Xianjin Yu

Terephthalic acid–4,4′-bipyridine (2/1)

In the title compound, 2C8H6O4·C10H8N2, the 4,4′-bipyridine molecule is located on an inversion centre. In the crystal structure, strong intermolecular O—H⋯N hydrogen bonds between the terephthalic acid and 4,4′-bipyridine molecules lead to the formation of chains with graph-set motif C 2 2(8) along the diagonal of the bc plane.

catena-Poly[[(2-{1-[2-(2-amino­ethyl­amino)ethyl­imino]­eth­yl}-5-methoxy­phenolato-κ4N,N′,N′′,O)copper(II)]-μ-nitrato-κ2O:O′]

In the title compound, [Cu(C13H20N3O2)(NO3)]n, the CuII atom is chelated by the Schiff base ligand via three N atoms and one O atom lying in an approximate square plane (r.m.s. deviation = 0.04 Å). The complex molecules are linked into a polymeric chain by bridging nitrate anions, forming axial Cu—O bonds of 2.535 (6) and 2.676 (7) Å, completing a distorted octahedral coordination geometry. The NH groups of the ligand form hydrogen bonds to the nitrate anions.

catena-Poly[[bis­(p-toluene­sulfonato-κO)palladium(II)]bis­(μ-1,3-di-4-pyridylpropane-κ2N:N′)]

In the title compound, [Pd(C7H7O3S)2(C13H14N2)2]n, the metal ion, located on a twofold rotation axis, exhibits a slightly distorted octahedral coordination environment, with bond angles that deviate by at most 2.2° from an ideal geometry, completed by two O atoms from two deprotonated p-toluenesulfonic acid ligands and four N atoms from four 1,3-di-4-pyridylpropane ligands. One of the sulfonate O atoms is disordered over two positions [ratio 0.70 (5):0.30 (5)].

Crystal structure of tetrakis(2-2-methylbenzoato)-bis(2-methylbenzoato)- bis(1,10-phenanthroline)dipraseodymium(III) monohydrate, Pr2(C8H7O2)4(C8H7O2)2(C12H8N2)2 · H2O

C72H60N4O13Pr2, triclinic, P1 (no. 2), a = 12.986(3) Å, b = 13.992(3) Å, c = 20.889(4) Å, 2 = 101.18(3)°, 0 = 93.88(3)°, / = 115.82(3)°, V = 3301.8 Å, Z = 2, Rgt(F) = 0.066, wRref(F) = 0.201, T = 293 K. Source of material A mixture of praseodymium(III) chloride (0.5 mmol), o-toluic acid (1 mmol), sodium hydroxide(1 mmol), 1,10-phenanthroline (0.5 mmol), H2O (8 ml) and ethanol (8 ml) in a 25 ml Teflon-lined stainless steel autoclave was kept at 433 K for three days. Colorless crystals were obtained after cooling to room temperature with a yield of 16 %. Chemical analysis — found: C, 58.70 %, H, 3.86 %, N, 3.75 %; calculated for C72H60N4O13Pr2: C, 58.74 %, H, 3.94 %, N, 3.81 %. Experimental details The hydrogen atom H1W was located from difference density map and was refined with d(O1—H1W) = 0.82(2) Å. The hydrogen atoms on methyl groups were placed in calculated positions with a d(C—H) = 0.98 Å and Uiso(H) = 1.5 Ueq of the respective carrier atom. All other H atoms were placed in calculated positions with d(C—H) = 0.95 Å and Uiso(H) = 1.2 Ueq of the respective carrier atom. Discussion In recent years, carboxylic acids have been widely used as polydentate ligands, which can coordinate to transition or rare earth ions yielding complexes with interesting properties that are useful in materials science. In the title crystal structure Pr(III) is chelated by two o-toluicate and one 1,10-phenanthroline. Two cations are linked into dimer via three bridging carboxylate groups from three o-toluicate. Pr(III) ion is nona-coordinated with seven O atoms and two N atoms.The d(Pr—N) and d(Pr—O) are in the range of 2.720(8) 2.757(8) Å and 2.452(6) 2.750(6) Å, respectively. The shortest distance between two Pr(III) cations is 4.100(2) Å. Z. Kristallogr. NCS 223 (2008) 415-418 / DOI 10.1524/ncrs.2008.0182 415

Crystal structure of N-antipyrine-3-methanyl-2-thienyldiminato, C17H18N3OS

C17H18N3OS, orthorhombic, P212121 (no. 19), a =6 .892(1) A, b =1 3.422(3) A, c =1 7.279(4) A, V =1 598.3 A 3 , Z =4 , Rgt(F) =0 .039, wRref(F 2 ) =0 .151, T =1 13 K. Source of material Am ixture of 3-methanyl-2-thienyldehyde (5.00 mmol) and 4- aminoantipyrine (5.00 mmol) in methanol (40.00 ml) is refluxed with stirring for one hour to give an orange precipitate. After fil- tration and washing with methanol it yields the pure Schiff base with ay ield of 86 %. Experimental deatils The hydrogen atom H1W was located from difference density map and was refined with d(O1—H1W) =0 .82(2) A.T he hydro- gen atoms on methyl groups were placed in calculated positions with d(C—H) =0 .98 A and Uiso(H) =1 .5 Ueq of the respective carrier atom. All other Ha toms were placed in calculated posi- tions with d(C—H) =0 .95 A and Uiso(H) =1 .2 Ueq of the respec- tive carrier atom. Discussion In the new Schiff base, the equal deviations of fitted atoms for the phenyl, thiophene, and pyrazole planes are 0.005, 0.003, and 0.028 A,r epectively. The dihedral angle between thiophene and pyrazole is 12.3(1)°. The dihedral angle between phenyl and pyrazole is 52.99(9)°. In the asymmetric unit, the imide bond lengths of C12—N3 and C2—N1 are 1.294(3) and 1.396(3) A,r e - spectively. The C—C bond lengths in the phenyl rings are in the range of 1.377(4) -1 .398(3) A.T he C—N and C—C bond lengths in the imidazole ring are in the range of 1.372(3) -1 .404(3) A and 1.369(3) -1 .448(3) A,r espectively. The C—S and C—C bond lengths in the thiopene ring are in the range of 1.711(3) -1 .727(4) A and 1.385(3) -1 .421(4) A,r espectively.

Bis(ethano-lato-κO)(5,10,15,20-tetra-phenyl-calix[4]pyrrole)manganese(III) hexa-fluoro-phosphate.

The title compound, [Mn(C2H5O)2(C44H28N4)]PF6, was synthesized from manganese(III) 2,4-pentanedionate and 5,10,15,20-tetraphenylcalix[4]pyrrole by a hydrothermal reaction. The MnIII atom is located on an inversion centre and the asymmetric unit comprises one half-formula unit. The MnIII ion is hexacoordinated by four N atoms from one 5,10,15,20-tetraphenylcalix[4]pyrrole ligand and two O atoms from two deprotonated ethanol molecules. The equatorially located atoms (the Mn and four N atoms) are planar. The dihedral angles between the planes of the phenyl rings and the equatorial plane are 53.3 (2) and 81.8 (2)°. One hexafluorophosphate anion balances the charge.