Reactions of 3d-metal nitrates with N,N′-bis(2-pyridyl)urea (LH2): preparation, X-ray crystal structures and spectroscopic studies of the products trans-[M(II)(ONO2)2(LH2)2] (M=Mn, Fe, Co, Ni, Cu, Zn) and mer-[Co(III)(LH)2](NO3)·MeOH

Zinc tri-tert-butoxysilanethiolates. Syntheses, properties and crystal and molecular structures of [Zn{μ-SSi(OBut)3}(acac)]2 and [{(ButO)3SiS}(H2O)2Zn{μ-SSi(OBut)3}Zn(acac){SSi(OBut)3}]

Syntheses, structures, and photoluminescent properties of four d10 metal-quinolinato coordination polymers with similar rod-like SBUs

The hydrogen-bonding networks for seven new binary compounds of dithiooxamide, (NH2CS)2 (dtox) and dithiobiurea (NH2CSNH)2 (dtur) with crown ethers, 18-crown-6 (18C6), 15-crown-5 (15C5), 12-crown-4 (12C4), cis-syn-cis-(DCHA), and cis-anti-cis-(DCHB) isomers of dicyclohexyl-18 -crown-6 are discussed. (15C5.dtox), (18C6.dtur) and (DCHB.dtur) afford one-dimensional hydrogen-bonded polymeric arrays where the components alternate. In (DCHA.2dtox) and (DCHB.2dtox) the similar hydrogen-bonded chains are further interlinked via dtox molecules to generate layered motifs. In (15C5.2dtur) the dtur molecules are self-assembled into layers via N-H...S hydrogen bonds. 15C5 spacers link adjacent layers into a three-dimensional network. In (12C4.dtur) the dtur molecules are arranged in chains. These chains alternate with the crown molecules attached to them through N-H...O hydrogen bonds in such a way that each 12C4 appears to be linked with four dtur molecules and vice versa thus providing a three-dimensional grid.

From 1D strands to extended molecular assemblies in the binary compounds of dithiooxamide and dithiobiurea with crown ethers

Preparation structural characterization and properties of malonamato(-1) complexes

Transition metal complexes of singly and doubly deprotonated 2-thiooxamic acid

The crystal and molecular structure determination of the title compound, K−SO2NC2H2,M
r=143.21, (1) is part of a series of determinations of N-substituted oxathioamidates. The structure has been refined using single-crystal X-ray diffraction data measured at 295 K [MoKα-radiation with λ=0.71073 A]. The crystals are orthorhombic, space group Pn2la,Z=8, with cell dimensions:a=11.399(2) A,b=22.131(2) A,c=4.021(1) A,V=1014.5(7) A3.D
calc.=1.875 mg m−3, Dobs=1.600 mg m−3,F(000)=576, μ=13.14 cm−1. The final agreement factors for 1979 observed reflections [I>3σ(I)] were:R=0.062 andR
w=0.067. The vibrational spectra confirm the geometrical differences between the two thiooxamidate molecules.

The crystal structure and vibrational spectra of potassium oxathioamidate

Preparation, properties and structural characterization of 2-oxathioamidate complexes

Synthetic procedures are described that allow access to the new monomeric complexes [M(HA)2(H2O)2]·2H2O (M = Mn or Co), [M(HA)2(H2O)2] (M = Fe, Ni or Zn) and [Cu(HA)2], and to the polymeric compounds [MA(H2O)]
 n
 (M = Mn, Co, Ni or Zn) and [CuA]
 n
 , where H2A = N-methyl-2-thiooxamic acid. The X-ray crystal structure of [Mn(HA)2(H2O)2]·2H2O reveals a trans, cis, cis octahedral geometry around the metal ion. The singlydeprotonated ligand behaves as a bidentate chelate with ligated atoms being the neutral thioamide sulfur and one of the carboxylate oxygens. The complexes were characterized by elemental analyses, conductivity measurements, X-ray powder patterns, magnetic susceptibilities and spectroscopic (e.s.r., ligand field, i.r., far-i.r., Raman) studies. The vibrational analysis of the complexes is presented using OH/OD, NH/ND, CH3/CD3 and metal isotopic substitutions. All data are discussed in terms of the nature of bonding in conjunction with known or assigned structures. The dianion A2− acts as a bis-bidentate O,N/O,S bridging ligand yielding highly symmetrical squares planar (CuII) and octahedral (MnII, CoII, NiII and ZnII) polymeric compounds.

Preparation, structural characterization and vibrational spectroscopic studies of transition metal complexes of singly- and doubly-deprotonated N-methyl-2-thiooxamic acid

The title compound (SO2NC4H6) has been prepared and characterized by X-ray diffraction and infra-red and Raman spectra. The structure has been refined using single-crystal X-ray diffraction data measured at 295K [MoKα-radiation with λ=0.71073 A]. The crystals are monoclinic, space groupP21/n,Z=4,a=6.240(2),b=6.786(2),c=19.988(1)A, γ=108.47(2)°,V=802.8(7)A3.Dcalc.=1.566 Mg m−3,F(000)=392, μ=8.582 cm−1. The final agreement factors for 1906 observed refections [I>3σ(I)] were:R=0.030 andRw=0.043. The dihedral angle between de C−C−S−N plane and the C−C−O−O plane is 88.31(4). The potassium atom within the title compound structure has a slightly distorted trigonal bipyramidal coordination. Infrared and Raman spectra of the normal CH3/CD3 and H2O/D2O isotopes and the waterfree compounds at different temperatures made it possible to perform isotopes complete vibrational analysis and clearly shows the very special hydrogen bonded water molecule in the crystal.

Marleen L. B. F. Hereygers

Papers

Transition metal complexes of singly and doubly deprotonated 2-thiooxamic acid

The crystal structure and vibrational spectra of potassium oxathioamidate

Preparation, properties and structural characterization of 2-oxathioamidate complexes

Preparation, structural characterization and vibrational spectroscopic studies of transition metal complexes of singly- and doubly-deprotonated N-methyl-2-thiooxamic acid

Synthesis, crystal and molecular structure and vibrational characterization of N,N-dimethyl-oxathioamidate monohydrate