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Dimeric mol­ecules of the title compound, [Ru2Cl4(C12H18)2], are located on a crystallographic centre of inversion with one mol­ecule in the asymmetric unit. The hexa­methyl­benzene rings are in an η6-coordination to the ruthenium centres, which are bridged by two chloride ligands. In addition, the ruthenium centres are bonded to another chloride ligand. The aromatic rings and the Ru2Cl2 four-membered ring enclose a dihedral angle of 55.85 (6)°.

The title compound, [Rh(C(15)H(16)PS)(C(18)H(15)P)(CO)], was synthesized from the reaction of the ligand rac-[Ph(2)PCH(2)CH(CH(3))SH] with trans-[Rh(F)(CO)(PPh(3))(2)] in a 1:1 molar ratio in toluene. The Rh atom is four-coordinated in a distorted square-planar geometry with the P-S ligand [Ph(2)PCH(2)CH(CH(3))S] acting as a chelate and the PPh(3) and disordered CO [site occupation factors of 0.61 (5) and 0.39 (5)] ligands completing the coordination.

The title compound, C20H27NOS, was obtained from the corresponding O-thiocarbamate. The structure features a C=O bond distance of 1.209 (2) Å and an sp3-hybridized S atom [C—S—C = 101.66 (1)°]. The steric bulk of the 1-adamantyl substituent on the 2-position of the aromatic ring is reflected in the S—C—C—C torsion angle [−7.5 (3)°].

In the title compound, C24H31BrO4, rings A and C adopt envelope and chair conformations, respectively, and rings B and D both adopt a conformation intermediate between half-chair and envelope. The A/B, B/C and C/D ring junctions are all trans. The molecules in the crystal are held together by van der Waals, C—H⋯Br and C—H⋯O interactions.

A systematic crystallographic study of organotin(IV) complexes of the 1-phenyl-1H-tetrazole-5-thiolato heterocycle (L), has been undertaken in order to examine the metal-ligand bonding behaviour. The structural evidence accumulated from several X-ray determinations of complexes of the type SnR3L and SnR2L2 performed mainly by us, as well as that of dimethylbis(1-phenyl-1H-tetrazole-5-thiolate)tin(IV), SnMe2L2, presented in this manuscript (the first reported with a heterocyclic ligand containing the unit and two non-bulky organic groups), has led to propose a rationalization of the solid-state bonding behaviour of organotin(IV) derivatives toward tetrazolethiolates and closely related ligands.

The following compounds [C4H8Te(Ph2(S)PNP(S)Ph2)2] (1), [C4H8Tel(Ph2(S)PNP(S)Ph2)] (2), [C8H8Tel(Ph2(S)PNP(S)Ph2)] (3), [C4H8Tel(Ph2(Se)PNP(Se)Ph2)] (4), and [(C4H8TeOTeC4H8)2(Ph2(O)PNP(O)Ph2)2][I, I3] (5) were isolated from the reaction of C4H8Tel2 or C8H8Tel2 with the appropriate M[Ph2(X)PNP(X)Ph2] (M= K or Na; X= O, S and Se) salt. The compounds have been characterized by IR, multielemental NMR spectroscopy, positive-ion FAB mass spectrometry and elemental analysis. Compounds 1,3,4 and 5 were also characterized by single-crystal X-ray diffraction analysis. The sulfur and selenium ligands display an asymmetrical chelating coordination mode on interaction with the tellurium center, while two oxygen ligands behave as bridges between two C4H8Te-O-TeC4H8 units, leading to a 16-membered ring.

The reaction of nBuSnCl3 and sodium salt of 2-mercaptoethanol gave the compound Sn(nBu)(Cl){(OCH2CH2S)2Sn(nBu)}2 (1). The compound 2, [(nBu)Sn(SCH2CH2O) SCH2CH2OH], was initially isolated from the reaction of 1, but was also synthesized from another route. Both compounds were characterized by IR, 119Sn, 13C and 1H NMR, FAB mass spectroscopy and elemental analyses and X-ray diffraction of single crystal. 1 is a tri-metallic Tin(IV) compound in which the central atom is in six-fold coordination while the two remaining tin atoms show five-fold coordination. The pentacoordinated tin atoms are bonded to two [OCH2CH2S]−2 ligands forming two stannolanes, which are fused with the hexacoordinated tin atom forming a distannoxane system. This arrangement is quite different from previous staircase structures. NMR data point the same structure in solution. 2 consists of [(nBu)Sn(SCH2CH2O)(SCH2CH2OH)] units, which are associated via intermolecular SnO interactions. The tin atom forms two ‘stannolane’ units by interacti...

The crystal structure of 4-bromo benzoylmethylenediphenyldiphenylphosphinomethylphosphorane was determined by X-ray crystallography. The compound crystallized in a monoclinic system and was characterized thus: P21/c, a = 13.3489(16)A, b = 18.933(2)A, c = 11.3211(14)A, β = 101.735(2)°, Z = 4, V = 2801.4(6)A3. The crystal was solved by direct methods and refined by full-matrix least-squares on F2 to final values of R1 = 0.0379 and wR2 = 0.0682.

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) A, b = 18.437(2) A, c = 9.656(1) A, β = 106.277(6)°, V = 1267.8(3) A3, Z = 4. 2 crystallizes in the monoclinic space group P21/c, with a = 8.064(2) A, b = 18.382(7) A, c = 9.865(5) A, β = 97.81(3)°, V = 1448.8(11) A3, Z = 4. 3 crystallizes in the monoclinic space group P21/c, with a = 11.472(1) A, b = 13.520(1) A, c = 10.088(1) A, β = 112.60(1)°, V = 1444.5(2) A3, Z = 4. 4 crystallizes in the triclinic space group P-1, with a = 4.583(3) A, b = 10.263(3) A, c = 14.396(3) A, α = 77.92(2)°, β = 88.55(4)°, γ = 80.02(4)°, V = 652.1(5) A3, 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.

Zinc(II) and platinum(II) complexes of 1-phenylglyoxal bis(3-piperidylthiosemicarbazone), H2Pgpip, have been prepared and the crystal structures of H2Pgpip and the two metal complexes have been solved. The two arms of H2Pgpip are on the same side of the carbon–carbon backbone and the N(2)H of the phenyl arm hydrogen bonds to the azomethine nitrogen of the aldehyde arm. Loss of the N(2)H hydrogens from both thiosemicarbazone moieties occurs for [Pt(Pgpip)], resulting in coordination of the dianion Pgpip as a tetradentate N2S2 ligand with the expected 5–5–5-chelate ring system. However, [Zn(HPgpip)Cl] involves the monoanion HPgpip on loss of the phenyl arm's N(2)H, resulting in a five-coordinate complex with coordination of the two azomethine nitrogens, a thione sulfur (aldehyde arm), a thiolato sulfur (phenyl arm) and an axial chloro ligand in an approximately square pyramidal arrangement.

Mononuclear and binuclear copper(II) and nickel(II) complexes with 5-methyl-2-hydroxyacetophenone N(4)-substituted thiosemicarbazones have been prepared and characterized. IR and 1H NMR spectra of the N(4)-substituted thiosemicarbazones and their metal complexes, as well as ESR spectra of the mononuclear copper(II) complexes, have been obtained. The crystal structures of 5-methyl-2-hydroxyacetophenone N(4)-dimethylthiosemicarbazone and a representative binuclear copper(II) complex have been acquired, and their structural features are compared to related thiosemicarbazones and previously reported binuclear copper(II) thiosemicarbazone complexes.