A. B. Ilyukhin

COMPLEXES OF BISMUTH(III) WITH AMINOPOLYCARBOXYLIC ACIDS. CRYSTAL STRUCTURES OF GUANIDINIUM AQUA(ETHYLENEDIAMINETETRAACETATO)BISMUTHATE(lll) AND AMINOGUANIDINIUM ETHYLENEDIAMINETETRAACETATOBISMUTHATE(III)

In the crystal structure of guaninidium aqua(ethylenedi9minetetraacetato)bismuthate(III), the ethylenediaminetetraacetato tetraanion chelates to the bismuth atom through its two amino and four carboxyl oxygen atoms. A carboxylate bridge [Bi-0 = 2.694(4) A] links adjacent water-coordinated [Bi-Owater = 2.673(4) A] ethylenediaminetetraacetatobismuthate(III) anions into a helical linear chain. The bismuth atom is eight-coordinate in a square-antiprismatic environment. The bismuth atom shows dodecahedral coordination in aminoguanidinium ethylenediaminetetraacetatobismuthate(III). The crystal structure features a short carboxyl bridge [Bi-O = 2.657(4) A] that links the bismuthate anions into a dinuclear entity; adjacent entities are linked by a long carbonyl bridge [Bi-0 = 2.931(4) A] into a linear chain. In both ethylenediaminetetraacetatobismuthates(III), the lone-pair of electrons is stereochemical^ inert.

The crystal structure of aluminium, iron (III), and gallium acid phosphites

The structures of three acid phosphites of trivalent metals [Al(HPO3H)3(H2O)] · H2O (I), K[Fe(HPO3H4)] (II), and Rb3[Ga(HPO3H)6] (III) have been determined. Structure I is layered, complex anions [Fe(HPO3H)4]− form polymer chains in structure II, and structure III is insular.

Products of reaction between Bis(citrate)hydroxogermanic acid and organic molecules. Molecular and crystal structure of (HNad)2[Ge(HCit)2] · 4H2O

Onium bis(citrate)germanates (HNad)2[Ge(HCit)2] · 4H2O (I), (HIm)2[Ge(HCit)2] · 2H2O (II), and (HInd)2[Ge(HCit)2] · 2H2O (III) (where Nad is nicotinamide, Im is imidazole, and Ind is isoniazid) were synthesized by the reaction between bis(citrate)hydroxogermanic(IV) acid (H5O2)[Ge(OH)(H2Cit)(H2.5Cit)]2 · 2CH3COOH · 2H2O (H4Cit is citric acid) and organic bases. The complexes were characterized by elemental analysis, thermogravimetry, and IR spectroscopy. The X-ray diffraction analysis of complex I was performed. The structural units of a crystal of complex I were found to be centrosymmetric complex [Ge(HCit)2]2− anions, HNad+ cations, and crystallization water molecules.

Aminoguanidinium (ethylenediamine-N, N, N', N'-tetraacetato)antimonate(III) monohydrate

In the title complex, (CH 7 N 4 )[Sb(C 10 H 12 N 2 O 8 )].H 2 O, the lone-pair electrons of the Sb atom occupy an axial site in the ψ-pentagonal bipyramidal polyhedron [Sb-N 2.265 (2)-2.507 (2) and Sb-O 2.144 (1)-2.543 (2) A]. The (ethylenediaminetetraacetato)antimonate anion, the aminoguanidinium cation and the lattice water are linked by hydrogen bonds into a two-dimensional network structure.

Synthesis, properties, and crystal structure of barium 1-oxyethylidenediphosphonatohydroxogermanate(IV) polyhydrate Ba3[Ge(μ-OH)(μ-Oedph)]6 · 25H2O

The barium salt of 1-oxyethylidenediphosphonatohydroxogermanium acid Ba3[Ge(μ-OH)(μ-Oedph)]6 · 25H2O (I) (H4Oedph is 1-oxyethylidenediphosphonic acid) was synthesized and studied by X-ray diffraction. The complex was characterized by elemental analysis, thermogravimetry, and IR spectroscopy. The hexanuclear cyclic complex anions [Ge(μ-OH)(μ-Oedph)]66-t-] cations, and water molecules of crystallization are the structural units of the crystal of I.

Synthesis and crystal and molecular structure of three heterometallic polymeric compounds {Ln2[LnGe6(μ-Oedph)6(μ-O)3(μ-OH)3(H2O)4] · xH2O}n [Ln = Nd, x ∼ 26 (I); Er, x ∼ 24 (II); Tm, x ∼ 20 (III); H4Oedph = 1-hydroxyethylidenediphosphonic acid]

The synthesis and X-ray diffraction study of three heterometallic compounds of general formula {Ln2[LnGe6(μ-Oedph)6(μ-O)3(μ-OH)3(H2O)4] · xH2O}n [Ln = Nd, x ∼ 26 (I); Er, x ∼ 24 (II); Tm, x ∼20 (III); H4Oedph = 1-hydroxyethylidenediphosphonic acid] are performed. The basis element of structures I–III is a hexanuclear complex anion [Ge(μ-Oedph)(μ-O)0.5(μ-OH)0.5]69−, in which bridging hydroxo and oxo ligands are statistically disordered with equally probability. Hexameric units are connected by Ln1(H2O)4 fragments into a framework whose channels are completely populated by disordered lanthanide atoms and water molecules.

Synthesis and physicochemical characterization of a porous coordination polymer of Sn-Cu xylarate: The structure of [Sn4Cu8.5(HL)2(L)4O2(OH)(H2O)12.5] · 17.2H2O

A porous coordination polymer of Sn-Cu xylarate [Sn4Cu8.5(HL)2(L)4O2(OH)(H2O)12.5] · 17.2H2O (H5L is xylaric acid) is synthesized for the first time and characterized by chemical analysis, IR spectroscopy, and X-ray diffraction. Centrosymmetric heterometallic fragments [Sn4Cu6(HL)2(L)4O2(H2O)6] (A) including copper Cu1–3 and tin Sn1,2 atoms are distinguished in the structure. The Cu4(OH)0.5(H2O)2.5 bridges connect A units into chains running along the c axis, and the Cu5(OH)(H2O) bridges connect A fragments into layers perpendicular to the c axis. The Cu4,5 atoms form a framework whose voids accommodate the crystallization water molecules.

Synthesis and crystal structure of the [WOCl3{PhNHC(O)CHC(O-)Me}] complex

The [WOCl3{PhNHC(O)CHC(O−)Me}] complex has been synthesized, and its crystal structure has been determined. The coordination polyhedron of the tungsten atom is a distorted octahedron with a meridional arrangement of three chlorine atoms. Two oxygen atoms of the acetoacetanilide bidentate chelating ligand occupy trans positions to the O(3) oxo atom and the Cl(3) atom. The crystal structures and the IR spectra of the WOCl3{PhNHC(O)CHC(Ot-)Me} and [MoO2Cl2{(o-MePh)NHC(O)CH2C(O)Me}] complexes are compared.

Structural features of copper(II) and lanthanide(III) tartratogermanate(IV) complexes

Four heterometallic tartratogermanate complexes, namely [Cu2Ge2(Tart)3(H2O)10]n · 3nH2O and (H3O)[LnGe2(Tart)3(H2O)6] · nH2O (Ln3+ = Gd, n = 3.5; Tm, n = 3; Yb, n = 3), have been prepared via the reaction between germanium tetrachloride and D-tartaric acid (H4Tart) in aqueous acetic acid. All complexes contain {Ge2(Tart)3}n4n- polymer chains. The Cu2+ and Ln3+ atoms coordinate only Tart carbonyl oxygen atoms.

Crystal structure of complexes of bivalent Co, Ni, and Cd with anions of benzoic and 2-(acetylamino)-5-nitrobenzoic acids

The structure of three complexes of bivalent metals (cobalt, nickel, and cadmium) with anions of benzoic (HL1) and 2-(acetylamino)-5-nitrobenzoic (HL2) acids, namely, [Co21 (H2O)2(μ-C4H4N2)]n (I), [NiL2(H2O)5]L2 · 2H2O (II), and [Cd(μ-L2)2(H2O)2]n · 2nH2O (III), is determined. In chainlike structure I, cobalt atoms are connected by bridging pyrazine molecules; structure II contains isolated complexes. In structure III, centrosymmetric (CdOCO)2 cycles and polymeric ribbons are formed due to the coordination of the carboxylate group of the L2 ligand to two cadmium atoms.