Published by De Gruyter

Volume 52 Issue 5

Issue of Zeitschrift für Naturforschung B

Contents
Journal Overview

June 2, 2014

Kantenverknüpfte VO₆-0ktaeder und PO₄-Tetraeder in BaCa(VO)(PO₄)₂ / Edge-Connected VO₆ Octahedra and PO₄ Tetrahedra in BaCa(VO)(PO₄)₂

S. Meyer, Hk. Müller-Buschbaum

Page range: 549-552

Abstract

Single crystals of the new compound BaCa(VO)(PO 4 ) 2 have been prepared by solid state reactions below the melting point of the reactants in evacuated quartz tubes. X-ray investigations led to monoclinic symmetry, space group C 2h 5 - P2 1 /c, a = 7.300(1), b = 7.053(1), c = 14.460(1) Å, β = 101,43(1)°, Z = 4. The crystal structure is characterized by layers of corner-and edge-connected PO 4 tetrahedra and VO 1+5 octahedra. There is an unusually short O(1)-O(4) distance in a VO 6 octahedron of 2.44 Å associated with the sharing of edges with PO 4 tetrahedra. The short V-O distance of 1.61 Å indicates a vanadyl group.

June 2, 2014

Geschlossene ¹_∞[(PtDy₄O₁₆)₄]-Polyedertunnel in Ba₁₃Dy₈Zn₄Pt₄O₃₇ Closed ¹_∞ [(PtDy₄O₁₆)₄] Polyhedra Tunnels in Ba₁₃Dy₈Zn₄Pt₄O₃₇

O. Sfreddo, Hk. Müller-Buschbaum

Page range: 553-556

Abstract

Single crystals of Ba 13 Dy 8 Zn 4 Pt 4 O 37 have been prepared by reaction of mixtures of BaCO 3 , ZnO and DyO 3 at temperatures up to 1225 °C using platinum crucibles. X-ray investigations led to a new crystal structure with tetragonal symmetry, space group C 4h 5 -I4/m, a = 18.659(7), c = 5.734(2) Å, Z = 2. The structure is characterized by PtO 6 and BaO 6 octahedra as well as by tetragonal ZnO 5 pyramids and single capped trigonal prisms of oxygen around dysprosium. The remaining barium positions show coordination numbers of nine and ten. The crystal structure has large ∞ 1 [(PtDy 4 O) 6 ) 4 ] polyhedra tunnels. Considering the ∞ 1 [Ln 4 O 16 ] 20- polyhedra groups some parts of the structure show similarities to BaZnLn 2 O 5 , Ba 5 Zn 4 Ln 8 O 21 and Ba 2 Ln 2 ZnPtO 8 .

June 2, 2014

Preparation and X-Ray Structure of

Tristram Chivers, Masood Parvez

Page range: 557-559

Abstract

The title compound was obtained in 82% yield by the intramolecular cyclization of 4-BrC 6 H 4 C(NSCCl 3 )[N(SiMe 3 ) 2 ] in CH 2 CI 2 at 23°C. It crystallizes in the triclinic system, space group P1̄, a = 7.957(3) Å, b = 10.864(5) Å, c = 5.625(1) Å, α = 95.94(3)°, β = 97.79(2)°, γ = 100.72(3)°, V = 469.2(3) Å 3 , and Z =2. The bond lengths of the planar C 2 N 2 S ring indicate partial π-delocalization.

June 2, 2014

Quaternary Equiatomic Manganese Pnictide Oxides AMnPO (A = La-Nd, Sm, Gd-Dy), AMnAsO (A = Y, La-Nd, Sm, Gd-Dy, U), and AMnSbO (A = La-Nd, Sm, Gd) with ZrCuSiAs Type Structure

Andre T. Nientiedt, Wolfgang Jeitschko, Peter G. Pollmeier, Markus Brylak

Page range: 560-564

Abstract

The 24 title compounds were prepared in well crystallized form by reaction of the rare earth elements (or uranium, respectively), manganese, the pnictide components, and MnO 2 in a NaCl/KCl flux. They crystallize with the tetragonal ZrCuSiAs type structure (P4/nmm, Z = 2), which has been refined from single-crystal X-ray data of NdMnPO (a = 398.9(1), c = 867.4(1) pm, R = 0.026), NdMnAsO (a = 404,9(2), c = 889.3(4) pm, R = 0.025), and NdMnSbO (a = 416.5(1), c = 946.2(2) pm, R = 0.021) for 107, 190, and 124 structure factors, respectively, and 11 variable parameters each. Chemical bonding in these compounds is briefly discussed.

June 2, 2014

Kristallstrukturen von (n-Bu₄N)[B₆Cl₆], (n-Bu₄N)[B₆Br₆] und (Ph₃P=N=PPh₃)[B₆I₆] sowie Schwingungsspektren und Normalkoordinatenanalyse der Hexahalogeno-c/osö-Hexaboratradikalanionen [B₆X₆]^-, X = Cl, Br, I / Crystal Structures of (n-Bu₄N)[B₆Cl₆], (n-Bu₄N)[B₆Br₆], and (Ph₃P=N=PPh₃)[B₆I₆], and Vibrational Spectra and Normal Coordinate Analysis of the Hexahalogeno-closo-hexaborate Radical Anions [B₆X₆]^- , X = Cl, Br, I

V. Lorenzen, W. Preetz

Page range: 565-572

Abstract

Oxidation of hexahalogeno-closo-hexaborates [B 6 X 6 ]2 - , X = Cl, Br, I, with (NH 4 ) 2 [Ce(NO 3 ) 6 ] in ethanol yields coloured radical ions [B 6 X 6 ] - . X-ray structure determina tions have been performed on single crystals of (n-Bu 4 N)[B 6 Cl 6 ] (1) (monoclinic, space group P2 1 /c,a = 13.144(2),6 = 12.594(2),c = 17.688(5) Å, β = 107.29(2)°,Z=4),(n-Bu 4 N)[B 6 Br 6 ] (2) (monoclinic, space group P2 1 /c, a = 13.529(5), b = 13.096(5), c = 17.863(5) Å, β = 107.20(5)°, Z = 4) and (Ph 3 P=N=PPh 3 )[B 6 I 6 ] (3) (triclinic, space group P1̄, a = 9.3137(8), b = 10.6988(10), c = 11.8760 Å , a = 102.220(7), β = 99.34J(8), 7 = 96.030(7)°, Z = 1). The average B-B distances are nearly equal (1.733 Å (1), 1.728 Å (2), 1.728 Å (3)) while the B-X distances increase (1.762 Å (1), 1.912 Å (2), 2.120 Å (3)). Using the molecular parameters, normal coordinate analyses have been performed and a good agreement of observed and calculated frequencies of 10 B and 11 B labelled derivatives has been achieved. The valence force constants f d (BB) and f d (BX) of [B 6 X 6 ] - are 1.17 and 4.17 (X = Cl), 1.18 and 3.34 (Br) and 1.18 and 2.60 mdyn/Å (I), respectively.

June 2, 2014

Synthese und Röntgenstrukturanalyse von [Fe(η⁶-C₆H₄{1,3-(CH3)2})(η⁵ -C₅(C₆H₅)₅]⁺ [FeCl₄]^- / Synthesis and X-Ray Structure Analysis of [Fe(η⁶-C₆H₄{1 ,3 -(CH₃)₂})(η₅-C₅(C₆H₅)5]⁺ [FeCl₄]^-

Herbert Schumann, Alexander Lentz, Roman Weimann

Page range: 573-576

Abstract

Fe[C 5 (C 6 H 5 ) 5 ](CO) 2 Br (1) reacts with m-xylene at 80°C followed by hydrolysis with diluted HCl in the presence of air, to give [Fe(η 6 -C 6 H 4 {1,3-(CH 3 )2})(775-C 5 (C 6 H 5 ) 5 )] + [FeCl 4 ] - (3). The 1 H, 13 CNMR and mass spectra as well as the single crystal X-ray diffraction analysis confirm the proposed sandwich cation structure. 3 crystallizes in the space group P 2 1 /n with a = 984,0(1), b = 2201,0(7), c = 1684,9(2) pm, β = 91,94(1)° and V = 3647(1) x 10 - 30m 3 . The final refinement resulted in R = 0,054 for 2982 observed reflections with F 0 ≥4σ (F 0 )

June 2, 2014

Funktionalisierung und Vernetzung von Poly(silylenmethylenen) Functionalization and Cross-Linking of Poly(silylenemethylenes)

Wolfram Uhlig

Page range: 577-586

Abstract

Functionalized 1,3-disilacyclobutanes (RSiX-CH 2 ) 2 have been prepared by protodesilylation of aminosubstituted 1,3-disilacyclobutanes with triflic acid and by conversions with nucleo philes. The ring-opening polymerisations of these compounds lead to novel high molecular weight poly(silylenemethylenes), which are characterized by a linear structure and alternating silicon and carbon atoms in the main chain. The hydrosilylation reaction between the poly(silylenemethylenes) (RSiH-CH 2 ) n and (RSiVi-CH 2 ) n results in a polymer network which may serve as an interesting preceramic material. The structures of the polymers were proven by NMR spectroscopy ( 29 Si, 13 C, 1 H).

June 2, 2014

The Crystal Structures of Et₂Sn(O₂PMe₂)₂ and Ph₂Sn(O₂PMe₂)₂; Synthesis and Spectral Studies of Ph₂Sn(O₂PMe₂)₂

Abdel-Fattah Shihada, Frank Weller

Page range: 587-592

Abstract

Ph 2 Sn(O 2 PMe 2 ) 2 has been synthesized by the reaction of HO 2 PMe 2 with Ph 2 SnO in toluene or by treating HO 2 PMe 2 with Ph 2 SnCl 2 in methanol. X-ray diffraction studies of Et 2 Sn(O 2 PMe 2 ) 2 and Ph 2 Sn(O 2 PMe 2 ) 2 show that the O 2 PMe 2 ligands function as bidentate bridges between the tin atoms. The ethyl and the phenyl groups are in trans-position in the resulting octahedral environment around tin. Et 2 Sn(O 2 PMe 2 ) 2 crystallizes in the monoclinic space group P2 1 /n (a = 817.11(9), b = 974.1(1), c = 970.1(1) pm, β = 113.749(6)°, Z = 2 and R = 0.032) and consists of a polymeric layer structure with centrosymmetric (SnOPO) 4 sixteen-membered rings. Ph 2 Sn(O 2 PMe 2 ) 2 also crystallizes monoclinically in the space group P2 1 /n (a= 1060.9(1), b = 999.4 (1), c = 1768.9(2) pm, β = 90.93(1)°, Z = 4 and R = 0.057) and has a polymeric ring-chain structure with centrosymmetric (SnOPO) 2 eight-membered rings. The IR and Raman spectra of Ph 2 Sn(O 2 PMe 2 ) 2 have been assigned and discussed in the light of structural information. The Sn(O 2 PMe 2 ) + ion represents the base peak in the mass spectrum of Ph 2 Sn(O 2 Me 2 ) 2 .

June 2, 2014

Dppa als Komplexligand: Metall-Koordination und P-N-Spaltung in Komplexen des Typs [CpM(L)dppa]X (M = Fe, Mn; L = CO, NO) / Dppa as a Ligand: Metal Coordination and P-N Cleavage in Complexes of the Type [CpM(L)dppa]X (M = Fe, Mn; L = CO, NO)

Jan Geicke, Ingo-Peter Lorenz, Petra Mürschel, Kurt Polbom

Page range: 593-603

Abstract

The reactions of [CpMn(CO) 2 (NO)]BF 4 or CpFe(CO) 2 Cl with PPh 2 NHR (R = Ph, PPh 2 ) lead to the salts [CpML(CO)PPh 2 NHR]X with monodentate aminophosphine ligands. In the case of R = PPh 2 (= dppa) the complexes [CpML(dppa)]X with bidentate dppa are also formed. The salt [CpFe(CO)(dppa)]Cl can be deprotonated to give the neutral complex CpFe(CO){(PPh 2 ) 2 N)} with the diphosphinoamide ligand, which can be N-alkylated by Mel to afford [CpFe(CO){(PPh 2 ) 2 NMe}]I. The complex [CpMn(NO)(dppa)]BF 4 undergoes a P-N cleavage reaction by the solvent methanol to form [CpMn(NO)(PPh 2 NH 2 )(PPh 2 OMe)]BF 4 . The non-chelated complexes [CpFe(CO) 2 PPh 2 NHR]Cl are deprotonated by DBU to give the neutral ferrioiminophosphoranes CpFe(CO) 2 PPh2 = NR. For R = PPh2 photolysis leads to CO-elimination and to CpFe(CO)(PPh 2 NPPh 2 ). CpFe(CO) 2 PPh 2 NPPh 2 can be alkylated by Mel or metallated by CpFe(CO) 2 Cl to form [CpFe(CO) 2 PPh 2 NPPh 2 Me]I or [CpFe(CO) 2 PPh 2 NPPh 2 (CO) 2 FeCp]Cl, respectively. Oxidation of CpFe(CO) 2 PPh 2 NPPh 2 is possible by (SiMe 3 ) 2 O 2 , sulfur, or selenium to lead to the neutral complexes CpFe(CO) 2 PPh 2 =NPPh 2 = E (E = O, S, Se) with a heterodiene system. The IR and NMR spectra of all species as well as the X-ray structures of the complexes [CpFe(CO)dppa]Cl, [CpMn(NO)dppa]BF 4 and [CpMn(NO)(PPh 2 NH 2 )(PPh 2 OMe)]BF 4 are reported and discussed.

June 2, 2014

Synthese und Kristallstruktur von 7-Azaindolato-Silber, einem dimeren Ag(I)-Komplex mit kurzem Ag-Ag-Abstand

J. Beck, M. Reitz

Page range: 604-608

Abstract

[Ag(C 7 H 5 N 2 )] 2 is obtained by the slow addition of a tetrahydrofuran (thf) solution of AgClO 4 to a solution of Na(C 7 H 5 N 2 ) in thf. The slightly yellow compound crystallizes in the monoclinic space group P2 1 /n with the lattice constants a = 554.5(1) pm, b = 954.6(2) pm, c = 1196.5(3) pm, β = 99.67(2)°. The structure consists of centrosymmetric, planar, dimeric complexes with ligand disorder in the crystal. The N atoms coordinate the Ag + ions nearly linearly (N-Ag-N = 168°, Ag-N = 213 pm). The Ag + ions in the dimeric unit have a short distance of 284 pm. The complexes are linked by weak intermolecular η 2 -Ag-C interactions to chains.

June 2, 2014

Zur Reaktion von Derivaten des 1,3-Dimethyl-2-iminoimidazolins mit CS₂ [1] / On the Reaction of 1,3-Dimethyl-2-iminoimidazoline Derivatives with CS₂ [1]

Norbert Kuhn, Riad Fawzi, Manfred Steimann, Jörg Wiethoff

Page range: 609-614

Abstract

1,3-Dimethyl-2-iminoimidazoline (4, ImNH) reacts with CS 2 to give the imidazolium salt [ImNH 2 ][(ImNCS 2 ) 2 H] (7) in which two dithioformimide fragments are linked by a hydrogen bridge. From the trimethylsilyl derivative ImNSiMe 3 (11) and CS 2 the adduct ImNSiMe 3 • CS 2 (12) is obtained which reacts with oxygen to give the disulfide (ImNCS 2 ) (14). The X-ray structures of 7 and 14 were determined.

June 2, 2014

Formation and Crystal Structures of the Hydrates of 18-Crown-6 [1]

Antje Albert, Dietrich Mootz

Page range: 615-619

Abstract

The melting diagram of the system 18-crown-6/water has been set up and the existence of four binary hydrates confirmed. Crystal structures have been determined for three of these, in addition to that for the hexahydrate already published. The hydrates are monoclinic, a tetrahydrate (previously reported as a 4.5-hydrate) with space group P2 1 /c and Z = 2 formula units per unit cell, an octahydrate with I2/a and Z = 4, and a dodecahydrate with P2 1 /n and Z= 2. In each structure the crown ether molecule has the (pseudo) D 3d conformation common for many of its complexes, and is immediately hydrogen-bonded by a group of four water molecules in a similar, characteristic pattern. In the tetrahydrate, with one of the waters disordered, the total connectivity is that of a 1D chain, while the overall structures of the octa-and dodecahydrate are 3D networks. Four of the six independent water molecules in the dodecahydrate are linked with each other into a rare 2D ice-like layer.

June 2, 2014

Substituierte 1,2,4-Thiadiazolium-dichloroaurate(I) und -tetra- chloroaurate(III) als Reaktionsprodukte von N-Thiocarbamoyl- benzamidinen mit TetrachIorogold(III)-Verbindungen / Substituted 1,2,4-Thiadiazolium dichloroaurates(I) and -tetrachloroaurates(III) as Products o f the Reaction o f N -Thiocarbam oyl-benzamidines with Tetrachlorogold(III) Compounds

Uwe Schröder, Rainer Richter, Jürgen Hartung, Ulrich Abram, Lothar Beyer

Page range: 620-628

Abstract

The reactions of N-diethylaminothiocarbonyl-benzamidines Et 2 N-C(S)-N=C(NHR)-Ph (1: R = Ph, 2: R = C 3 H 7 , 3: R = H) with gold(III) compounds were studied. Treatment of 1 and 2 with equivalent amounts of tetrachlorogold acid gives 2,3-substituted 5-diethylamino-1,2,4- thiadiazoliumdichloroaurates(I) (1a, 2a). With tetrachlorogold acid in excess 1 yields 2,3-diphenyl- 5-diethylamino-l,2,4-thiadiazolium-tetrachloroaurate(III) 1b. With 3 and Na[AuCl 4 ] bis(3-phenyl-5- diethylamino-1,2,4-thiadiazolium)-chloride-tetrachloroaurate(III) 3b is produced. The structures of la, 2a and 3b were investigated by X-ray structure analysis. In la and 2a the dichloroaurate(I) ions are linear. In the 1,2,4-thiadiazolium cations the N-C-bond lengths alternate characteristically. In 3b the tetrachloroaurate(III) ion is square planar. The 1,2,4-thiadiazolium cation shows a different alternation of N-C bond lengths in comparison with la and 2a which suggests changes in the thiadiazolium ring in 3b to a tautomeric form as confirmed by the localization of the H atom at the N atom in ring position 4 instead of ring position 2. The structures of 1a, 1b, 2a and 3b were confirmed by elemental analysis, ES-MS, FAB-MS, 1 H and 13 C NMR and IR spectroscopy.

June 2, 2014

Neue Synthesen mit Magnesiumhydrid Teil 2: Wege zu neuen komplexen Hydriden und zum Aluminiumwasserstoff / New Syntheses with M agnesium Hydride Part 2: Pathways to New Complex Hydrides and A luminium Hydride

Wilfried Knott

Page range: 629-634

Abstract

The reaction between autocatalytically prepared magnesium hydride (Tego ® Magnan) and aluminium halides in ethers generates a new class of reducing agents, i.e. magnesium aluminium hydridohalides. By choosing dioxane-1,4 as solvent a route to an aluminium hydride dioxane complex is opened. The new reducing agents show outstanding selectivity especially in the field of organosilico-nes, combined with a maximum of safety in their application.

June 2, 2014

Synthese und Kristallstrukturen der neuen Zinn-Chalkogen-Vierringe [{Cp(Ph₃P)Ni}₂Cl₂Sn₂E₂] (E = Se, S) / Synthesis and Crystal Structures of the New Four-M em bered Tin-Chalcogen Rings [{Cp(Ph₃P)Ni}₂Cl₂Sn₂E₂] (E = Se, S)

Harald Kraus, Kurt Merzweiler

Page range: 635-638

Abstract

[{Cp(Ph 3 P)Ni}SnCl 3 ] reacts with Se(SiMe 3 ) 2 within several days to give [{Cp 4 (Ph 3 P) 3 Ni 5 Sn 6 Se 9 ] (1). If the reaction is stopped after 16h, green crystals of the intermediate [{Cp(Ph 3 P)Ni} 2 Cl 2 Sn 2 Se 2 ] (2) can be isolated. According to the X -ray structure determination, 2 consists of a planar Sn 2 Se 2 ring with terminal {Cp(Ph 3 P)Ni} and Cl substituents in a trans arrangement. The analogous reaction of [{Cp(Ph 3 P)Ni}SnCl 3 ] with S(SiMe 3 ) 2 leads to the sulfur derivative [{Cp(Ph 3 P)Ni} 2 Cl 2 Sn 2 S 2 ] 3 which has an analogous structure.

June 2, 2014

Die zu BaMg₂Cu₈V₆O₂₆ isotypen Cadmium-Kupferoxovanadate KCd_0,67Cu_4,33V₃O₁₃, RbCd_0,5Cu_4,5V₃O₁₃ sowie TlCd_0,5Cu_4,5V₃O₁₃ /The BaMg₂Cu₈V₆O₂₆ isotypic Cadmium-Cooperoxovanadates KCd_0,67Cu_4,33V₃O₁₃, RbCd_0,5Cu_4,5V₃O₁₃ and TlCd_0,5Cu_4,5V₃O₁₃ /

B. Mertens, Hk. Müller-Buschbaum

Page range: 639-642

Abstract

Single crystals of KCd 0,67 Cu 4,33 V 3 O 13 (I), RbCd 0,5 Cu 4,5 V 3 O 13 (II) and TlCd 0,5 Cu 4,5 V 3 O 13 (III) have been prepared by crystallization from melts. X-ray analysis led to monoclinic symmetry, space group C 2 2h -P2 1 /m (Nr. 11) and the lattice constants (I) - (III): a = 10.728(1), 10.746(3), 10.746(3), b = 6.155(1), 6 .163(2), 6.175(2), c = 8.363(2), 8.350(2), 8.337(3) Å , β = 97.69(2), 97.73(2), 97.61(5)°, Z = 2. The crystal structures are isotypic to the BaMg 2 CU 8 V 6 O 26 type. Cu 2+ occurs in square pyramidal and unusual trigonal bipyram idal coordination by oxygen . The MgO 6 octahedra of the aristo type BaMg 2 Cu 8 V 6 O 26 are statistically occupied by cadmium and copper. The distortion of the (Cd /Cu)O 6 octahedra is discussed with respect to the polyhedra network.

June 2, 2014

Dicobaltoarsenat -(CoAsO₇) -Baugruppen im Cobaltoxid-Tellurat Co₆O₂[T eO₄(CoAsO₅)₂] / Dicobaltoarsenate - (CoAsO₇) - Groups in the Cobalt Oxide Tellurate Co₆O₂[TeO₄(CoAsO₅)₂]

M. Staack, Hk. Müller-Buschbaum

Page range: 643-646

Abstract

The compound Co 6 O 2 [TeO 4 (CoAsO 5 ) 2 ] has been prepared by solid state reactions. Single crystal X -ray techniques led to orthorhombic symmetry, space group D 18 2h -Cmca, a = 6.020(1), b = 23.763(5), c = 8.841(2) Å , Z = 4. The new structure type contains the hitherto unknown cobaltoarsenate group CoAsO 7 , oxidic oxygen connected exclusively to cobalt, and TeO 6 octahedra.

June 2, 2014

Kondensationsreaktionen von Trifluornitrosomethan CF₃NO mit Sulfanilamid H₂NC₆H₄SO₂NH₂-Darstellung von CF₃NNC₆H₄SO₂NH₂, CF₃NNC₆H₄SO₂NNCF₃, CH₃C(O)N(H)C₆H₄SO₂NNCF₃ und CF₃C(0)N (H)C₆H₄SO₂NH₂ / Condensation Reactions of Trifluoronitrosomethane CF₃NO with Sulfanilamide H₂NC₆H₄SO₂NH₂- Preparation of CF₃NNC₆H₄SO₂NH₂, CF₃NNC₆H₄SO₂NNCF₃, CH₃C(0)N(H)C₆H₄SO₂NNCF₃ and CF₃C(0)N (H)C₆H₄SO₂NH₂

Rolf Minkwitz, Jens Jakob, Andreas Winter

Page range: 647-654

Abstract

We report the condensations of trifluoronitrosom ethane with sulfanilamide. The new compounds p-trifluorom ethylazophenylsulfonamide CF 3 NNC 6 H 4 SO 2 NH 2 , p-trifluorom ethylazosulfonyltrifluorom ethylazobenzole CF 3 NNC 6 H 4 SO 2 NNCF 3 and p-trifluoromethylazosulfonylacetanilide CH 3 C(O)N(H)C 6 H 4 SO 2 NNCF 3 were characterized by elemental analysis, IR, Raman, mass, 1 H , 19 F and 13 C NMR spectroscopy. In addition we present our approach to the preparation of p-trifluorom ethylazosulfonylaniline H 2 NC 6 H 4SO 2 NNCF 3 by using protecting groups for the amino group.

June 2, 2014

Übergangsmetall-substituierte Acylphosphane und Phosphaalkene, XXXIY [1] Methylendiyl(thioxo)- und MethyIendiyl(selenoxo)-λ₅,σ3-phosphorane als μ-Liganden in [(η⁵-C₅H₅)₂Fe₂(CO)₃]-Komplexen. Synthese und Struktur von / Transition Metal Substituted Acylphosphanes and Phosphaalkenes, XXXIV [1] Methylenediyl(thioxo)- and M ethylenediyl(selenoxo)-λ⁵ ,σ³-phosphoranes as μ-Ligands in [(η⁵-C₅H₅)₂Fe₂(CO)₃] Complexes. Synthesis and Structure of

Lothar Weber, Iris Schumann, Matthias H. Scheffer, Hans-Georg Stammler, Beate Neumann

Page range: 655-662

Abstract

The isophosphaalkyne complex (η 5 -C 5 H 5 ) 2 (CO) 2 Fe 2 (μ-CO)(μ-C=PMes) (2a) was converted into the methylenediyl(thioxo)- and methylenediyl(selenoxo)- λ 5 , σ 3 -phosphorane complexes (η5-C 5 H 5 ) 2 (CO) 2 Fe 2 (μ-CO)(μ-C=P(E)Mes) (5a: E = S; 5b E = Se) by oxidation with sulfur or selenium . Reaction of the μ-carbyne complex [(μ75-C 5 H 5 ) 2 (CO) 2 Fe 2 (μ-CO)(μ- CSMe)] + SO 3 CF 3 (1) with tBuP(H)SiMe 3 in the presence of DBU afforded the μ-phosphinocarbyne complex (η 5 -C 5 H 5 ) 2 (CO) 2 Fe 2 (μ-CP(H)tBu] (μ -SMe] (12). μ-Carbene complex (11) was isolated as an initial product of this conversion and fully characterized by single crystal X-ray analysis.

June 2, 2014

Zum Mineral Johillerit verwandte Oxovanadate RbCd₄V₃O₁₂ und TlCd₄V₃O₁₂ / Oxovanadates RbCd₄V₃O₁₂ and TlCd₄V₃ O₁₂ Related to the Mineral Johillerite

B. Mertens, Hk. Müller-Buschbaum

Page range: 663-668

Abstract

Single crystals of I RbCd 4 V 3 O 12 and TlCd 4 V 3 O 12 II have been prepared by solid state reactions in closed iron tubes. The compounds crystallize closely related to the Johillerite structure in the space group C 6 2h - C2/c with I: a = 13.058(3); b - 13.528(3), c = 7 .0 6 0 (2 )Å , β = 114.88(2)°; II: a = 12.999(6), b = 13.527(7), c = 7.055(3) Å , β = 114.88(4)°, Z = 4. Special features are the loss of Cu 2+ in order to gain an additional Cd 2+ position. The crystal structure is discussed with respect to related compounds of the Johillerite type.

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Objective
Zeitschrift fuer Naturforschung B (ZNB) publishes novel research in all areas of inorganic chemistry, organic chemistry, and analytical chemistry. In particular, the journal focuses on solid state chemistry, coordination chemistry, main group element chemistry, synthetic organic chemistry, natural product chemistry and, to a lesser extent, on analytical chemistry. For more than 65 years Zeitschrift fuer Naturforschung B has been open to contributions from all fields of experimental and theoretical chemistry. Zeitschrift fuer Naturforschung B publishes 12 issues per volume/year. Sometimes double issues occur.

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Solid state chemistry
Coordination chemistry
Main group element chemistry
Organic chemistry
Natural product chemistry

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Volume 52 Issue 5

Issue of Zeitschrift für Naturforschung B

Kantenverknüpfte VO6-0ktaeder und PO4-Tetraeder in BaCa(VO)(PO4)2 / Edge-Connected VO6 Octahedra and PO4 Tetrahedra in BaCa(VO)(PO4)2

Abstract

Geschlossene 1∞[(PtDy4O16)4]-Polyedertunnel in Ba13Dy8Zn4Pt4O37 Closed 1∞ [(PtDy4O16)4] Polyhedra Tunnels in Ba13Dy8Zn4Pt4O37

Abstract

Preparation and X-Ray Structure of

Abstract

Quaternary Equiatomic Manganese Pnictide Oxides AMnPO (A = La-Nd, Sm, Gd-Dy), AMnAsO (A = Y, La-Nd, Sm, Gd-Dy, U), and AMnSbO (A = La-Nd, Sm, Gd) with ZrCuSiAs Type Structure

Abstract

Abstract

Synthese und Röntgenstrukturanalyse von [Fe(η6-C6H4{1,3-(CH3)2})(η5 -C5(C6H5)5]+ [FeCl4]- / Synthesis and X-Ray Structure Analysis of [Fe(η6-C6H4{1 ,3 -(CH3)2})(η5-C5(C6H5)5]+ [FeCl4]-

Abstract

Funktionalisierung und Vernetzung von Poly(silylenmethylenen) Functionalization and Cross-Linking of Poly(silylenemethylenes)

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The Crystal Structures of Et2Sn(O2PMe2)2 and Ph2Sn(O2PMe2)2; Synthesis and Spectral Studies of Ph2Sn(O2PMe2)2

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Dppa als Komplexligand: Metall-Koordination und P-N-Spaltung in Komplexen des Typs [CpM(L)dppa]X (M = Fe, Mn; L = CO, NO) / Dppa as a Ligand: Metal Coordination and P-N Cleavage in Complexes of the Type [CpM(L)dppa]X (M = Fe, Mn; L = CO, NO)

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Synthese und Kristallstruktur von 7-Azaindolato-Silber, einem dimeren Ag(I)-Komplex mit kurzem Ag-Ag-Abstand

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Zur Reaktion von Derivaten des 1,3-Dimethyl-2-iminoimidazolins mit CS2 [1] / On the Reaction of 1,3-Dimethyl-2-iminoimidazoline Derivatives with CS2 [1]

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Formation and Crystal Structures of the Hydrates of 18-Crown-6 [1]

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Neue Synthesen mit Magnesiumhydrid Teil 2: Wege zu neuen komplexen Hydriden und zum Aluminiumwasserstoff / New Syntheses with M agnesium Hydride Part 2: Pathways to New Complex Hydrides and A luminium Hydride

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Synthese und Kristallstrukturen der neuen Zinn-Chalkogen-Vierringe [{Cp(Ph3P)Ni}2Cl2Sn2E2] (E = Se, S) / Synthesis and Crystal Structures of the New Four-M em bered Tin-Chalcogen Rings [{Cp(Ph3P)Ni}2Cl2Sn2E2] (E = Se, S)

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Die zu BaMg2Cu8V6O26 isotypen Cadmium-Kupferoxovanadate KCd0,67Cu4,33V3O13, RbCd0,5Cu4,5V3O13 sowie TlCd0,5Cu4,5V3O13 /The BaMg2Cu8V6O26 isotypic Cadmium-Cooperoxovanadates KCd0,67Cu4,33V3O13, RbCd0,5Cu4,5V3O13 and TlCd0,5Cu4,5V3O13 /

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Dicobaltoarsenat -(CoAsO7) -Baugruppen im Cobaltoxid-Tellurat Co6O2[T eO4(CoAsO5)2] / Dicobaltoarsenate - (CoAsO7) - Groups in the Cobalt Oxide Tellurate Co6O2[TeO4(CoAsO5)2]

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Zum Mineral Johillerit verwandte Oxovanadate RbCd4V3O12 und TlCd4V3O12 / Oxovanadates RbCd4V3O12 and TlCd4V3 O12 Related to the Mineral Johillerite

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Kantenverknüpfte VO₆-0ktaeder und PO₄-Tetraeder in BaCa(VO)(PO₄)₂ / Edge-Connected VO₆ Octahedra and PO₄ Tetrahedra in BaCa(VO)(PO₄)₂

Geschlossene ¹_∞[(PtDy₄O₁₆)₄]-Polyedertunnel in Ba₁₃Dy₈Zn₄Pt₄O₃₇ Closed ¹_∞ [(PtDy₄O₁₆)₄] Polyhedra Tunnels in Ba₁₃Dy₈Zn₄Pt₄O₃₇

Synthese und Röntgenstrukturanalyse von [Fe(η⁶-C₆H₄{1,3-(CH3)2})(η⁵ -C₅(C₆H₅)₅]⁺ [FeCl₄]^- / Synthesis and X-Ray Structure Analysis of [Fe(η⁶-C₆H₄{1 ,3 -(CH₃)₂})(η₅-C₅(C₆H₅)5]⁺ [FeCl₄]^-

The Crystal Structures of Et₂Sn(O₂PMe₂)₂ and Ph₂Sn(O₂PMe₂)₂; Synthesis and Spectral Studies of Ph₂Sn(O₂PMe₂)₂

Zur Reaktion von Derivaten des 1,3-Dimethyl-2-iminoimidazolins mit CS₂ [1] / On the Reaction of 1,3-Dimethyl-2-iminoimidazoline Derivatives with CS₂ [1]

Synthese und Kristallstrukturen der neuen Zinn-Chalkogen-Vierringe [{Cp(Ph₃P)Ni}₂Cl₂Sn₂E₂] (E = Se, S) / Synthesis and Crystal Structures of the New Four-M em bered Tin-Chalcogen Rings [{Cp(Ph₃P)Ni}₂Cl₂Sn₂E₂] (E = Se, S)

Dicobaltoarsenat -(CoAsO₇) -Baugruppen im Cobaltoxid-Tellurat Co₆O₂[T eO₄(CoAsO₅)₂] / Dicobaltoarsenate - (CoAsO₇) - Groups in the Cobalt Oxide Tellurate Co₆O₂[TeO₄(CoAsO₅)₂]

Zum Mineral Johillerit verwandte Oxovanadate RbCd₄V₃O₁₂ und TlCd₄V₃O₁₂ / Oxovanadates RbCd₄V₃O₁₂ and TlCd₄V₃ O₁₂ Related to the Mineral Johillerite