Sonochemical technique has lead the synthesis of nano-scale cobalt(III) compounds from pentaammineazidocobalt(III) chloride and sodium salts of metal oxoanions (Na2MO4 center dot 2H(2)O, M = Mo or W) in an aqueous medium. These dark red coloured particles have composition [Co(NH3)(5)N-3]MO4 (M = Mo or W) and further characterization by UV-Vis, IR, SEM, Zeta-sizer and PXRD. Through classical method their crystals have also been grown and their characterization has been done by UV-Vis, IR, PXRD and SCXRD. Thermal stability of single crystalline and nano-scale cobalt(III) compounds have been determined by thermal gravimetric analysis. The binding ability of pentaammineazidocobalt(III) cation for oxoanions has been observed (in an aqueous solution) with UV-Vis spectroscopic titrations (log k = 2.35 (MoO42-), 3.76 (WO42-). Single crystal X-ray structures of both the compounds have revealed the presence of one cation and one anion. Electrostatic forces of attraction and strong H-bonding interactions (N-H center dot center dot center dot O) have stabilized crystal lattices in both the structures. All compounds along with sodium salts of oxoanions has further revealed their antibacterial activities using a strain of gram negative bacteria, a strain of gram positive bacteria and acid fast bacteria (Escherichia coli, Bacillus thuringiensis and Mycobacterium smegmatis respectively). This study predicts that these new nano compounds have two-fold more inhibitory activity as compared to the normal crystalline compounds and sodium salts of oxoanions.

The odd couple: The red chromophore of both the rare silicate mineral gillespite (BaFeSi4O10; see picture, left, on sanbornite, BaSi2O5) and the bis(meso-oxolanediolato)ferrate(II) anion in its lithium salt (right) is the square-planar, high-spin-d6 ferrous center. The unusual combination of structure and spin state for the FeO4 moiety is not forced by a rigid environment of the central metal, but rather results from an intrinsically stable entity.

Ungewöhnliche Kombination: Der rote Chromophor des Silicatminerals Gillespit (BaFeSi4O10, im linken Bild auf Sanbornit, BaSi2O5) und des Bis(meso-oxolandiolato)ferrat(II)-Anions in dessen Lithiumsalz (rechtes Bild) ist das quadratisch-planare High-Spin-d6-Eisen(II)-Zentrum. Die ungewöhnliche Kombination von Struktur und Spin des FeO4-Fragments ist nicht durch eine starre Umgebung des Zentralmetalls erzwungen; vielmehr liegt ein intrinsisch stabiles Baumotiv vor. Detailed facts of importance to specialist readers are published as ”Supporting Information”. Such documents are peer-reviewed, but not copy-edited or typeset. They are made available as submitted by the authors. Please note: The publisher is not responsible for the content or functionality of any supporting information supplied by the authors. Any queries (other than missing content) should be directed to the corresponding author for the article.

N-Nitroso- (5a,c) and N-nitraminotetrazoles (6a-c) were synthesized from the corresponding aminotetrazoles (3a-c) either by the direct nitration with acetic anhydride/HNO3 or by dehydration of the corresponding nitrates (4a-c) with concentrated sulfuric acid. The conversion of the N-nitrosoaminotetrazoles (5a,c) with peroxytrifluoroacetic acid (CF3CO3H) yielded the corresponding nitramines in high yield (6a (82%), 6c (80%)). The N-nitroso- (5a,c) and N-nitraminotetrazoles (6a-c) have been fully characterized by vibrational (IR, Raman) and multinuclear NMR spectroscopy (14N/15N, 1H, 13C), mass spectrometry, and elemental analysis. A detailed discussion of the 15N chemical shifts and 1H-15N coupling constants is given. The molecular structures in the solid state were determined by single-crystal X-ray diffraction (3a,c; 5a,c; 6a-c) and a detailed discussion of the molecular structures will be presented. Furthermore, the structure and bonding as well as N,N rotational barriers are discussed on the basis of theoretically obtained data (B3LYP/6-31G(d,p), NBO analysis). In the case of two N-nitraminotetrazoles (6a,c) the physicochemical properties (e.g., D, P, delta(f)H degrees) were evaluated. The heat of formation was calculated to be positive for 6a and 6c (+2.8 and +85.2 kcal mol(-1), respectively) and the calculated detonation velocity with 5988 (6a) and 7181 (6c) m s(-1) reaches values of TNT and nitroglycerin.

The invention relates to edible film-shaped preparations with cola flavor, which disintegrate rapidly and without leaving a residue on contact with moisture.

AbstractTransmetallation of Tin(II) in [Sn(μ3‐PSitBu3)]4 by Barium – from Sn4P4 Heterocubane Structures to Heterobinuclear Cage Compounds with a Central BanSn4−nP4 Heterocubane Polyhedron (n = 1, 2 and 3)For the preparation of compounds of the type [BanSn4−n(PSitBu3)4] (n = 1 (2), 2 (3) and 3 (4)) two synthetic routes are applicable: in the transmetallation reaction homometallic [Sn4(PSitBu3)4] (1) reacts with barium metal and in a deprotonation reaction (metallation) tri(tert‐butyl)silylphosphane reacts simultaneously with (thf)2Ba[N(SiMe3)2]2 and Sn[N(SiMe3)2]2. During the transmetallation reaction mixtures of the heterobimetallic cage compounds 2 to 4 are obtained, however, analytically pure compounds 2 and 3 are accessible by the metallation reaction. Compound 4 is formed as a minor product together with 3. Due to the larger Ba‐P bond lengths compared to the Sn‐P values the substitution of tin by barium leads to strong distortions of the heterocubane moiety. With NMR‐spectroscopic experiments one could show that all the above mentioned compounds form BanSn4−nP4 heterocubane cage structures.

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

The reaction of alkylzinc triisopropylsilylamide with dialkylmagnesium leads to a ligand exchange. Besides the starting materials, heteroleptic alkylmagnesium triisopropylsilylamide and homoleptic magnesium bis(triisopropylsilylamide) are detected by NMR spectroscopy. After the addition of 1,2-bis(dimethylamino)ethane (TMEDA) to the reaction mixture, (tmeda)Mg[N(H)SiiPr3]2 (1) precipitates as colorless cuboids (C24H60MgN4Si2, a = 2269.6(2), b = 1029.58(5), c = 1593.2(1) pm, beta = 120.826(8) degrees , monoclinic, C2/c, Z = 4). The amide nitrogen atoms are coordinated planarily with strongly widened Mg-N-Si bond angles of 139.2(1) degrees . The metalation of triisopropylsilylamine with dimethylmagnesium in THF yields quantitatively heteroleptic [(thf)MeMg-N(H)SiiPr3]2 (2) which crystallizes as colorless needles (C28H66Mg2N2O2Si2, a = 1982.4(2), b = 2034.1(1), c = 907.22(6) pm, beta = 95.021(9), monoclinic, P2(1)/n, Z = 4). Because of the bridging position of the triisopropylsilylamide anion, the tetracoordinate nitrogen atoms show rather long Mg-N bond lengths of 210.7 pm (average value).

Cyclodextrin ligands: Carbohydrates can be used as framework molecules that provide patterns of metal-binding oxygen atoms. The divalent forms of the biologically important metals iron and manganese can be part of such assemblies (see structure: Fe blue, O red, counterion green, hydrogen bonds between water molecules yellow). The assemblies are stabilized by favorable contributions other than the carbohydrate–metal interaction.

In contrast to the ferrate K-2[Fe(CO)(4)], the phosphane-substituted ferrate K-2[Fe(CO)(3)(PPh3)] (1) reacts with the stibane derivative Ph2SbCl by metal-assisted reductive Sb-Sb coupling to give the distibane complex trans- [Fe(CO)(3)(PPh3) (Sb2Ph4)] (3). The distibane ligand in 3 is terminally eta-coordinated trans to the phosphane ligand. However, the stiborane derivative Me3SbCl2 reacts with 1 in a metathetical substitution reaction to form the monostibane complex trans-[Fe(CO)(3)(PPh3)(SbMe3)] (5). Both compounds have been characterized by spectroscopic (IR, NMR, MS), analytical (C, H) and X-ray diffraction analyses. (C) Wiley-VCH Verlag GmbH Co.

The reaction of [(dme)LiAsH2] with F(3)CSO(3)SitBU(3) yields tri(tert-butyl)silylarsane (1). The reaction of 1 with n-butyllithium. in 1,2-dimethoxyethane gives [(dme)LiAs(H)SitBU(3)](2) (2), whereas the lithiation of 1 in THF leads to the formation of the one-dimensional polymer [(THF)LiAs(H)SitBU(3)](infinity) (3). The Li-As bond lengths of both of these compounds show a similar value of approximately 260 pm. However, the smaller co-ordination number of the lithium atom in 3 leads to a short Li-O distance of 190 pm, whereas in 2, which has a tetracoordinate lithium atom, an average bond length of 199 pm is observed. ((c) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2005).

For the preparation of compounds of the type [BanSn4-n(PSitBu(3))(4)] (n = 1 (2), 2 (3) and 3 (4)) two synthetic routes are applicable: in the transmetallation reaction homometallic [Sn-4(PSitBu(3))(4)] (1) reacts with barium metal and in a deprotonation reaction (metallation) tri(tert-butyl)silylphosphane reacts simultaneously with (thf)(2)Ba[N(SiMe3)(2)](2) and Sn[N(SiMe3)(2)](2). During the transmetallation reaction mixtures of the heterobimetallic cage compounds 2 to 4 are obtained, however, analytically pure compounds 2 and 3 are accessible by the metallation reaction. Compound 4 is formed as a minor product together with 3. Due to the larger Ba-P bond lengths compared to the Sn-P values the substitution of tin by barium leads to strong distortions of the heterocubane moiety. With NMR-spectroscopic experiments one could show that all the above mentioned compounds form BanSn4-nP4 heterocubane cage structures.

AbstractThe dimeric μ2‐amino‐phenoxy complexes of rhenium [(CO)3Re(μ2‐O∩NH2)]2 (1) do not react with the C‐nitroso compounds R−C6H4NO [R = NMe2 (2), H (2′)] in the presence of AlCl3 by a condensation reaction to give the desired azo dye complexes [(CO)3Re(μ2‐O∩N=NC6H4R)]2. Instead, they react to give the novel neutral η2‐N,O‐bridged C‐nitroso complexes [{CO)3ReCl}2ONC6H4R] (3, 3′) by means of a substitution reaction. Both complexes yield golden gleaming crystals, and their solutions are deeply blue (3) or violet (3′) due to the broad UV/Vis absorption at λ = 617 (3) and 505 nm (3′). Single crystals of 3, 3′ show nonlinear optical properties, they are dichroic and have a red and blue (3) or violet and green (3′) side. The molecular structures of 3, 3′ have been determined by single‐crystal X‐ray analyses. Both compounds contain two face‐joined octahedra, with two chloro and the NO ligands as bridges. The C‐nitroso groups together with the NC2 moiety of NMe2 (3) lie almost exactly within the symmetry plane of the molecules. Both the N atoms of 3 have a trigonal‐planar geometry. 3 and 3′ are the first single, neutral and dinuclear C‐nitroso complexes with the rare non‐assisted μ‐(η2‐N,O) bridge and only single atoms as additional bridges. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004)