Crystal and molecular structure of 6-0-acetylgrayanotoxin III

The crystal and molecular structure of a grayanotoxin III derivative, 6-0-acetylgrayanotoxin III is presented. The crystal is orthorhombic, space group P2₁2₁2₁, witha=15.582(3),b=21.304(3),c=6.339(3)Å,V=2104(1) ų Z=4. The structure was solved by direct methods and refined by full matrix least-squares methods to a finalR=0.047 for 1763 independent reflections withF ₀>3 (F ₀) The molecule is based on a tetracyclic structure consisting of two five-membered, one six-membered, and one seven-membered ring with various conformations.     

Crystal and molecular structure of triethanolammonium nitrate (TEAN)

The crystal and molecular structure of crystalline triethanolammonium nitrate (TEAN) was determined. TEAN is monoclinic with space groupP2₁/c and has lattice parametersa=6.592(1),b=16.358(1),c=9.3850(8)Å and=90.87(1)°. Based on four formula weights of TEAN per unit cell, the computed density is 1.393 g/cm^–3. The structure is a three-dimensional hydrogen bonded network of cations and anions. An interesting feature of the cation conformation is the presence of intramolecular trifurcated hydrogen bonding of the proton.     

Crystal and molecular structure oftrans-dichlorobis(oxazole)palladium(II)

The crystal and molecular structure oftrans-dichlorobis(oxazole)palladium-(II), Pd(C₃H₃ON)₂Cl₂, has been determined by single-crystal X-ray diffraction techniques using counter methods and has been refined by full-matrix least-squares procedures to a finalR index of 0.022. The complex crystallizes in the triclinic space groupP¯1 with unit cell dimensions ofa = 6.957(1),b = 7.506(1),c = 5.538(1) Å, = 109.22(1), = 91.37(1), and = 115.09(1) °, withZ = 1. The palladium(II) ion, located at an inversion center, is coordinated in a regular square-planar manner to two chloride ions at 2.293(1) Å and, at 2.016(2) Å, to the nitrogen atoms of two oxazole ligands. The planar oxazole rings are tilted 33 ° with respect to the PdN₂Cl₂ plane. Further verification of the presence of oxazole in the complex was obtained by high-resolution mass spectrometry. Crystals of Pd(C₃H₃ON)₂Cl₂ resulted irreproducibly from attempts to prepare single crystals of a previously reported dimeric palladium(II) disulfide complex by treating Pd(CH₃CN)₂Cl₂ with a slight excess of diphenyl disulfide in benzene in the atmosphere. The source of the oxazole is not understood.     

Crystal and molecular structure oftrans-dichlorobis(N-propylimidazole)palladium(II)

The crystal structure of Pd(N-PropIm)₂Cl₂ has been determined from X-ray data collected by counter methods. The compound crystallizes in the monoclinic space groupP2₁/n with four molecules per unit cell, the dimensions of which area=14.554(5),b=8.204(2),c=14.860(3) Å,=115.63(2)°. Full-matrix least-squares refinement gave a final R value of 0.0263 for 1913 independent observed reflections. The Pd atom is four-coordinated and is surrounded in atrans square planar fashion by two N atoms of the imidazole groups and by two Cl ions.     

Crystal and molecular structure of bis(diphenylmethyl) ether

Bis(diphenyl methyl)ether, C₂₆H₂₂O, crystallizes in the monoclinic system:a = 9.823(2),b = 22.638(5),c = 9.275(2) Å, β = 104.89(1) °,Z = 4,P2₁/n. The structure has been determined by direct methods, using CuKα photographic data, and refined by full-matrix least squares toR = 0.058 with Cu Kα diffractometer data for 1974 observed reflections. The molecules are held together entirely by van der Waals' forces. There is a marked difference in the molecular conformation, as defined by dihedral angles, on each side of the central oxygen atom.     

Crystal and molecular structure of tetrapyridyl-copper(II)-bis-nitrato-bis-pyridine

The crystal and molecular structure of a pyridine complex of anhydrous copper(II)nitrate is described. The structure has been solved by vector search methods and refined by least-squares methods to R₁=0.049 [I>2(I)]. The complex lies on a twofold axis parallel toa, and two solvent pyridine molecules lie on twofold axes parallel toc. The copper atom is coordinated by four pyridyl groups and two monodentate NO₃ groups. Crystal data: C₃₀H₃₀N₈O₆Cu, orthorhombic, space group Pnna(52),a=14.446(7),b=12.154(5),c=16.881(4) Å,V=2964(2) ų,Z=4.     

Crystal and molecular structure of hexahydropyridine (piperidine) hydrochloride

The structure of hexahydro pyridine (piperidine), a compound of psychobiological importance, has been determined in the form of its hydrochloride by the heavy-atom technique, using three-dimensional X-ray data. Hexahydro pyridine hydrochloride, (C₅H₅N)H₆.HC1, crystallizes in the orthorhombic space groupPbcm with four molecules per unit cell of dimensionsa = 9.68(2),b = 7.30(3),c = 9.67(2) Å. The positions of the hydrogen atoms were located from a difference-Fourier synthesis. The structure was refined by the full-matrix least-squares method, using anisotropic temperature factors, leading to the finalR-value of 0.094. The hexahydro pyridine ring has a chair conformation. The crystallographic mirror plane atz = 1/4 coincides with the molecular mirror plane passing through the C1, N and C(3) atoms of the molecule in such a way that C(1)′ and C(2)′ are the mirror images of C(1) and C(2). The dihedral angles which plane I, containing C(1), C(2), C(2)′ and C(1)′, makes with plane II, containing C(2), C(3) and C(2)′, and planeIII, containing C(1), N and C(1)′, are 120.47 and 116∶42 °, respectively. The molecules are held together by a network of hydrogen bonds of type N⁺ —H ... C1^? in thexy-plane, and by van der Waals forces in thez-direction. Both the hydrogen atoms in the NH ₂ ⁺ group of the molecule take part in the formation of hydrogen bonds.