bluuebunny/crossref_metadata_2025 huggingface dataset:
Synthese und Kristallstruktur von (Ph3PAu)4[AuMn(CO)5]2 und (Ph3PAu)3Re(CO)4/ Synthesis and Crystal Structure of (Ph3PAu)4 [AuMn(CO)5]2 and (Ph3PAu)3Re(CO)4
Authors: Richter Markus , Fenske Dieter , Strähle Joachim
Published: February 2015

The reaction of [Mn(CO)5]- with the cluster cation [(Ph3PAu)8]2+ in thf yields the heterometallic cluster [(Ph3PAu)4 [AuMn(CO)5]2 (1) as the main product besides small amounts of (Ph3PAu)3Mn(CO)4. The former crystallizes as 1-thf in form of red blocks in the triclinic space group P1 with a = 1391,0( 1), b = 1426.7( 1), c = 2308.3(2) pm, α = 92.87(1), β = 97.54( 1), γ = 96.43(1)° and Z = 2. The inner Au6 skeleton of the almost centrosymmetrical cluster consists of two Au4 tetrahedra sharing one edge. Two gold atoms bind a Mn(CO)5 fragment, whereas to the other four gold atoms phosphine ligands are coordinated. The Au-Au distances range from 263.2(1) to 281.9(1) pm, and the Au-Mn distances are 256.6(3) and 256.9(2) pm. By the reaction of [(Ph3PAu)8]2+ with [Re2(CO)9]2- the cluster (Ph3PAu)3Re(CO)4 (2) is obtained in low yield besides the homometallic cluster [(AuPPh3)7]+ as the main product. 2 crystallizes from toluene as 2 C7H8 in the form of yellow blocks with the orthorhombic space group Pna21, and a = 1758.7(3), b = 1648.7(5), c = 2049.3(5) pm. The four metal atoms form a planar lozenge with the Re atom in equatorial position. The Re-Au distances range from 271.2(1) to 273.7(1) pm, and the Au-Au distances are 278.2(1) and 278.4(1) pm
Metallkomplexe von biologisch wichtigen Liganden, CXXIX [1]. Palladium(II)-und Platin(II)-Komplexe von 4,4-disubstituierten Oxazolonen und C2-symmetrischen Bis(oxazolonen) Metal Complexes of Biologically Important Ligands, CXXIX [1]. Palladium(II) and Platinum(II) Complexes of 4,4-Disubstituted Oxazolones and of C2-Symmetric Bis(oxazolones)
Authors: Bauer Werner , Ponikwar Walter , Beck Wolfgang
Published: February 2015

4-Benzyl-4-methyl-2-phenyl-5(4H)-oxazolone (1) forms with the chloro bridged compounds [R3PMCl2]2 (M = Pt, Pd) the complexes Cl2Pt(PR3)(l) (R = Et, nBu) and Cl2Pd(PEt3)(l). The enantiomeric pure C2-symmetric CMe2 bridged bis(oxazolones) 5 and 6 have also been employed which give with PdCl2 the chelate complexes 13 and 14. The X-ray structural determination of Cl2P d[O-C (O)-CMe2-N=C-CMe2-C=N-CMe2-C (O)-O ] (10) shows that one of the methyl group of the CMe2 bridge is located near the palladium atom. This can also be detected in the 1H NMR spectrum.
Synthese und Komplexierung Phosphorylierter spacer-modifizierter Glucosederivate/ Synthesis and Complexation of Spacer Modified Phosphorylated Glucose Derivatives
Authors: Siedentop Tjark , Neda Ion , Schmutzler Reinhard
Published: February 2015

Treatment of the spacer modified glucose derivative 1 with diethylaminotrimethylsilane furnished the bis-silylated molecule 2. Reaction of 2 with two equivalents of the phosphorus compounds 3, 4, and 5 led to the spacer phosphorylated glucosyl derivatives 6, 7 and 8. Complexation of 6 with (COD)PtCl2 gave complex 9; the cis-conformation of 9 could be confirmed by 31P NMR investigations
Synthesis, Complex Formation and Spectral Investigation of New Tritopic Bis(Crown Ether) Compounds Containing Recognition Sites for Sodium and Nickel Guest Cations*
Authors: Hayvali Zeliha , Gündüz Necla , Kilic Zeynel , Weber Edwin
Published: February 2015

New bis(crown ether) ligands (1 - 3) of Schiff base type containing recognition sites for sodium and nickel guest cations have been synthesized by the condensation of two equivalents of 4′-formyl-5′-hydroxy(benzo-15-crown-5)with 1,5-diamino-3-azapentane, 1,8-diamino-3,6- diazaoctane or 1,8-diamino-3,6-dioxaoctane. Homonuclear ditopic crystalline 2:1 (Na+:ligand) complexes (1a - 3a) of the ligands with NaClO4 have been prepared. Heteronuclear tritopic crystalline 2:1:1 (Na⊕ : Ni2⊕ : ligand) complexes (2b and 3b) have also been synthesized from the reactions of the ditopic complexes (2a and 3a) with Ni(CH3COO)2 · 6H2O. The UV-VIS spectra of 1 - 3, their sodium complexes 1a - 3a and sodium-nickel complexes 2b and 3b have been recorded in polar and non-polar solvents as well as in acidic and basic media. In polar solvents and basic solutions, tautomeric equilibria (phenol-imine and keto-amine forms, O-H···N⇌O···H-N ) are present, depending on the hydrogen bonding. The results indicate that the concentrations of the keto forms of the compounds generally increase as the polarity of the solvent increases
N -Methoxyalkyl-Funktionalisierte α-Diketodiimide/ N -Methoxyalkyl Functionalized α-Diketodiimides
Authors: Kuhn Norbert , Steimann Manfred , Walker Isabel
Published: February 2015

The α-diketodiimides C10H20N2O2 (2a) and C12H24N2O 2 (2b) are prepared by reacting butane- 2,3-dione with the corresponding α,ϖ-amino- (methoxy)alkanes (1); the X-ray structure of 2a is reported
Generation of Bis[2,6-di(4-methoxy-phenyl)phenyl]plumbylene and its Insertion into n-Butyliodide to Give a Tetrahedral Triorganolead(IV) Iodide
Authors: Wegner Gerald L. , Berger Raphael J. F. , Schier Annette , Schmidbaur Hubert
Published: February 2015

1 -Iodo-2,6-bis(4-methoxy-phenyl)benzene (BipapI) was prepared in a Grignard reaction from 4-bromo-anisol and 2,6-dibrom o-1 -iodo-benzene in tetrahydrofuran (61% yield). Treatment of BipapI with Az-butyllithium in hexane/diethylether gave the corresponding terphenyl-lithium compound BipapLi which crystallized as the dietherate in 83% yield. The structure of BipapLi • (OE2)2 has been determined by single crystal X-ray methods. The molecule is a monomer in the lattice, and the lithium atom is three-coordinate. Preparation of BipapLi in the presence of PbCl2 in diethylether gave a green solution, from which yellow crystalline (n -Bu)(Bipap)2Pbl was isolated in 73% yield. In the crystal this triorganolead(IV) iodide is monomeric and has tetrahedrally four-coordinate lead atoms.
Crystal and Molecular Structures of the Functional Lithium Cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph, Me
Authors: Bildmann Ulrich Jürgen , Winkler Martin , Müller Fachbereich Gerhard
Published: February 2015

The crystal and molecular structures of the phosphinomethyl-substituted lithium cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph (1), Me (2) (tmeda = N,N,N',N'-tetramethylethylenediamine) were determined as their tmeda adducts on the basis of low temperature single crystal X-ray diffraction. (Crystal data: 1: monoclinic, space group P21/n, a = 8.511(5), b = 11.936(2), c = 24.20(1) Å, β = 90.02(3)°, Z = 4.2: monoclinic, space group P21/n, a = 10.887(2), b = 13.326(2), c = 13.131(2) Å, β= 92.872(6)°, Z = 4). In both compounds lithium has a slightly distorted 17 coordination to the cyclopentadienide (Cp) ring. There are no interactions between lithium and the phosphine donors in the solid state as the phosphinomethyl substituents are oriented to the other side of the Cp ring for steric reasons. The isopropene-substituted lithium cyclopentadienide, which is formed as a by-product in the synthesis of phosphinomethyl cyclopentadienides containing a CMe2 bridge, was also structurally characterized as its tmeda adduct [Li(tmeda)][H2C=CMeC5H4] (3). (Crystal data: monoclinic, P21/c, a = 8.00(2), b = 16.701(2), c = 11.942(6) Å, β= 112.68(7)°, Z = 4). As in 1 and 2, lithium is η5 -coordinated to the Cp ring, and there is no interaction of the functional group (isopropene) with lithium.
Formation and Structure of Cinchona Alkaloid (Bis-2,3-naphthalenediyl)orthoborate Salts
Authors: Kubicki Maciej , Borowiak Teresa , Gawrońska Krystyna , Gawroński Jacek
Published: February 2015

A series of (bis-2,3-naphthalenediyl)orthoborate salts of Cinchona alkaloids has been synthesized and characterized. The interactions between ions in the salts have been studied by means of circular dichroism spectroscopy and X-ray crystal structure determination. The CD spectra of the dihydroquinidine salt show that in non-polar solvents it exists as a tightly held ion pair. The crystal structure of the cinchonidine salt proves the existence of ions in the solid state. The protonation takes place at the quinuclidine nitrogen atom. The hydrogen bonds connect cation and anion into one recognizable unit. Additional hydrogen bonds (with hydroxy group as a hydrogen donor and quinoline nitrogen atom as an acceptor) form infinite chains of cations along the [001] direction. There are cavities in the crystal structure that are partially filled by solvent molecules (acetone).
Synthesis and Structure of the Substituted Lithium Benzyl [Li(tmeda)2]+[C(PMe2)(SiMe3)C6H3-3,5-Me2]-. The First Metal Phosphinomethanide Consisting of Solvent-Separated Ion Pairs
Authors: Knapp Volker , Winkler Martin , Müller Gerhard
Published: February 2015

The lithium dimethylphosphinomethanide with trimethylsilyl and 3,5-dimethylphenyl substituents in a position [Li(tmeda)2]+[C(PMe2)(SiMe3)C6H3−3 ,5-Me2]− (2) was synthesized from Me2P-CH(SiMe3)C6H3−3 ,5-Me2 (1) and LinnBu/tmeda in hexane in 56% yield (tmeda = N, N, N′, N′-tetramethylethylenediamine). In the solid state it consists of solvent-separated ion pairs which probably is also the case in solution (crystal structure data: tetragonal, space group I41cd, a = b = 19.303(3), c = 34.905(7) Å, Z = 16, R(F) = 0.054 for 2309 unique data and 299 refined parameters). The a-substituted lithium benzyl 2 is the first metal phosphinomethanide containing “free”, uncoordinated anions in the solid state. The lack of metal coordination of the anion is reflected in the bonding parameters at the planar carbanionoid benzylic carbon atom C1 (C1-P 1.773(8), C1-Si 1.846(8), C1-C2(Ph) 1.442(9) Å; C2-C1-P 125.3(5), C2-C1-Si 127.1(5), P-C1-Si 107.5(3)°; sum of the angles at C1: 359.9°).
Formation of Methylchloroaluminium Alkanethiolates, MeAl(SR)Cl, and Dichloroaluminium Alkanethiolates, Cl2AlSR, from Methylaluminium Dichloride and Trimethylsilyl Alkanethiolates, Me3SiSR
Authors: Hoffmann Gerhard G.
Published: February 2015

Depending on the reaction conditions methylaluminium dichloride, MeAlCl2, and trimethylsilyl alkanethiolates, Me3SiSR, give dichloroaluminium alkanethiolates, Cl2AlSR with R = Me and Et or methylchloroaluminium alkanethiolates, MeAl(SR)Cl with R = Me, Et, and i-Pr. The reaction pathways are described and IR and 1H NMR spectroscopic data are presented.
Characterization of the Inorganic/Organometallic Osmium(IV) Compound [Cp2 OsIVCl]2 [OsIVCl6] as Formed by the Reaction of OSCI3 with Pentamethylcyclopentadiene in Air
Authors: Sixta Torsten , Kaim Wolfgang , Preetz Wilhelm
Published: February 2015

Reaction of OsCl3, with pentamethylcyclopentadiene in ethanol in air yields the ionic osmium( IV) compound [Cp*2OsCl]2[OsCl6] which has been identified structurally and by vibrational spectroscopy. Under comparable conditions the RuCl3 homologue yields the ruthenium( III) compound [Cp*RuCl2]2, illustrating the more facile oxidation of the 5d element to the tetravalent state
Coordination Compounds of Lanthanide Nitrates with Dimorpholido-N-trichloroacetylphosphorylamide. The Structure of Di(dimorpholido-N-trichloroacetylphosphorylamide)- diaqua Neodymium(III)trinitrate
Authors: Ovchynnikov Vladimir A. , Timoshenko Taras P. , Amirkhanov Vladimir M. , Sieler Joachim , Skopenko Viktor V.
Published: February 2015

Lanthanide, Carbacylamidophosphate The coordination compounds of the general formula Ln(NO3)3(HL)2(H2O)2 H2O , where Ln = La, Ce -Nd, Sm -Dy, HL = CCl3C(O)NHP(O)[N(CH2CH2)2O]2, dimorpholido-N-tri-chloroacetylphosphorylamide, have been synthesized. The complexes were studied by IR, 1H and 31P NMR and UV-VIS absorption spectroscopies. X-ray diffraction analyses indicate that all synthesized compounds are isostructural. The crystal structure of Nd(NO3)3(HL)2(H2O)2 H2O was solved (monoclinic, a = 11.0467(3), b = 15.9080(5), c = 24.1921(7) Å, β = 96.4080(10)°, space group P21/n, V = 4224.7(2) Å3, Z = 4, R = 0.049, wR = 0.0915). The complex has a molecular structure. The monodentate neutral phosphorictriamide ligands are coordinated to the metal atom via the phosphoryl oxygen atom. The coordination polyhedron of Nd is a sphenocorona; C.N. = 10(60[NO3
-], 20[HL], 20[H2O]).

It was shown that these compounds in methanol solution are 1:1 electrolytes, and in acetone solution weak electrolytes. According to NMR data in acetone solution the complexes of the lanthanides with the ligand {HL} have axial symmetry.
A Novel Convenient Synthesis of Mixed-Valence TiIII/TiIV Double Phosphates Starting with Titanium Nitride TiN
Authors: Zatovsky Igor V. , Slobodyanik Nikolay S. , Stratiychuk Denis A. , Domasevitch Konstantin V. , Sieler Joachim , Rusanov Eduard B.
Published: February 2015

A new synthetic approach for the low- and mixed-valence double titanium phosphates starting with titanium nitride, TiN, and based on the controlled oxidation of a low-valent metal in the phosphate melt is presented. The reaction of the system MI
2O - P2O5 - TiN (MI = Na, K) in air (800-1050 °C) leads to loss of nitrogen, N2, and results in the formation of a number of double phosphates: KTiP2O7, K2TiniTiIV(PO4)3, KTiOPO4, NaTiP2O7, NaTi2(PO4)3 and a new mixed-valent diphosphate, NaTiIIITiIV(P2O7)2. The mixed-valent species K2TiIIITiIV(PO4)3 and NaTiIIITiIV(P2O7)2 were characterized by single crystal X-ray diffraction. The described synthetic procedure is proposed as a simple and convenient method for the preparation of lowand mixed-valent phosphate materials
β-Enaminonitriles in Heterocyclic Synthesis: Synthesis of New 1,4-Dihydropyridine, PyrazoIo[1,5-a]pyrimidine, Aminothiophene and Pyridine Derivatives
Authors: Hafiz Ibrahim S. A.
Published: February 2015

Utility of 3-aminocinnamonitrile (1) in the synthesis of new 1,4-dihydropyridine, pyrazolo- [1,5-a]pyrimidine, aminothiophene and pyridine derivatives is reported
High-spin Cyclopentadienyl Complexes, Part 6. σ/π-Rearrangement of Aryl Ligands Connected to Cyclopentadienyliron Fragments
Authors: Wallasch Mark W. , Rudolphi Felix , Wolmershäuser Gotthelf , Sitzmann Helmut
Published: February 2015

Dimeric tri(tert-butyl)cyclopentadienyliron(II) bromide [CpmFe(μ-Br)]2 (1) reacts with phenylmagnesium bromide to give the dinuclear di(cyclohexadienylidene) complex [(CpmFe)2(μ,η5:η5-H5C6=C6H5)] (2), and with mesitylmagnesium bromide either to the dinuclear complex [CpmFe-(μ,η5:η1-C6H2Me3)Fe(Br)Cpm] (3) or to the mononuclear mesityl complex [CpmFeC6H2Me3] (4), depending on the reaction conditions. The mesityl complex 4 undergoes rearrangement and adds via the mesityl ipso carbon atom to bromide 1 with formation of 3. A similar reaction occurs with the nickel analog of bromide 1. In the latter case, however, mesityl is replaced by tolyl during reaction in toluene, with phenyl in benzene, and remains unchanged if the reaction is carried out in pentane solution. An electrophilic attack at the arene solvent used is discussed for the exchange reaction. For the crystallographically characterized complexes 3 and [CpFem(μ,η1:η5-C6H4Me)Ni(Br)Cpm] (5) with a meta-tolyl ligand a significant deviation of the CpmFe fragment from a symmetrical position above the six-membered ring ligand raises questions regarding a possible contribution of a cyclohexadienylylidene resonance structure.
Formation of Quaternary Stereogenic Centers by Wagner-Meerwein Rearrangement – Synthesis of Optically Active Cyclopentadienyl Complexes from Borneol and Fenchol
Authors: Färber Christian , Wolmershäuser Gotthelf , Sitzmann Helmut
Published: February 2015

The development of optically active cyclopentadienyl complexes as enantioselective catalysts calls for simple synthetic procedures for cyclopentadienes with optically active alkyl substituents. While exo-bornyl chloride and exo-fenchyl bromide do not react or exclusively eliminate hydrogen halide with cyclopentadienylmetal compounds in ether solvents or ammonia, they undergo Wagner- Meerwein rearrangement and substitution with cyclopentadienylmagnesium chloride in toluene. The bornyl cation yields racemic exo-bornylcyclopentadiene and partially racemized isocamphylcyclopentadiene, but for the fenchyl cation no racemization pathway is available, and the main diastereomer among the lithium salts of the ensuing substituted cyclopentadienes can be isolated in 95% diastereomeric purity by solvent extraction. This material with the IUPAC name lithium (2R)- 2,5,5-trimethylbicyclo[2.2.1]hept-2-ylcyclopentadienide carries an alkyl substituent having no trivial name so far. Exo-norbornylcyclopentadiene could be synthesized in high yield with a similar procedure. The same protocol works with 1-bromoadamantane. The novel alkylcyclopentadienes have been converted to ferrocenes and molybdenum complexes of the type [CpRMo(CO)3CH3]. (2R)- 2,5,5-Trimethylbicyclo[2.2.1]hept-2-ylcyclopentadiene with an optical purity of 78% ee (the optical purity of the starting material fenchol) was converted into an optically active titanocene dichloride and tested in the catalytic hydrogenation of 2-phenyl-1-butene. The hydrogenation product was obtained with 31% ee, which compares favorably with results obtained with other group 4 metallocene dichlorides with one optically active alkyl substituent on each ring ligand. Facile procedures for the synthesis of the starting compounds exo-bornyl chloride and exo-fenchyl bromide based on the tosylate method have been developed with a tosylate melt or with toluene serving as solvents.
Adduct Compounds (MCl5)2(β-P4Ch4) with M = Nb, Ta and Ch = S, Se
Authors: Hoppe Diana , Pfitzner Arno
Published: February 2015

Adduct compounds of the general composition (MCl5)2(β -P4Ch4), M = Nb, Ta and Ch = S, Se, were obtained from solutions of M2Cl10 and P4Ch3 in CS2 / n-hexane. The compounds are isotypic with (NbCl5)2(β -P4S4), crystallizing in the monoclinic space group P 21/n (no. 14) with Z = 4. The lattice constants are a = 6.304(2), b = 13.071(3), c = 26.552(6) Å , β = 93.74(3)◦, V = 2183(1) Å3 for (TaCl5)2(β -P4S4), a = 6.360(2), b = 13.322(3), c = 26.710(6) Å , β = 93.81(3)0, V = 2258(1) Å3 for (TaCl5)2(β -P4Se4), and a = 6.334(2), b = 13.267(6), c = 26.583(7) Å , β = 93.71(3)0, V = 2229(2) Å3 for (NbCl5)2(β -P4Se4). The adduct molecules consist of two MCl5 units which are linked with two of the basal phosphorus atoms of the central β -P4Ch4 cage.
Activation of Polarized Phosphorus–Phosphorus Bonds by Alkynes: Rational Synthesis of Unsymmetrical 1,2-Bisphosphine Ligands and Their Complexes
Authors: Burck Sebastian , Hajdók Imre , Nieger Martin , Bubrin Denis , Schulze Simon , Gudat Dietrich , Gudat Dietrich
Published: February 2015

The reactions of 1,1-diamino-2,2-diphenyl-substituted diphosphines featuring various degrees of P-P bond polarization with different alkynes were investigated. All diphosphines reacted with alkynes carrying one or two electron withdrawing carboxylic ester moieties under cleavage of the P-P bond and stereospecific phosphinyl-phosphination at the triple bond to give unsymmetrical ethane-1,2- bisphosphines. Several of the products were further converted into chelate complexes upon reaction with group-10 metal dihalides. All isolated compounds were characterized by analytical and spectroscopic data, and several of the new ligands and complexes by single-crystal X-ray diffraction studies.
Simple Prediction of Some Physical Properties of Ionic Liquids: The Residual Volume Approach
Authors: Bogdanov Milen G. , Kantlehner Willi
Published: February 2015

A new method for prediction of fundamental physical properties of ionic liquids (ILs) is proposed. The Residual Volume Approach (RVA) allows the estimation of density and viscosity of unknown ILs, using a simple linear correlation between a given property and a newly defined substituent parameter βX. The proposed method has been developed for the density estimation of 50 n-alkyl-substituted imidazolium and tetraalkylammonium salts in a homologous series of ILs and has been extended for the estimation of viscosity, which also correlates linearly with the corresponding βX. In addition, the parameters βX are temperature and pressure independent, which allows the prediction of these values at any temperature and pressure
Synthetic and Cytotoxic and Antimicrobial Activity Studies on Annomuricatin B
Authors: Dahiya Rajiv , Maheshwari Monika , Yadav Rakesh
Published: February 2015

Graphical Abstract

Synthetic and Cytotoxic and Antimicrobial Activity Studies on Annomuricatin B
Flavonoid, Phenylethanoid and Iridoid Glycosides from Globularia aphyllanthes
Authors: Kırmızıbekmez Hasan , Bassarello Carla , Piacente Sonia , Akaydın Galip , Çalış İhsan
Published: February 2015

A new flavone glycoside, 6-hydroxyluteolin 7-O-[6m-benzoyl-β -D-glucopyranosyl-(1 → 2)]-β - D-glucopyranoside (aphyllanthoside, 1) was isolated from the MeOH extract of the aerial parts of Globularia aphyllanthes. Besides this new compound, two flavonoid glycosides (6-hydroxyluteolin 7-O-[6m-(E)-caffeoyl-β -D-glucopyranosyl-(1 → 2)]-β -D-glucopyranoside and isoquercitrin), three phenylethanoid glycosides (verbascoside, rossicaside A, and trichosanthoside A), and 11 iridoid glycosides (aucubin, catalpol, 10-O-benzoylcatalpol, globularin, asperuloside, besperuloside, asperulosidic acid, daphylloside, scandoside, alpinoside and baldaccioside) were also obtained and characterized. Identification of the isolated compounds was carried out by spectroscopic analysis including 1D and 2D NMR experiments as well as HRMS
Synthesis and Structural Characterisation of a Hexanuclear GdIII Compound Gd6(μ3-OH)6(acac)12·1.25 CHCl3 as a Potential Precursor for Gd2O3 Nanomaterials
Authors: Pandey Ashutosh , Pandey Anjana , Mayer Peter , Parak Wolfgang J.
Published: February 2015

While aging the reaction mixture of gadolinium tri-isopropoxide with acetylacetone (pentane-2,4- dione, acacH) in a 1 : 2 molar ratio in toluene for crystalisation, crystals of Gd6(μ3-OH)6(acac)12・1.25 CHCl3 (1) were obtained in high yield. The crystal structure analysis reveals that 1 has a M6O12 core which is constituted of two distorted, tricapped, face-sharing cubane units (each with one missing edge) wherein the metal atoms are octacoordinated with a distorted square-antiprismatic geometry. In a sol-gel treatment the amorphous xerogel obtained from 1 was transformed into a nano-crystalline product at 600 °C while the xerogel of Gd(OPri)3 under similar conditions required a heat treatment up to 900 °C for the same development.
Synthesis and Crystal Structure of a New 3D Copper B-Paradodecatungstate Compound: [Na2(H2O)8][Na8(H2O)20][Cu(en)2][W12O42] · 3H2O
Authors: Xu Xiuhong , Luo Fang , Luo Weihong , Chen Ji
Published: February 2015

A new polyoxotungstate complex [Na2(H2O)8][Na8(H2O)20][Cu(en)2][W12O42] ・3H2O (1) (en = ethylenediamine) has been synthesized in aqueous solution and characterized by elemental analysis, IR spectroscopy and TG analysis, together with a single crystal X-ray diffraction study. In compound 1, the Cu(en)2
2+ complex cation links the [W12O42]12− anions to form a 1D chain, and the 1D chains are further interconnected with Na8(H2O)20
8+ and Na2(H2O)8
2+ cations to construct a new 3D framework.
Synthesis, Crystal Structure and Magnetic Properties of Bixbyite-type Vanadium Oxide Nitrides
Authors: Nakhal Suliman , Hermes Wilfried , Ressler Thorsten , Pöttgen Rainer , Lerch Martin
Published: February 2015

Ammonolysis of vanadium sulfide leads to the formation of bixbyite-type vanadium oxide nitrides. Small amounts of nitrogen incorporated in the structure result in the stabilization of the bixbyite type not known for vanadium oxides. The crystal structure was investigated using X-ray diffraction and X-ray absorption spectroscopy. At temperatures above 550 °C the powders decompose to corundumtype V2O3 containing no detectable amount of nitrogen. Below 39 K magnetic ordering is observed.
3-O-Sulfo-triterpenoid Saponins from Gypsophila trichotoma Wend
Authors: Krasteva Ilina , Jenett-Siems Kristina , Kaloga Maki , Nikolov Stefan
Published: February 2015

Three new sulfated oleanane-type saponins were isolated from the roots of Gypsophila trichotoma Wend. (Caryophyllaceae). Their structures were established as 3-O-sulfoechinocystic acid 28-β -glucopyranosyl ester (1), 3-O-sulfooleanolic acid 28-β -glucopyranosyl ester (2) and 3-Osulfoquillaic acid 28-β -glucopyranosyl ester (3) on the basis of chemical and spectral evidences.
Detection of Adducts with Matrix Clusters in the Positive and Negative Ion Mode MALDI-TOF Mass Spectra of Phospholipids
Authors: Petković Marijana , Schiller Jürgen , Müller Matthias , Süß Rosmarie , Arnold Klaus , Arnhold Jürgen
Published: February 2015

It is usually accepted that neutral phospholipids (PLs) generate singly positively charged ions, whereas negative PLs are easily detectable in the negative ion mode when analysed by matrix-assisted laser desorption and ionisation time-offlight mass spectrometry (MALDI-TOF MS). In this study, we demonstrate that some caution is required in the interpretation of MALDI-TOF mass spectra of PLs, since also neutral PLs have appeared to be detectable in the negative ion mode as well. Neutral and negatively charged phospholipids can generate adducts with the most commonly used matrix - 2,5-dihydroxybenzoic acid - yielding singly negatively charged ions that are detectable in the spectra. This further contributes to the complexity of the spectra and potentially leads to severe misinterpretation, particularly when unknown mixtures of PLs are analysed by MALDI-TOF MS.
An Organozinc Hydrazide-Thiolate Aggregate with a Zn3N4S2 Core
Authors: Jana Surajit , Mitzel Norbert W.
Published: February 2015

The first organometallic zinc hydrazide-thiolate cluster, [(MeZn)2(PhSZn)(HNNMe2)(H2N-NMe2)(SPh)2]2 (1) has been prepared by alkane elimination from dimethylzinc solutions upon treatment with N,N-dimethylhydrazine and thiophenol and characterised by NMR spectroscopy, elemental analysis and single crystal X-ray diffraction. Compound 1 forms asymmetric aggregates containing a Zn3N4S2 core. The core features rings with different connectivities. A seven-membered ZnSZnNNZnS ring comprises three fivemembered rings, two of a ZnSZnNN and one of a ZnNZnNN atom sequence. Intermolecular S···H bonding is observed in the crystal.
Pr2CBr: Ein Ferromagnet mit Pr2C-Schichten/ Pr2CBr: A Ferromagnet with Pr2C Layers
Authors: Mattausch Hansjürgen , Kremer Reinhard K. , Simon Arndt
Published: February 2015

Single-phase Pr2CBr was prepared by heating a mixture of PrBr3, Pr and C (1 : 5:3) to 1140 °C for 18 d. The crystal structure was investigated by X-ray single crystal diffraction (space group P63/mmc, a = 3.8071(3), c = 14.7787(12) Å). In the structure the Pr atoms form C-centered octahedra condensed into Pr2C sheets via common edges; these sheets are separated by the Br atoms which are in a trigonal prismatic environment of Pr atoms. Pr2CBr is a black shiny compound with metallic conductivity. It is a ferromagnet with Tc = 13.8(5) K.
Non-hydrothermal Synthesis of a Complex {[Zn(phen)2]2(γ-Mo8O26)} Constructed from [γ-Mo8O26]4– Anions
Authors: Hao Zhaomin , Luo Weihong , Xu Xiuhong , Luo Fang
Published: February 2015

An octamolybdate-supported complex, {[Zn(phen)2]2(γ-Mo8O26)} (phen = 1,10-phenanthroline) (1), has been obtained and characterized by IR spectroscopy, TGA analysis and single crystal X-ray diffraction. Crystal data: C48H40O26N8Mo8Zn2, monoclinic, P21/n, a = 12.986(5), b = 16.704(5), c = 13.996(5) Å , β = 106.551(5)°, V = 2910.2(18) Å3, Z = 2. The structure of compound 1 consists of a γ -octamolybdate cluster covalently attached to two [Zn(phen)2]2+ complexes. The complexes are tightly packed via C-H・ ・ ・O contacts between phen and [γ-Mo8O26]4− anions
Reaction of 9-Borabicyclo[3.3.1]nonane with Alkyn-1-yltin Compounds. Molecular Structure of the 9-Propyn-1-yl-9-borabicyclo[3.3.1]nonane Pyridine Adduct
Authors: Wrackmeyer Bernd , Bihlmayer Christoph , Shahid Khadija , Milius Wolfgang
Published: February 2015

Trimethyl- and triethyl(propyn-1-yl)tin react with 9-borabicyclo[3.3.1.]nonane (9-BBN) mainly by exchange of the propynyl group against hydrogen, accompanied by numerous side reaction. This is in contrast to the findings for other alkynyltin compounds bearing a second bulky substituent at the C≡C bond. The exchange product, 9-propyn-1-yl-9-borabicyclo[3.3.1]nonane, was isolated as its crystalline pyridine adduct and fully characterised by NMR spectroscopy in solution and X-ray structural analysis in the solid state.
Synthesis, Structure and Fluorescence Properties of a Trinuclear Zn(II) Complex with N,N,O-donor Schiff Base Ligands and Bridging Acetates
Authors: Shit Shyamapada , Chakraborty Joy , Samanta Brajagopal , Rosair Georgina M. , Mitra Samiran
Published: February 2015

A new centrosymmetric trinuclear Zn(II) complex [Zn3L2(CH3COO)4] (1) has been synthesized by the reaction of Zn(CH3COO)2 · 2H2O with a tridentate N,N,O-donor Schiff base ligand HL [C5H4NC(CH3)=NC6H4(OH)] and systematically characterized by elemental analysis, FT-IR, UV/Vis and thermal methods. Single crystal X-ray structure analysis reveals that three Zn(II) centers are in two different coordination environments. Two terminal Zn(II) centers adopt a distorted squarepyramidal geometry leaving the central Zn(II) in a distorted octahedral environment. Two adjacent metal centers are connected through single μ2-phenolato as well as double μ-acetato-O,O´ syn-syn bridges. Fluorescence properties of the complex as compared to the ligand indicate that the former can serve as a potential photoactive material.
A New Lanostane Triterpene from Skimmia laureola
Authors: Sultana Nighat , Sultana Razia
Published: February 2015

Aerial parts of Skimmia laureola yielded a new (+)-lanostane-3β ,24-dihydroxy-25-ene triterpene (1) along with fourteen known compounds. The structures were identified by spectroscopic studies
Preparation and Characterization of the First Organosulfonium Azides
Authors: Klapötke Thomas M. , Scherr Matthias , Krumm Burkhard
Published: February 2015

The first triorganosulfonium azides [Me3S]N3 and [Ph3S]N3 were prepared by reaction of the corresponding sulfonium bromides/iodides with silver azide and characterized by spectroscopic methods. The molecular structure of [Ph3S]N3 as well as that of the precursor, [Ph3S]Br, have been determined by X-ray diffraction.
Controllable Formation of MgCl2-based Spherical Catalyst Support Precursors via Composites of Liquid Inorganics and Polymers
Authors: Chen Liyi , Hanisch Christian , Rieger Bernhard
Published: February 2015

Anhydrous MgCl2 was reacted with 2 equiv. of ethanol to generate the MgCl2(EtOH)2 adduct 1. An appropriate amount of higher alcohol having a long carbon chain, such as 1-decanol, was anchored on the surface of a part of adduct 1 to give a mixture of MgCl2 adducts having an internal surfactant. A multifunctional polymer/oligomer, e. g. poly(ethylene glycol)-200 (PEG-200), was introduced into this system yielding a composite of liquid inorganics and polymers (CLIP). Under the regulation of the internal surfactant and the multifunctional polymer, this composite was melted and dispersed in an inert hydrocarbon solvent under vigorous agitation at elevated temperatures followed by fast cooling to generate a MgCl2-based spherical catalyst support precursor. SEM pictures show that this support precursor has a narrow particle size distribution, and its surface structure is an intricate combination of smaller MgCl2-based crystallites.
Metal and Boron Derivatives of Fluorinated Cyclic 1,3-Dicarbonyl Compounds
Authors: Sevenard Dmitri V. , Khomutov Oleg G. , Boltachova Nadezhda S. , Filyakova Vera I. , Vogel Vera , Lork Enno , Sosnovskikh Vyacheslav Ya. , Iaroshenko Viktor O. , Röschenthaler Gerd-Volker
Published: February 2015

Starting from the corresponding cyclic 1,3-diketones or other precursors (cyclic ketones as well as lactones), several new salts and chelate complexes of fluorinated 1,3-dicarbonyls were obtained. Their preparative significance was demonstrated by straightforward syntheses of fluorinated pyrazoles, benzimidazoles and 1,7-ketoesters. The structure of a boron chelate of 2-(trifluoroacetyl)- cyclohexanone was investigated by X-ray diffraction.
Determination of the Lipophilicity of Some New Derivatives of Semicarbazide and 1,2,4-Triazol-5-one with Potential Antibacterial Activity
Authors: Pitucha Monika , Polak Beata , Świebodac Ryszard , Kosikowska Urszula , Malm Anna
Published: February 2015

The chromatographic behavior of new derivatives of 1,2,4-triazol-5-one and semicarbazide was determined. The lipophilicity was confirmed by the use of a RP-TLC method. The partition coefficients were calculated by use of theoretical procedures. The correlation between theoretical and experimental lipophilicity was determined. All obtained compounds were tested for their antimicrobial activity.
Quaternary 4-Amino-1,2,4-triazolium Salts: Crystal Structures of Ionic Liquids and N-Heterocyclic Carbene (NHC) Complexes
Authors: Schwärzler Alexander , Laus Gerhard , Kahlenberg Volker , Wurst Klaus , Gelbrich Thomas , Kreutz Christoph , Kopacka Holger , Bonn Günther , Schottenberger Herwig
Published: February 2015

Quaternary salts were prepared by reaction of 4-amino-1,2,4-triazole and 4-amino-3,5-dialkyl- 1,2,4-triazoles (alkyl = Me, Et) with dimethyl and diethyl sulfate at ambient temperature. Subsequent ion metathesis gave hexafluorophosphates and bis(trifluoromethylsulfonyl)imides as crystalline derivatives or ionic liquids.Methylation at 100 ◦C gave the 4-(dimethylamino)-1-methyl-1,2,4- triazolium salt, a precursor for a new carbene ligand which was incorporated into Ag and Rh complexes. The synthesis of 5-bromo-4-(dimethylamino)-1-methyl-1,2,4-triazolium hexafluorophosphate is also reported. Crystal structures of fourteen compounds have been determined by X-ray diffraction
Hydroxy-1H-imidazole-3-oxides – Synthesis, Kinetic Acidity, and Application in Catalysis and Supramolecular Anion Recognition
Authors: Bartz Susan , Blumenröder Bettina , Kern Anika , Fleckenstein Julia , Frohnapfel Sabine , Schatz Jürgen , Wagner Alexander
Published: February 2015

Using ab initio calculations (B3LYP 6-31G*) the geometries of diethyl, dimethoxy and dimethylamino imidazolium salts were studied as representative models of imidazolium salts bearing heteroatoms directly attached to the ring nitrogen atoms of the imidazolium core units. In all cases the syn and anti arrangement of the substituents could be identified. In addition to the theoretical studies, eleven dialkoxy imidazolium salts were prepared by alkylation of six 1-hydroxy-imidazole-3-oxides using dimethyl or diethyl sulfate as strong alkylating reagents. The kinetic acidities of these compounds were studied by measuring the pseudo-first order reaction rates of the H/D exchange process of the C2-H proton of compounds 3 - 9. The observed kinetic acidities are much higher than reaction rates observed for simple imidazolium salts; half-lifes of the H/D exchange are usually in the range of minutes. Similar to dialkyl/aryl imidazolium salts, all prepared dialkoxy imidazolium salts could be used as precatalysts in standard aqueous Suzuki coupling reactions. In addition, two representative dialkoxy imidazolium salts could be used in supramolecular anion recognition, as demonstrated by binding studies towards iodide as guest.
Synthesis of a Regular 24-membered Cyclodepsipeptide by Direct Amide Cyclization
Authors: Kottgen Peter , Linden Anthony , Heimgartner Heinz
Published: February 2015

The synthesis of a 24-membered cyclic depsipeptide with an alternating sequence of phenyllactic acid and α-aminoisobutyric acid (Aib) is described. The linear precursor was prepared via the ‘azirine/oxazolone method’ using 2,2-dimethyl-3-amino-2H-azirines as building blocks for the α,α-disubstituted α-amino acid Aib. The macrolactonization leading to the cyclodepsipeptide was achieved by the ‘direct amide cyclization’, i. e., by treatment of a solution of the linear precursor in toluene with HCl gas.
Synthesis and Structures of LiBH4 Complexes with N-Heterocycles [1]
Authors: Leiner Stefanie , Mayer Peter , Nöth Heinrich
Published: February 2015

LiBH4 solutions in diethyl ether or tetrahydrofuran react with N-methylmorpholine, Nmethylimidazole or piperidine not only with the formation of adducts LiBH4(L)n (n = 1 or 3) but also with formation of amine boranes BH3(L). While LiBH4 and N-methylimidazole form the 1 : 3 adduct 1, N-methylmorpholine produces the 1 : 1 adduct 2. In both cases the adducts contain hexacoordinated Li atoms. In 1 the Li atom is coordinated to three N atoms and three H atoms. However, in compound 2 the molecules are connected in the solid state with one another to form a two-dimensional polymer built from dimeric units (LiBH4)2 that are connected to adjacent dimeric units via the O and N atoms of the N-methylmorpholine ligand. Each of the Li atoms in 2 is connected to four H atoms via Li-H-B hydrogen bridges and an O and an N atom. The reaction of LiBH4 with piperidine leads to the compound (LiBH4)6(HNC5H10)16, 3, which consists of two independent LiBH4(HNC5H10)3 molecules and two others of composition (LiBH4)2(HNC5H10)5 containing penta- and hexacoordinated Li atoms.
Low-temperature Crystal Structure and 57Fe Mössbauer Spectroscopy of Sr3Sc2O5Fe2As2
Authors: Tegela Marcus , Schellenberg Inga , Hummel Franziska , Pöttgen Rainer , Jorendt Dirk
Published: February 2015

The crystal structure of the layered iron arsenide Sr3Sc2O5Fe2As2 was determined between 300 and 10 K. The lattice parameters of the tetragonal cell decrease anisotropically according to Δc/c : Δa/a ≈ 4.2, which results in a slight flattening of the As-Fe-As bond angle within the FeAs layers. No indication of a structural instability could be detected. 57Fe Mössbauer spectroscopic data show only a single signal at 4.2, 77, and 298 K, subjected to quadrupole splitting. The isomer shift increases from 0.36(1) mms−1 at 298 K to 0.49(1) mms−1 at 4.2 K. No indication for magnetic ordering was found.
Structural Characterization of 2,2-Di-n-butyl-4-methyl-1,3,2- dioxastannolane Isolated from Supercritical CO2 Conditions
Authors: Plasseraud Laurent , Cattey Hélène , Richard Philippe
Published: February 2015

The title compound has been isolated as single crystals from the synthesis of propylene carbonate from racemic 1,2-propanediol and carbon dioxide using n-Bu2SnO as a catalyst precursor. The X-ray crystallographic structure analysis revealed the self-assembly of di-n-butyltin(IV) 1,2-propanediolate units, linked together through long-distance Sn-O interactions leading to a one-dimensional polymeric architecture organized in a syndiotactic arrangement. The coordination geometry around the tin atoms can be described as an unusual faced-capped trigonal bipyramidal environment.
Three Crystal Structures of Terephthalic Acid Salts of Simple Amines
Authors: Jones Peter G. , Ossowski Jerzy , Kus Piotr , Dix Ina
Published: February 2015

Diphenethylamine forms two adducts (1 : 1, 1a and 2 : 1, 1b) with terephthalic acid (H2TPA). The former is bis(diphenethylammonium)H2TPA・TPA2− and the latter is bis(diphenethylammonium) ・TPA2−. The amine cis-2,6-dimethylpiperidine forms a hydrated 2 : 1 adduct, bis(2,6-dimethylpiperidinium) ・TPA2−・H2O (2). The crystal structures of all three compounds were determined. All H2TPA and TPA2− residues display inversion symmetry, while the water oxygen atom of 2 lies on a twofold axis. Packing analyses have identified some supramolecular synthons known from related structures.
Synthesis of Phenylsubstituted 2H,5H-Pyrano[ 4,3-b] pyran-5-ones and Related Heterocycles via a Domino Knoevenagel Condensation/ 6π-Electron Electrocyclization of 4-Hydroxy-6-phenyl-2H-pyran-2-one with Cyclic and Acyclic α, β-Unsaturated Aldehydes under Different Conditions Synthesis and Crystal Structure of the High-pressure Iron Borate β-FeB2O4 Synthesis and Crystal Structure of the High-pressure Iron Borate β-FeB2O4 Synthesis and Crystal Structure of the High-pressure Iron Borate β-FeB2O4 Synthesis and Crystal Structure of the High-pressure Iron Borate β-FeB2O4 Synthesis and Crystal Structure of the High-pressure Iron Borate β-FeB2O4
Authors: Leutbecher Heiko , Rieg Sylvia , Conrad Jürgen , Mika Sabine , Klaiber Iris , Beifuss Uwe
Published: February 2015

A range of new 7-phenyl-2H,5H-pyrano[4,3-b]pyran-5-ones and related tricyclic heterocycles was prepared in a single step by means of a domino Knoevenagel condensation/6π-electron electrocyclization under different reaction conditions, including thermal and microwave conditions. The influence of several ionic liquids as solvents was also studied
Diastereoselective Formation of Cyclopropanols by a Chromium(II)-mediated Cross-coupling Reaction
Authors: Lang Steffen , Groth Ulrich
Published: February 2015

Various 2-(α-hydroxyalkyl)cyclopropanols were generated by chromium(II)-mediated crosscoupling of acroleins and aldehydes with high diastereoselectivities up to 95%. The unstable diols were converted selectively to the stable monosilyl ethers by treatment with TBDMS-Cl in the presence of the second secondary alcohol
The Anion [Co(C8H12)2]–. A Comparative Study of the Crystal Structures of [{K(18-crown-6)}2(C5H5)][Co(C8H12)2] and Co(C8H12)(C8H13)
Authors: Wang Jian-Qiang , Fässler Thomas F.
Published: February 2015

The cobalt complex [{K(18-crown-6)}2(C5H5)]- [Co(C8H12)2]・(THF)2 (3) has been synthesized and characterized by X-ray single-crystal structure determination. The crystal structure of Co(C8H12)(C8H13) (2) has been reinvestigated and compared with the structure of 3. The 1,5-cyclooctadiene (C8H12) and C8H13 ligands are coordinated in an η4 and η3 fashion, respectively. The cyclopentadienyl anion in [{K(18-crown-6)}2(C5H5)]+ in 3 is η5-coordinated to the two crown ether-encapsulated potassium cations
Syntheses of 1,1-Organo-substituted Silole Derivatives. 1,1-Ethylboration, 1,1-Vinylboration and Protodeborylation
Authors: Khan Ezzat , Bayer Stefan , Wrackmeyer Bernd
Published: February 2015

1,1-Organoboration of dialkyn-1-ylsilanes using triethylborane, BEt3, and 9-ethyl-9-borabicyclo [3.3.1]nonane, Et-9-BBN, was carried out at elevated temperatures, 100 - 120 °C. These reactions afforded selectively silole derivatives bearing the dialkylboryl group in 3-position. The siloles are formed via intermolecular 1,1-alkylboration, followed by intramolecular 1,1-vinylboration. Two examples of boryl-substituted siloles were treated with an excess of acetic acid at ambient temperature to afford the respective protodeborylated compounds. All new compounds were characterized in solution by multinuclear magnetic resonance spectroscopy (1H, 13C, 11B and 29Si NMR).
Ag(I)-, Hg(II)- und Pt(II)-Komplexe von Maleonitril-thiakronenethern/ Ag(I), Hg(II) and Pt(II) Complexes with Maleonitrile-thiacrown Ethers
Authors: Müller Holger , Kelling Alexandra , Schilde Uwe , Holdt Hans-Jürgen
Published: February 2015

The synthesis and single crystal X-ray structures of eight AgI, HgII, and PtII complexes with the thiacrown ethers maleonitrile-tetrathia-12-crown-4 (mn12S4), maleonitrile-tetrathia-13-crown-4 (mn13S4), and maleonitrile-pentathia-15-crown-5 (mn15S5) (1) are reported. The ligand mn15S5 was synthesized for the first time and characterized by X-ray diffraction. With silver(I) perchlorate and silver(I) tetrafluoroborate it forms the chiral complexes [Ag(mn15S5)]ClO4・CH3NO2 (2) and [Ag(mn15S5)]BF4・CH3NO2・0.25H2O (3) with half-sandwich moieties. AgI is located in a distorted tetrahedral coordination environment, involving three sulfur atoms of the crown cycle and a fourth one of the adjacent half-sandwich moiety, forming a helical structure. The reaction of Hg(ClO4)2 with mn13S4 yielded the dinuclear complex [Hg2(mn13S4)3](ClO4)4 (4) containing two half-sandwich moieties with a third ligand molecule as a bridging unit. Mercury(II) chloride and mercury(II) iodide react with mn12S4 and mn13S4 to form complexes of the general composition [HgX2(L)] (X = Cl, I; L = mn12S4, mn13S4): [HgCl2(mn12S4)] (5), [HgI2(mn12S4)] (6), [HgCl2(mn13S4)] (7) or [HgX2(L)2] (X = I; L = mn13S4): [HgI2(mn13S4)2] (8). Only one or two sulfur atoms of the ligand are involved in the complexation, and chain or ribbon structures are formed. In these compounds the HgX2 units (X = Cl, I) are preserved, coordinated by sulfur atoms of bridging mn12S4 or mn13S4 ligands. In all complexes of this type, the metal atoms are not coordinated inside the cavity, but in an exocyclic mode, because the diameter of the macrocycle is too small. Additionally, the PtCl2 complex of mn12S4 was investigated, where PtII is coordinated in an exocyclic mode forming the complex [PtCl2(mn12S4)] (9). Two of the four sulfur atoms of the macrocycle are bonded to the metal giving together with both chlorine atoms a square-planar coordination geometry. Together with a long-range interaction with a further sulfur atom of the macrocycle a square-pyramidal coordination environment is formed.
Synthesis of Antimicrobial N-Phthaloyl-alanyl-derived Amidophosphates and Triazoles
Authors: Abdou Wafaa M. , Ganoub Neven A. , Sabry Eman
Published: February 2015

N-Phthaloyl-alanylazide reacts smoothly with trialkyl phosphites producing the corresponding α- aminophosphates. With dialkyl hydrogenphosphonates in the presence of benzoyl peroxide, amidophosphates were the isolated products whereas the oxoaziridin-1-yl-phosphonic diamide was preferentially provided from the reaction of the azide with tris(dimethylamino)phosphine. The azide was also allowed to react with α-keto-, α-ethoxycarbonyl- and α-cyanomethylenetriphenylphosphorane to give the corresponding linear disubstituted 1,2,3-triazoles. Screening results of antibiotic potency for the products were discussed in terms of structure-activity relationship (SAR), and an attempt was made to define the structural features for lead compounds.
Antibacterial Ellagic Acid Derivatives and Other Constituents from Pancovia pedicellaris
Authors: Soh René F. , Bankeu Jean K. , Lenta Bruno N. , Mbáning Brice M. , Ngouela Silvère , Tsamo Etienne , Sewald Norbert
Published: February 2015

Two new ellagic acid derivatives, named panconosides A (1) andB(2) were isolated from Pancovia pedicellaris together with eleven known compounds (3 - 13). The structures of 1 and 2, as well as those of the known compounds were established by spectroscopic methods and by comparison with previously reported data. Compounds 1 and 2 were tested in vitro for their antibacterial potential against six strains of microorganisms: Micrococcus luteus, Streptococcus ferus, Streptococcus minor, Escherichia coli, Bacillus subtilis, and Pseudomonas agarici. They were found to exhibit moderate antibacterial activity against all the tested strains compared to standard drugs.
A Major Saponin from Leaves Extract of Acer velutinum
Authors: Glénsk Michał , Włodarczyk Maciej , Bassarello Carla , Pizza Cosimo , Stefanowicz Piotr , Świtalska Marta
Published: February 2015

A major triterpenoid saponin was isolated from the leaves extract of Acer velutinum. This compound was characterized as 21β ,22α-O-diangeloylprotoaescigenin 3-O-[β -D-glucopyranosyl- (1→2)][β -D-glucopyranosyl-(1→4)]-β -D-glucuronopyranosyl acid.

Its structure was elucidated by 1H, gCOSY, ROESY, gHSQC, gHMBC NMR as well as ESI-MS experiments. Isolated saponin exhibited in vitro cytotoxicity against HL-60, B16-F0 and BALB/3T3 cell lines.
Neue Koordinationspolymere mit Acetylendicarboxylat als verbrückenden und Pyridin als terminierenden Liganden / New Coordination Polymers with Acetylenedicarboxylate as Bridging and Pyridine as Terminating Ligands
Authors: Stein Irena , Ruschewitz Uwe
Published: February 2015

By slow diffusion of pyridine (py) into an aqueous solution containing the respective metal salt and acetylenedicarboxylic acid (H2ADC), single crystals of coordination polymers of composition 1
∞[MII(H2O)2(py)2ADC] with MII = Zn (1) and Cd (2) were obtained. The crystal structures consist of octahedral MIIN2O4 units, which are connected to chains via acetylenedicarboxylate dianions. Hydrogen bonds between O atoms of the dianions and of the water molecules lead to the formation of layers perpendicular to [010]. The structure is further held together by weak aromatic stacking interactions between the pyridine ligands.