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The crystal structure of the Cu(I) mixed ligand salt, [Cu(MeCN)2(PPh3)2](CF3SO3), 1, was determined using single crystal X-ray diffraction, a = 23.249(2), b = 26.665(1), c = 19.4201(9) Å β = 102.614(1) Å, in the P21/c space group. The packing of this complex is quite similar to the PF6 −, BF4 −, and ClO4 − analogs but contains three crystallographically unique [Cu(MeCN)2(PPh3)2](CF3SO3) complexes per asymmetric unit (instead of one). Upon dissolution and recrystallization of this salt in either toluene or tetrahydrofuran, anion (and solvent) coordination results in the formation of two new neutral species Cu(PPh3)2(CF3SO3)(MeCN) 2 and Cu(PPh3)2(CF3SO3)(THF) 3, respectively. Both 2 and 3 crystallize in the orthorhombic Pca21 space group with a = 22.533(1), b = 9.0688(5), c = 18.4689(9) Å, and a = 22.434(1), b = 8.9789(5), c = 18.418(1) Å, respectively. With the perchlorate anion, [Cu2(ClO4)(MeCN)(PPh3)4(THF)](ClO4) 4, is isolated, which crystallizes in the monoclinic space group C2/c with a = 27.308(1), b = 28.064(1), c = 21.448(1) Å, and β = 120.342(1)°. Surprisingly, it is comprised of an analogous solvent coordinated neutral molecule, Cu(PPh3)2(THF)0.8(MeCN)0.2(ClO4) together with an anion-bridged dimeric species, [Cu2(PPh3)4(MeCN)1.6(THF)0.4(ClO4)]+, charge balanced by one additional non-coordinated ClO4 − anion. The coordinated solvent molecules are disordered in both moieties. Compounds 1–3 were further characterized using thermal gravimetric analysis.

The crystal structure of dichloro-(N,N,N′,N′-tetramethylethylenediamine)zinc(II), C6H16Cl2N2Zn, has been determined from 1684 reflexions measured on a Siemens four-circle diffractometer (A.E.D.) using the ω/2θ-scan technique and CuKα radiation. The crystals are monoclinic, space groupP21/c,a = 7·716(3),b = 13·335(9),c =11·545(5) Å, β = 105·59(6) ° andZ = 4. The structure was solved by Fourier methods, and refined by full-matrix least squares to a finalR (conventional) of 6·7 %. Anisotropic thermal parameters were evaluated for the non-hydrogen atoms, but the hydrogen atoms were assigned the equivalent isotropic thermal parameters of the carbon atoms to which they were bonded. The geometry around the zinc atom is distorted tetrahedral, with the Zn-Cl and Zn-N average bond lengths of 2·207(4) and 2·08(1) Å respectively.

C14H17N3OS,M r+275.37, CAD4F diffractometer. CuKα,T+293K.cis: orthorhombic, Fdd2,a+22.166(2),b+48.948(3), andc+5.165(1)Å: finalR+0.045 for 2519 observed reflections,trans: triclinic, $$P\bar 1$$ ,a+11.375(2),b+11.388(2),c+11.823(1)Å, α=110.72(1), β=89.97(1) and γ=93.86(2)o; final R=0.043 for 3993 observed reflections. Structures were wolved with direct methods and refined by full-matrix least-squares with anisotropic thermal parameters for non-H-atoms. The molecules of the studied isomers have very similar conformations, except for the obvious difference in the bicyclic system junction. Similar orientations of a flexible phenylcarbamoyl substituent results from an intramolecular hydrogen bond S...H−N(carbamoyl). Generally, molecules of thetrans form are flat and those ofcis are not. The observation may be of pharmacological importance as thetrans isomer is a far more potent tuberculostatic agent than thecis.

The crystal and molecular structure of 3-phenyl-7-bromoisoxazolo[4,5-d]-pyridazin-4(5H-one, C11H6BrN3O2, has been determined from two- and three-dimensional X-ray data and refined by Fourier and least-squares methods toR = 0·101 for 1187 observed reflexions. Crystals of 3-phenyl-7-bromoisoxazolo-[4, 5-d]pyridazin-4(5H)-one are monoclinic:a = 7·67,b = 6·84,c = 20·52 Å, β = 91·5 °,Z = 4, space groupP21/c. The benzene ring makes an angle of 4·5 ° with the plane of the isoxazole ring, and the other part of the molecule is slightly non-planar. The bond distances and angles compare well with those of other similar molecules. Two N-H...O hydrogen bonds join the two molecules related by a centre of symmetry. Close molecular packing is found in layers parallel to (100).

The crystal and molecular structure of 3,5-cycloandrostan-6β-ol-17-one has been determined by X-ray analysis,13C-NMR,1H-NMR, IR and elemental analyses. The compound was obtained from dehydroepiandrosterone (DHEA) via the 3β-tosyl derivative by refluxing in a butan-2-one/water mixture. The X-ray analysis shows that the planar cyclopropane ring is predominantlyα orientated and the formation of the C(3)-C(5) bond enables the A ring to adopt a distorted boat conformation. Spectroscopic evidence for the presence of the cyclopropane ring and the 6β-hydroxy group are presented.

The hydrogen acceptor capability of the sulfur atom in the biologically relevant N-2-pyridylmethyl-N′-arilthioureas was explored. N-2-Pyridylmethyl thioreas were selected to avoid the formation of intramolecular six-membered hydrogen-bonded ring. The compounds studied were N-2-pyridylmethyl-N′-phenylthiourea (1), N-2-pyridylmethyl-N′-2-methoxythiourea (2), N-2-pyridylmethyl-N′-4-methoxyphenylthiourea (3), and N-2-pyridylmethyl-N′-4-bromophenylthiourea (4). 1 crystallizes in the monoclinic space group P21/c, with a = 7.419(1) Å, b = 18.437(2) Å, c = 9.656(1) Å, β = 106.277(6)°, V = 1267.8(3) Å3, Z = 4. 2 crystallizes in the monoclinic space group P21/c, with a = 8.064(2) Å, b = 18.382(7) Å, c = 9.865(5) Å, β = 97.81(3)°, V = 1448.8(11) Å3, Z = 4. 3 crystallizes in the monoclinic space group P21/c, with a = 11.472(1) Å, b = 13.520(1) Å, c = 10.088(1) Å, β = 112.60(1)°, V = 1444.5(2) Å3, Z = 4. 4 crystallizes in the triclinic space group P-1, with a = 4.583(3) Å, b = 10.263(3) Å, c = 14.396(3) Å, α = 77.92(2)°, β = 88.55(4)°, γ = 80.02(4)°, V = 652.1(5) Å3, Z = 2. Both thiourea N–H groups form intermolecular hydrogen bonds, one with the thione sulfur atom and the other with the pyridine nitrogen atom but the H-bonding schemes are not the same maybe due to the flexibility of the molecules.

The X-ray structures of four pharmacologically active lidocaine analogs, containing substituted pyrazole moieties as the basic residue and an o-nitrophenyl moiety as the hydrophobic residue, have been determined. They are 2-(pyrazol-1-yl)-2′-nitroacetanilide (1), 2-(3,5-dimethyl-pyrazol-1-yl)-2′-nitroacetanilide (2), 2-(3,5-dimethyl-4-iodo-pyrazol-1-yl)-2′-nitroacetanilide (3), and 2-(3,5-dimethyl-4-nitro-pyrazol-1-yl)-2′-nitroacetanilide (4). Crystal data are 1: space group Pn with a = 4.6944(1), b = 22.3890(3), c = 15.7481(2) Å, β = 96.810(1)°, Z = 6; 2: P $$\overline {\text{1}} $$ with a = 4.7277(2), b = 11.6878(5), c = 12.0355(6) Å, α = 87.689(2), β = 85.048(2), γ = 85.975(2)°, Z = 2; 3: I2/a with a = 24.108(5), b = 4.7321(9), c = 25.337(5) Å, β = 96.09(3)°, Z = 8; 4: P21 with a = 5.7788(2), b = 8.9844(3), c = 14.0304(5) Å, β = 101.611(1)°, Z = 2. Molecules of compound 1 adopt a unique, folded conformation stabilized by intramolecular hydrogen bonds and the crystal structure lacks significant intermolecular interactions. In contrast, molecules of 2–4 adopt common, extended conformations and their crystal structures are based on linear arrays of hydrogen bonded (N—H...O=C) molecules. Compound 3 displayed the highest local anesthetic activity while 2 was the most active in tests for anti-arrhythmic effects.

N 1-acetylacetamidrazones and N 1-benzoylacetamidrazones (1a–d) were characterized by 1H and 13C NMR spectroscopy. The actual tautomeric form present has been shown to be the amide hydrazone. NMR spectra of N 1-acetylacetamidrazones (1a,b) showed the existence of Z and E isomers in solution, while N 1-benzoylacetamidrazones (1c,d) were present as Z isomers. The crystal structures of the amidrazones have been determined at 173 and 293 K, respectively. The amidrazones 1c and 1d crystallize in the monoclinic system: in particular for 1c space group P21/c, with a = 11.016(5), b = 20.594(14), c = 13.657(7) Å β = 98.29(3)° V = 3066(3) Å3 and D c = 1.243 g/cm3 for Z = 4; for 1d space group P21/a, with a = 9.410(5), b = 10.449(3), c = 14.295(11) Å β = 101.04(5)° V = 1380(1) Å3 and D c = 1.220 g/cm3 for Z = 4. The X-ray diffraction analysis carried out on 1c has shown the presence of three molecules in the asymmetric unit which differ for the orientation of the phenyl ring.