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.     

Crystal structure of trismorpholino phosphiniminocyclotrithiazene

The title compound (OC₄H₈N)₃P=N–S₃N₃ crystallizes in a monoclinic crystal system with unit cell parameters a = 8.9996(3), b = 17.2895(7), and c = 12.3648(9) Å, = 90.63(5)°, Z = 4, and space group P2₁/n. Strikingly the exocylic S1–N4 bond length is 1.545(3) ÅR and is accompanied by the largest angle at P–N4–S1 as 131.2(2)°. The tricoordinated sulfur atom of the cyclotrithiazene ring deviates from the mean plane of other five atoms by 0.654(1) Å.     

Crystal structure analysis of norbornadiene adduct of diphenyl hexamethylenimino phosphiniminocyclotrithiazene

The title compound (C₆H₁₂N)Ph₂P-N S₃N₃ C₇H₈ crystallizes in the monoclinic space group P2₁/n with unit cell dimensions: a = 9.9200(5), b = 16.3316(11), c = 15.7009(17) Å, = 91.99(1)°, and Z = 4. The cyclotrithiazene ring adopts a chair conformation with equal bond distances and the norbornadiene is fused in an exo, exo fashion to the heterocycle. Norbornadiene addition to the cyclotrithiazene influences the bonding pattern in the ring as well as the P N S moiety.     

Spectroscopic Studies and Crystal Structure of 1-(Morpholino (Phenyl) Methyl) Pyrrolidine-2,5-Dione

Abstract  

A new mannich base 1-(morpholino(phenyl)methyl)pyrrolidine-2,5-dione formed by the direct condensation of morpholine, succinimide and benzaldehyde has been synthesized. The structure of this mannich base has been elucidated on the basis of micro elemental analysis, IR, ¹H NMR, ¹³C NMR, UV–Visible Techniques and Mass. The crystal structure of the title compound C₁₅ H₁₈ N₂ O₃ was determined. It crystallizes in the triclinic system, space group P − 1, with a = 8.8122(13) ?, b = 9.2794(14) ?, c = 9.814 (3) ?, α = 107.154(9)°, β = 97.936(9)°, γ = 110.197(7)°,V = 693.4(2) ?³, D _x  = 1.314 Mg/m³. The structure was solved by the full-matrix least squares on F² and had a refined R value of 0.0486 for 8567 observed reflections. The six membered heterocyclic ring of the morpholino moiety adopts a chair conformation. The crystal structure is stabilized by weak intermolecular C–H···O interactions that link the molecules into inversion dimers.     

Crystal structure analysis of (<Emphasis Type="Italic">N</Emphasis>-methyl piperazino) (phenyl) (dicyclohexylamino) phosphiniminocyclotrithiazene

The title compound (NC₄H₈NCH₃)(C₆H₅)[N(C₆H₁₁)₂]P{—N–S₃N₃ crystallizes in the triclinic crystal system with unit cell dimensions: a = 9.7572(2), b = 10.6845(1), c = 16.9381(3) Å, = 71.75(1), = 80.65(2), = 65.93(1), and Z = 2. The tricoordinated sulfur atom (S1) in the cyclotrithiazene deviates from the mean plane of the other five atoms by 0.716(6) Å, which is the highest among the known phosphiniminocyclotrithiazene structures. In the exocyclic P{—N4–S1 moiety, the two bond distances are short: 1.585(6) and 1.527(6) Å; but the bond angle is large 135.3(4). The S1 displacement is highly correlated with the endocyclic angle at the nitrogen atom (diagonally opposite to S1), but the nature of correlation is bimodal (R = 1.0 + or –1.0) for the cyclic and acyclic substituents (R) in the (R)(C₆H₅)[N(C₆H₁₁)₂]P{—N–S₃N₃ series. On the other hand, the S1–N4 bond distances are negatively correlated (R = –0.94) with the P{—N4–S1 bond angle in the above series.     

Crystal structure of aquo (hydroxo) (ethylenediaminetetraacetato) sodium(I) tin(IV), NaSn(OH)(edta)(H2O)

NaSn(OH)(edta)(H₂O) is monoclinic, space groupP2₁/c, witha=9.747(3)Å,b=9.121(3)Å,c=16.430(6)Å, =98.69(4)°, ų, andZ=4. The coordination environment of Sn(IV) is a capped octahedron. Sn–O distances range from 1.990(6)Å to 2.351(7)Å. Na(I) is five coordinated to three different edta molecules. Na–O distances range from 2.283(9)Å to 2.414(7)Å. The edta ligand presents the E, G/R conformation. The crystal structure is composed of sheets parallel to (001): inside a sheet Sn(OH)(edta) molecules are connected to each other by the Na(I) interactions.     

Crystal Structure of [4-(Methylsulfanyl)Phenyl]Acetic Acid

Abstract  

The title compound, C₉H₁₀O₂S, (I), crystallizes in the triclinic space group, P − 1, with unit cell parameters a = 6.2249(3), b = 7.3733(5), c = 19.5708(12), Å, α = 86.746(5)°, β = 88.682(5)°, γ = 86.988(5)°, Z = 4. The molecule consists of a methyl sulfanyl group bonded to benzyl acetic acid at the 4 position crystallizing with two molecules in the asymmetric unit. The carboxylic acid group from the acetic acid moiety in these two molecules forms a classic O–H···O hydrogen bonded dimer with O···O distances of 2.673(2) and 2.646(2) Å, in a R₂² (8) graph-set motif which link the molecules into pairs around inversion centers in the unit cell. The dihedral angles between the mean planes of the R₂² (8) graph-set motif with the mean planes of the two nearby benzyl groups within the same dimer in the unit cell are 64.1(6)° and 71.3(4)°, respectively. Within the same dimer the dihedral angle between the two benzyl groups is 45.2(1)°. The structure is supported by a weak intermolecular C–H···Cg π-ring interaction and gives support to molecular packing stability in the unit cell. Comparison to a MOPAC AM1 computational calculation provides support to these observations.     

Crystal and molecular structure of [Rh(μ-SBut)(CO)(PPh3)]2

Reaction of [Rh(CO)₂Cl]₂ with Bu ^t SLi followed by refluxing with PPh₃ yields [Rh(-SBu ^t )(CO)(PPh₃)]₂(1). The structure of (1) has been determined by X-ray crystallography. Empirical formula: Rh₂P₂S₂C₄₆H₄₈O₂,M=964.78, triclinic, P¯1,a=11.408(9),b=13.241(8),c=15.830(3) Å,=93.67(3),=93.12(5),=110.8(6)°,Z=2,D _calc=1.44 g cm^–3,R=0.048 (R _w =0.062) for 5939 observed reflections. In the solid state, the compound exhibitscis geometry with respect to the phosphine and CO ligands. The geometry about the two metals is essentially square planar, with a dihedral angle of 103.2°, and a butterfly angle of 102.3°. Compound (1) is stereochemically rigid on the NMR time scale from –80 to +80°C.     

Crystal and molecular structure of di(perchlorato)(1,4,8,11-tetraazacyclotetradecane)copper (II). Cu(cyclam) (ClO4)2

The title compound, Cu(C₁₀H₂₄N₄)(ClO₄)₂, crystallizes in the triclinic system with unit cell dimensionsa= 8.744,b= 8.022,c= 8.677 Å, α = 118.7, β = 56.9, γ = 113.5 °,Z= 1, space group P¯1. The structure was solved by Fourier methods and refined by least-squares techniques using the 1545 nonzero three-dimensional counter-diffraction intensity data (CuKα) to give a conventionalR factor of 0.056. The coordination sphere of the copper ion is defined by a planar arrangement of the four nitrogen donors in the macrocyclic ligand with oxygen atoms from the perchlorate groups lying above and below this plane. The resulting tetragonally distorted octahedron of donor atoms gives interatomic distances Cu?N = 2.02(4) Å and 2.02(3) Å, and Cu?N = 2.57(4) Å.     

Crystal Structure of 1-(4-(5,6-Dihydropyridazin-1(4H)-yl)Phenyl)-N-Methylmethanesulfonamide

Crystallography Reports - The title compound, 1-(4-(5,6-dihydropyridazin-1(4H)-yl)phenyl)-N-methylmethanesulfonamide (C12H17N3O2S), was isolated as an impurity during the preparation of sumatriptan...     

Crystal structure of bis(benzimidazolium) tetrabromocuprate(II)

Stable, dark-violet crystals of (C₇H₇N₂)₂CuBr₄ were obtained from an aqueous solution of CuBr₂, HBr, and benzimidazole. The crystal structure was determined by three-dimensional X-ray analysis. The crystals are monoclinic:C2/c, a=15.651(4),b=7.945(1),c=15.775(4) Å,=91.44(2)°,Z=4,V _c=1960.96 ų,D _x=2.105 g cm^–3. The structure was refined by full-matrix least squares to giveR=0.042 andR _w=0.048 for 1254 intensities above 3(I). The copper(II) ions are four-coordinated in the form of a distorted tetrahedron CuBr₄ ofC ₂ symmetry. Two different Cu-Br bond lengths are observed: Cu-Br(1)=2.426(2), Cu-Br(2)=2.330(2) Å. Only one flattened angle [Br(2)-Cu-Br(2)=132.71(9)°] in the CuBr₄ tetrahedron is noted. The angles Br(1)-Cu-Br(1)=108.83(7), Br(2)-Cu-Br(1)=99.92(5) and Br(2)-Cu-Br(1)=107.13(5)° have been found. Hydrogen bonds explain the deformation of the CuBr ₄ ^2– coordination polyhedron. The structure is compared with other CuX ₄ ^2– complexes.     

Crystal structure of chloritopentamminecobalt(III) tetracyanopalladate(II)

The X-ray crystal structure of [(NH₃)₅Co(ClO₂)][Pd(CN)₄]·H₂O consists of two discrete complex ions and a water of hydration. The red crystals are triclinic, P , with lattice parameters a = 7.1992(5), b = 9.4873(7), c = 11.7752(8) Å. = 66.680(1), = 75.784(1), = 82.203(1)°, and Z = 2 giving a cell volume of 715.27(9) ų and a calculated density of 2.043 g/cm³ at 293°. The chlorite ion is O-bonded to the cobalt atom with amine N—Co distances all equal. The chlorite ion is bent with a O—Cl—O angle of 110.8(2)° and the Cl—O distances being 1.601(3) and 1.558(3) Å, the longer value for the O atom also coordinated to Co. The Pd(CN)^–2 ₄ ions are planar, C-coordinated and stack along the x-axis, separated by 3.599(1) Å and alternatively rotated by 29.9(5)°.     

Crystal structure of dicyanatobis(pyridinato)-copper(II)

The crystal structure of dicyanatobis(pyridinato)copper(II), C₁₂H₅CuN₄O₂, was determined from 658 X-ray diffraction data obtained by the -2 scanning technique with MoK radiation on a SYNTEX P2₁ four-circle diffractometer. The blue crystals are tetragonal:I4₁/a,a = 15.649(3),c = 9.917(3) Å, andZ = 8. The structure was determined by the heavy-atom method and refined by full-matrix least squares toR = 7.1%. Nonhydrogen atoms were refined anisotropically, and the positional parameters of hydrogen atoms were calculated from geometrical considerations. The copper atom is planarlytrans coordinated by two nitrogen atoms from the NCO groups and two nitrogen atoms from the pyridine molecules. The oxygen atoms from two of the approximately linear NCO groups complete the Cu(II) coordination as a distorted octahedron. Through their oxygen and nitrogen atoms, the NCO groups link the metal atoms to the skeleton structure. The bond lengths are 1.15 and 1.18 Å for N-C and C-O, respectively, the N-C-O bond angle being 176.8 °. The bond lengths Cu-N in square-planar coordination are 1.95 and 2.05 Å, while the Cu-O bonds are out of plane and 2.61 Å in length.Part XVIII in the seriesCyanatocopper(II) complexes with organic ligands; Part XVII: J. Kohout, A. Malejova and J. Gazo, Chem. Zvesti, in press.     

Crystal structure of tris(methylcyclopentadienyl) tetrahydrofuranatosamarium

The first crystal structure of tris(methylcyclopentadienyl) tetrahydrofuranato (THF) lanthanide complexes, (CH₃Cp)₃Sm · THF, is determined. The complex crystallizes from mixed solvents of tetrahydrofuran and hexane as a monomer in the orthorhombic space group Pc2₁n with the unit cell parameters a = 9.135(2) Å, b = 13.263(2) Å, c = 16.176(3) Å, and Z = 4.     

Crystal structure of monomethylammonium monochlorodibromomercurate(II)

The crystal structure of monomethylammonium monochlorodibromomercurate (II) was refined from single crystal X-ray data including the fractional contribution of centrosymmetric domains. The refinement converged toR=0.05 in space groupC2. The fraction of structure and its inverse were detected in the refinement. The structure is one-dimensional consisting of distorted tetrahedra (HgCl₂Br₂) connected together by chlorine atoms, The CH₃NH ₃ ⁺ groups are connected to the chains by hydrogen bonds to the halogen atoms contributing to the cohesion of the crystal.     

Crystal structure of monomethylammonium monochlorodibromomercurate(II)

The crystal structure of monomethylammonium monochlorodibromomercurate (II) was refined from single crystal X-ray data including the fractional contribution of centrosymmetric domains. The refinement converged toR=0.05 in space groupC2. The fraction of structure and its inverse were detected in the refinement. The structure is one-dimensional consisting of distorted tetrahedra (HgCl₂Br₂) connected together by chlorine atoms, The CH₃NH ₃ ⁺ groups are connected to the chains by hydrogen bonds to the halogen atoms contributing to the cohesion of the crystal.     

Crystal structure of monomethylammonium tribromocadmate(II)

CH₃NH₃CdBr₃ crystallizes in the space group Ccm2₁, a = 13.693(1) Å, b = 7.906(1) Å, c = 6.886(1) Å, V = 745.46(15) ų, Z = 4, D _x = 3.42 Mg m^–3. The structure of the title compound is one-dimensional consisting of infinite chains made of face sharing CdBr₆ octahedra. The methylammonium groups are situated in the space between chains. The cations and anions are joined by hydrogen bonding.     

Crystal structure of penthylenediammonium pentachlorothallate(III)

The penthylenediammonium pentachlorothallate(III) salt is orthorhombic with the following unit cell dimensions: a = 7.696(3) Å, b = 13.2890(17) Å, and c = 13.503(18) Å, space group P2₁2₁2₁ with Z = 4. The structure was solved by Patterson methods and refined to a final R value of 0.0387 for 1991 observed reflections. The structure consists of penthylenediammonium cations and polynuclear anions in which slightly distorted [TlCl₆]^3– octahedral sharing two vertices are interconnected into chains. These chains are themselves interconnected by means of the N–HCl bonds originating from the [NH₃(CH₂)₅NH₃]²⁺ entities forming a three-dimensional network.     

Crystal structure of tetrakisdiphenylammonium hexadecachlorotetrabismuthate(III)

[(C₆H₅)₂NH₂]₄ ⁺[Bi₄Cl₁₆]^4– crystallizes in the triclinic space group witha=11.835(2),b=12.393(2),c=12.625(3)Å, =108.37(3), =108.69(3), =96.00(3)° andD _c=2.135 g cm^–3 forZ=1. The [Bi₄Cl₁₆]^4– anion is a centrosymmetric cluster of four distorted edge-sharing BiCl₆ octahedra. The ranges of the Bi–Cl bonds are 2.484(4)–2.606(3)Å for Bi–Cl(terminal), 2.691(3)–2.956(4)Å for Bi-Cl(µ₂), and 2.960(3)–3.120(4)Å for Bi-Cl(µ₃). The cations and anions are held in place by weak hydrogen bonds.