Andreas Biegerl

Universität Regensburg, Ratisbon, Bavaria, Germany

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Publications (7)14.91 Total impact

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    ABSTRACT: The synthesis and characterization of hybrid polymers combining organic P,P′ (dppe) or N,N′ (pyrazine) ligands and inorganic donors (P4S3) as cross-linkers between copper(I) halide aggregates is described. As a simple model system the reaction of a mixture of P4S3, PEt3, and CuX (X = Cl, Br, I) was studied. According to X-ray diffraction analysis, pseudotetrahedral monomers [CuX(PEt3)2(P4S3)] (1–3) were formed, in which P4S3 coordinates through the apical phosphorus atom. Layering a mixture of P4S3, Ph2PCH2CH2PPh2 (dppe), and toluene with CuCl in MeCN under diffusion conditions gives 1D-[CuCl(dppe)(MeCN)] (6), which contains (Cu2Cl2)2(μ-dppe)2 clusters linked by another dppe ligand. The analogous reaction with CuI gives 1D-[CuI(P4S3)(dppe)] (7), which is built up of alternating trans-(Cu2I2)(P4S3)2 units and dppe linkers. Hybrid polymers 2D-[CuX(P4S3)(dppe)] [X = Br (8), I (9)] are formed if CH2Cl2 is used instead of toluene. The 2D structures of 8 and 9 may be derived from that of 7 by connecting neighboring (CuX)(dppe) strands with pairs of inversely coordinated P4S3 cages. Replacement of dppe by pyrazine (pyz) yields 3D-[(CuCl)4(P4S3)2(pyz)] (10) and 3D-[(CuBr)3(P4S3)(pyz)] (12), respectively. The structure of 10 comprises a 3D network composed of alternating, linked 2D-[(CuCl)2(P4S3)] and 2D-[CuCl(pyz)] layers. The structure of 12 contains cradles built from opposing (CuBr)6 rings and pairwise pyz and P4S3 bridges. These cradles are organized into a 3D framework by condensation of the (CuBr)6 rings, and the layers formed are linked by additional pyz molecules. The resulting voids are occupied by toluene molecules. The behavior of P4S3 and P,P′ or N,N′ ligands as competitive building blocks is also expressed by the formation of binary P4S3/CuX or pyz/CuX polymers.
    Berichte der deutschen chemischen Gesellschaft 09/2011; 2011(27). · 2.94 Impact Factor
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    ABSTRACT: The formation of coordination polymers (CuCl)P4Se3 (1), (CuBr)3(P4Se3)2 (2), (CuI)3(P4Se3)2 (3) and (CuI)P4Se3 (4), from solutions of copper(I) halides and P4Se3 by diffusion methods has been studied. The new compounds were characterized by X-ray crystallography, solid-state 31P MAS NMR and Raman spectroscopy. Theoretical studies on the DFT level in the crystalline phase allowed the unequivocal assignment of the recorded Raman shifts between 200 and 480 cm−1. The structure of 1 consists of a 2D network of castellated [CuCl]n chains and bidentate P4Se3 molecules. The 3D network of 2 comprises [CuBr]n chains, which are linked by tridentate P4Se3 molecules. Compound 3 is a three-dimensional polymer composed of four-membered (CuI)2 rings and castellated [CuI]n chains, which are linked by tridentate P4Se3 molecules involving two basal and the apical P atoms. Thermal conversion of 1 at 230 °C gives (CuCl)3(P4Se3)2 (5), which is isostructural with 2. The thermal conversion of (CuI)3P4S3, which was studied for comparison gave at 371 °C (CuI)3P4S4, Cu3PS4 and small amounts of Cu6PS5I.
    Journal of Solid State Chemistry 07/2011; 184(7):1719–1725. · 2.04 Impact Factor
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    ABSTRACT: ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.
    ChemInform 06/2010; 41(24).
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    ABSTRACT: The formation of a new type of organometallic-inorganic hybrid coordination polymer from P4S3·W(CO)5 (1) and CuI has been studied. The structure of {P4S3·W(CO)5}(CuI) (3) has been verified by the combination of spectroscopic (IR, Raman, 31P MAS NMR) and X-ray diffraction methods. Theoretical studies of β-P4S3, P4S3·W(CO)5 (1), 1D-(P4S3)(CuI) (2), and 3D-(P4S3)(CuI)3 (4), which may be considered as potential building blocks of 3, were carried out on the DFT level in the crystalline phase. The comparison of calculated and measured vibration modes of the P4S3 cage allows the unequivocal assignment of the recorded Raman shifts between 200 and 480 cm–1 and the determination of the degree of integration of P4S3 within the one-dimensional stacks of 2 or copper iodide networks of 3 and 4.
    Berichte der deutschen chemischen Gesellschaft 02/2010; 2010(8):1231 - 1237. · 2.94 Impact Factor
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    ABSTRACT: The formation of coordination polymers from copper(I) bromide and P4S3, a potentially tetradentate P-donor bridging ligand, was studied. Whereas (P4S3)3(CuBr)7 (1) formed in excellent yield, (P4S3)(CuBr)3 (2) and (P4S3)(CuBr) (3) crystallized as mixtures. The new compounds were characterized by X-ray crystallography and solid-state 31P MAS NMR spectroscopy. The structure of 1 consists of a 3D network of cylindrical (CuBr)n columns, castellated (CuBr)n chains and diatomic CuBr units. These building blocks are linked by tetradentate P4S3 molecules. The structure of 2 comprises undulated (CuBr)n layers, which are intra- and interlayer linked by tridentate P4S3 molecules. Compound 3 is a one-dimensional polymer composed of four-membered Cu2Br2 rings, which are bridged by the P3 bases of two P4S3 molecules.
    Zeitschrift für anorganische Chemie 01/2010; 636(5):770-774. · 1.16 Impact Factor
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    ABSTRACT: ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 200 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.
    ChemInform 01/2008; 39(7).
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    ABSTRACT: Layering solutions of P(4)S(3) in CH(2)Cl(2) with solutions of CuCl or CuI in CH(3)CN gives the coordination polymers (P(4)S(3))(3)(CuCl)(7) (1), (P(4)S(3))(2)(CuCl)(3) (2), (P(4)S(3))(CuI) (3) and (P(4)S(3))(CuI)(3) (4), respectively, after slow diffusion. The yellow compounds were characterised by elemental analysis, (31)P magic-angle spinning (MAS) NMR spectroscopy and single-crystal X-ray crystallography. The solid-state structures demonstrate the unexpected ligand versatility of the P(4)S(3) molecule, which interacts through two, three, or even all of the phosphorus atoms with copper according to the nature of the copper halide. Compound 1 has a three-dimensional network in which linear and cylindrical infinite CuCl subunits coexist with diatomic CuCl building blocks. For the first time, all four P atoms of the P(4)S(3) cage are involved in coordination with metal atoms. The 3D structure of 2 contains stacks of P(4)S(3) that are interconnected by slightly undulated and planar [CuCl](n) ribbons. Compound 3 is a one-dimensional polymer composed of alternating (CuI)(2) rings and P(4)S(3) bridges. The structure of 4 consists of undulated [CuI](n) layers in which the P(4)S(3) cage functions as a bridge within the layer, as well as a spacer between the layers. The (31)P MAS NMR spectra obtained are in good agreement with the solid-state structures obtained crystallographically. Thus, analytically pure 3 and 4 show singlet peaks that correspond to uncoordinated P and quartets owing to coupling with (63)Cu and (65)Cu, respectively, whereas that of 1 contains quartets according to all-P coordination. The spectrum of 2 was obtained from a sample that still contained 40 % of 1.
    Chemistry 02/2007; 13(33):9270-6. · 5.83 Impact Factor