bluuebunny/crossref_metadata_2025 huggingface dataset:
Synthese neuer Pyridin-C-nukleoside der 2 ,3 -Didesoxyribose durch „inverse“ [4+2]-Cycloaddition Synthesis of Novel Pyridine-C-nucleosides of 2,3-Dideoxyribose by „Inverse“ [4+2]-Cycloaddition
Authors: Seitz Gunther , Siegl Johanna
Published: August 2018

The anomeric imido esters 5 and 6, appropriate precursors for C-nucleoside synthesis, were prepared and utilized as heterodienophiles in a Diels-Alder reaction with inverse electron demand to yield the novel, protected 1.2.4-triazine C-nucleosides 8 and 9. They could be deprotected by treatment with 70% trifluoroacetic acid to furnish the free C-nucleosides 10 and 11. The triazine „aglycon“ of 8 contains an electron deficient diazadiene system, highly activated to react with various electron rich dienophiles such as enamines, enol ethers and several cyclic ketene acetals in an „inverse“ [4+2]-cycloaddition reaction. The Diels-Alder adducts spontaneously eliminate N2 and after follow-up reactions the O-TBDPS protected pyridine-C-nucleosides 13, 15, 17,19, 21 and 23 are formed. Removal of the protecting group by treatment with CF3CO2H /H2O leads to the corresponding 2’,3’-dideoxy-β-D-ribofuranosyl- pyridines.
Darstellung, 11B-, 1H-NMR und Schwingungsspektren von 4-Aminopyridylundecahydro-closo-dodecaborat(1-) sowie Kristallstruktur von (Ph4As)[(4-(NH)-C5H4N)B12H11]·2CH3CN / Synthesis, 11B , 1H NMR and Vibrational Spectra of 4-Aminopyridylundecahydro-closo- dodecaborate(1-) and Crystal Structure of (Ph4As)[(4-(NH)-C5H4N)B12H11]·2CH3CN
Authors: Koch T , Preetz W
Published: August 2018

By reaction of (n-Bu4N)2[B12H12] with 4-aminopyridine at 190°C the 4-aminopyridylundecahydro- closo-dodecaborate anion [(4-(NH)-C5H4N)B12H11]- is obtained which can be separated from excess [B12H12]2- by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose. The X-ray structure determination of (Ph4As)[(4-(NH)-C5H4N)B12H11]-2CH3CN (orthorhombic, space group Pbca, a = 14.294(2), b = 19.587(2), c = 27.279(5)Å, Z = 8) reveals that the 4-aminopyridine substituent is bonded via the nitrogen atom of the amino group. The 11B NMR spectrum exhibits the characteristic feature (1:5:5:1) of a monosubstituated B12 cage with a downfield shift of ipso-B1 to -5.4 and antipodal-B12 to -18.1 ppm. The 1H NMR spectrum reveals the pattern of a monosubstituated pyridine. The IR and Raman spectra exhibit characteristic BH stretching vibrations between 2489 and 2521 cm-1 and the CC and CN stretching vibrations in the range of 1405 to 1636 cm-1.
Darstellung und Kristallstruktur von [P(C6H5)4]2[2-SnCl2(C6H5)B10H9] / Synthesis and Crystal Structure of [P(C6H5)4]2 [2-SnCl2(C6H5)B10H9]
Authors: Nachtigal C , Preetz W
Published: August 2018

By reaction of [N(C4H9)4]2[B10H10] with dichlorodiphenyltin in acetonitril at 80°C the 2- (dichlorophenyltin)-decaborate anion [2-SnCl2(C6H5)B10H9]2- is formed and can be isolated by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose. The X-ray structure of [P(C6H5)4]2[2-SnCl2(C6H5)B10H9] (triclinic, space group P1̄ with a = 11.2342(11), b = 11,2549(13), c = 22.265(6) Å, α = 89.478(14), β = 84.511(13), γ = 74.049(8)°) reveals that the SnCl2(C6H5) substituent is bonded with a B2-Sn distance of 2.182(6) Å.
Über ein cadmiumreiches Orthovanadat Ba2,5Cd11(VO4)9 mit Cadmium in oktaedrischer und tetragonal pyramidaler Koordination / On a Cadmium Rich Orthovanadate Ba2,5Cd11(VO4)9 Showing Cadmium in Octahedral and Square Pyramidal Coordination
Authors: Mertens B , Müller-Buschbaum Hk
Published: August 2018

Single crystals of Ba2,5Cd11(VO4)9 have been prepared by solid state reactions. The new compound crystallizes with orthorhombic symmetry, space group D142h-Pbcn, a = 20.842(6), b = 13.471(3), c = 11.838(9) Å, Z = 4. The crystal structure is characterized and dominated by CdO6 octahedra and unusual square pyramids of O2- around Cd2+ forming a three-dimensional [Cd11O36] network. The interstices are occupied by V5+ and Ba2+ ions. This results in VO4 tetrahedra and irregular BaO10 polyhedra isolated from each other. Occupation of the barium positions is deficient in agreement with the valence state V5+ and calculations of the coulomb terms of lattice energy.
Darstellung, Kristallstruktur und Schwingungsspektren von Rubidiumperoxoniobat (Rb3NbO8) / Preparation, Crystal Structure, and Vibrational Spectra of Rubidiumperoxoniobate (Rb3NbO8)
Authors: Haeuseler H. , Wagener M. , Müller H.
Published: August 2018

The crystal structure of Rb3NbO8 (SG I4̅2m, Nr. 121) has been determined on single crystals to a final R = 0.041. The structure is isotypic to the K3CrO8 type. Vibrational spectra of the title compound have been recorded on powdered samples and are discussed with respect to the internal vibrations of the peroxo-group and the dodecahedral NbO8
3- ion. The stretching vibrations of the O2
2- groups are found at 838 (Raman) and 813 cm- 1(IR). A factor group analysis for the K3CrO8 type is given.
Synthesis and Characterization of the Manganese Pyroarsenate Mn2As2O7 · 2H2O
Authors: Stock N. , Stucky G. D. , Cheetham A. K.
Published: August 2018

The manganese pyroarsenate hydrate, Mn2As2O7 · 2 H2O, has been obtained as a single phase product using hydrothermal methods and the structure has been determined by single crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group P21/n with a = 6.6576(4), b = 14.555(1), c = 7.8147(5) Å, β = 94.935(1)°, V = 754.46(8) Å3 and Z = 4. The manganese ions are each coordinated to five oxygen atoms and a water molecule in a distorted octahedral arrangement. Edge-sharing MnO6 octahedra form chains which are connected to a three-dimensional framework by As2O7
4- ions. The pyroarsenate anion, which attains a nearly eclipsed conformation, has a mean As-O distance for the terminal As-O bonds of 1.669(2) Å, while for the bridging oxygen atom a mean value of 1.757(2) Å is observed. Magnetic susceptibility measurements indicate the presence of high-spin Mn2+ ions. Thermogravimetric as well as IR and Raman spectroscopic studies of Mn2As2O7 · 2 H2O are presented.
Alkalimetall-Oxosilicate A6[Si3O9] und A6[Si2O7] (A = Rb, Cs): Darstellung und Kristallstruktur/ The Alkaline Metal Oxo-Silicates A6[Si3O9] and A6[Si2O7] (A = Rb, Cs): Preparation and Crystal Structure
Authors: Hoch C. , Röhr C.
Published: August 2018

The title compounds were synthesized via reaction of quartz and AO2 (A = Rb, Cs) with the elemental alkali metals. Their crystal structures were determined on the basis of single crystal X-ray data. All compounds crystallize in the monoclinic system with space group P21/c and lattice constants a = 656.0(l)/684.7(3), b = 1329.7(3)/1375.7(4), c = 1647.6(3)/1703.6(8) pm, β = 107.78(3)/108.23(2)°, Z = 4 (A6[Si3O9], A = Rb/Cs) and a = 668.59(8)/711.4(1), b = 911.37(9)/952.1(2), c = 1121.09(9)/1192.7(7) pm, β = 125.52(9)/126.22(3)°, Z = 2(A6[Si2O7], A = Rb/Cs) respectively. The rubidium and cesium compounds are isotypic with the corresponding potassium silicates.
Notizen: Efficient Medium-Scale Synthesis of 2-Bromo-5-tert-butylbenzene-1,3-dicarbaldehyde
Authors: Klingele Marco H. , Kersting Berthold
Published: August 2018

A short and efficient multi-gram synthesis of the title compound has been designed which al­lows its preparation from commercially available material in only three steps in overall yields of 60-70 % .
The Structure Directing Effect of Hydrogen Bonding in the Novel Polymeric Thioantimonate Mn2(H2N(CH2)2NH2)2Sb2S5
Authors: Schur Michael , Bensch Wolfgang
Published: August 2018

A new transition metal thioantimonate(III) with composition Mn2(H2N(CH2)2NH2)Sb2S5 has been synthesised under solvothermal conditions. Two trigonal SbSb3 pyramids and two octahedrally coordinated Mn atoms are interconnected to form Mn2SbS4 heterocubanes as secondary building units (SBU’s). The SBU’s are covalently linked into linear infinite onedimensional rods. Long Sb-S bonds connect the rods to form layers. The two N atoms of the ethylenediamine molecule (en) are chelating one Mn(II) ion. The amino hydrogen atoms of the en ligand are engaged in hydrogen bonding which is responsible for the different structure pattern of the title compound compared to a previously reported series of Mn-amino-thioantimonates(III) with analogous stoichiometry built up from different amino ligands.
Secondary Bonding Interactions in Some Haloanilinium Halides
Authors: Gray Lilian , Jones Peter G.
Published: August 2018

The crystal packing in the structures of various solvent-free (mono)haloanilinium halides involves with one exception the formation of approximately planar hydrophilic regions that contain classical hydrogen bonds N-H···X- (X = halogen). Common to the substructures of all layers are rings of general graph set Rn
2n(4n), involving equal numbers of chloride acceptors and NH2 moieties (two hydrogen atoms of the positively charged NH3 groups). The 2-substituted derivatives contain the shortest X···X- contacts, and these are within the layers; it could be argued that the contacts are forced upon the system by the 2-substitution pattern. In 3-chloroanilinium chloride and its bromine analogue, the layers consist of ribbons connected by short C-H···X- interactions. In all these compounds, the aromatic groups project from the layers and form hydrophobic regions; the layers are linked by weak interactions of the form X···X or C-H···X . There is appreciable interdigitation of hydrophobic groups from adjacent layers except for the ribbon structures. 3-Iodoanilinium iodide displays a completely different structure, in which all the atoms except some hydrogen atoms of the NH3 groups lie in a crystallographic mirror plane, but without forming separate hydrophilic and hydrophobic regions. The salt 4- bromoanilinium bromide could only be obtained as a hemihydrate; it too forms hydrophilic layers, but these are highly puckered.
Quaternary Phosphide Oxides Pr3Cu4P4O2–x and Sm3Cu4P4O2–x with Ordered Zr3Cu4Si6-Type Structure
Authors: Kaiser Joachim W. , Jeitschko Wolfgang
Published: August 2018

The compounds Ln3Cu4P4O2-χ (Ln = Pr, Sm) were prepared by annealing the elemental components in a NaCl/KCl flux. They crystallize with an ordered Zr3Cu4Si6-type structure (space group I4/mmm, Z = 2), which was refined from single-crystal X-ray data for both compounds; Pr3Cu4P4O2-χ: a = 397.8(1), c = 2658.7(3) pm, R = 0.046 for 235 structure factors and 19 variable parameters; Sm3Cu4P4O2-χ: a = 392.8(1), c = 2643.6(3) pm, R = 0.057 for 145 F values and 19 variables. The refinements showed partial occupancy for the oxygen positions resulting in approximately 1.5 oxygen atoms per formula unit. Half of the phosphorus atoms form pairs with typical two-electron bond distances of 222.8(4) and 221.7(8) pm, respectively. Using oxidation numbers chemical bonding in these phosphide oxides can be rationalized with the formula (Ln+3)3(Cu+1)4(P-P)-4(P-3)2(O-2)1.5. Hence, the empirical formula may also be doubled (Ln6Cu8P8O3), and the compounds are expected to be semiconducting.
Anodische Oxidation von 2-Thiobarbitursäuren unter Bildung neuartiger, tetracyclischer Dimerer / Anodic Oxidation of 2-Thiobarbituric Acids under Formation of New Tetracyclic Dimers
Authors: Thomas Hans Günter , Rasp Michael , Raabe Gerhard
Published: August 2018

2-Thiobarbituric acids 1 can be dimerized anodically in acceptable yields if the special ultrasonic electrolysis cell described here is used. In some cases two isomeric dimers 2 and 4 were isolated. 2 is of the same type as the corresponding barbituric acid dimers. The other dimer 4 has a completely different, tetracyclic structure characterized by NMR spectra and X-ray diffraction. The mechanism postulated for the formation of the tetracyclic dimers is supported by cyclovoltammetric measurements.
Multinuclear (1H, 13C and 15N) Magnetic Resonance Spectroscopy and Substituent Effects on N-Phenoxyethylanilines
Authors: Jios Jorge L. , Romanelli Gustavo P. , Autino Juan C. , Magiera Damian , Duddeck Helmut
Published: August 2018

1H, 13C and 15N NMR spectra of twenty substituted N-phenoxyethylanilines 1-20 were completely and unambiguously assigned using a combination of both homo- and heteronuclear (gs-COSY), 1H detected heteronuclear one-bond (gs-HMQC) and long-range (gs- HMBC) gradient-selected correlation experiments. Correlations between chemical shifts and substituent constants are analyzed separately for both phenyl rings using variable substituents para to the fixed substituent -OCH2CH2NHC6H5 (series I) and -NHCH2CH2OC6H5 (series II), respectively. The correlation coefficient for chemical shifts vs. a linear combination of inductive and resonance substituent constants is high and improves when only the six values, corresponding to each para-monosubstituted series, were used. For nitrogen chemical shifts excellent linear dependences were obtained. The results show that the ethylene chain is not able to transmit the substituent effect from one aromatic ring to the other.
Synthesis of C-Glycosides from S-Glycosyl Phosphorothioates
Authors: Kudelsk W.
Published: August 2018

Treatment of O-benzyl protected S-glucosyl phosphorothioates with 1,3,5 trimethoxybenzene in the presence of iodine or boron trifluoride etherate led to appropriate aryl C-β-Dglucosides. The reaction of O-benzyl and O-acetyl-protected phosphorothioates of monosaccharides with allyltrimethylsilane, using boron trifluoride etherate as activator, gave mainly or exclusively, the corresponding 3-(α-D- glycopyranosyl)-1-propenes. C-Glucosidation of furan with O-benzyl protected S- glucosyl phosphorothioate in the presence of boron trifluoride etherate afforded (2- furyl)-α-C-glucoside.
Complexation of Organic Dyes by Peptides Built of Lysine and Glutamic Acid Amides
Authors: Mehlmann Heinz , Olschewski Daniel , Olschewski Andrey , Feigel Martin
Published: August 2018

Two amide libraries, Fmoc-[Lys(aci)]4-Gly-resin (1) (aci = 2-naphthylcarbonyl, 1-adamantylcarbonyl and benzyloxycarbonyl) and Fmoc-[δ-Glu(α-amidei)]4-Gly-resin (2) (amidei = morpholineamide, piperidineamide, (N´-phenyl)-piperazineamide), have been synthesized from the corresponding Fmoc-protected amino acid derivatives. Beads of the libraries complex organic dyes (crystal violet and Sudan black) differently according to the sequence of residues in 1 or 2. The results are considered a step towards artificial receptors for small organic molecules build from linear oligoamides.
A Novel Ring Enlargement of 2H-Azirine-3-methyl(phenyl)amines via Amidinium-Intermediates: A New Synthetic Approach to 2,3-Dihydro-1,3,3-trimethylindol-2-one
Authors: Mekhael Maged K.G , Smith Richard J. , Bienz Stefan , Linden Anthony , Heimgartner Heinz
Published: August 2018

2,2,N-Trimethyl-N-phenyl-2H-azirin-3-amine (1a) was prepared by successive treatment of 2,N-dimethyl-N-phenylpropanamide (18) with phosgene, triethylamine, and sodium azide. Reaction of 1a in THF solution with boron trifluoride gave 2-amino-1,3,3-trimethyl-3H-indolium tetrafluoroborate (19) in high yield.T he latter reacted with acetic anhydride in pyridine to give a mixture of N-(2,3-dihydro-1,3,3-trimethylindol-2-yliden)acetamide (22) and 2,3-dihydro- 1,3,3-trimethylindol-2-one (21).On hydrolysis with aqueous HCl, 22 was converted to 21.T he molecular structures of 19 and 22 were established by X-ray crystal structure determination.
Pyrido[1,2-a]pyrazine - Startprodukte für regioselektive Ringtransformationen und supramolekulare Architekturen / Pyrido[1,2-a]pyrazines - Starting Materials for Regioselective Ringtransformation Reactions and Supramolecular Architectures
Authors: Müller D. , Frank B. , Beckert R. , Görls H.
Published: August 2018

The easily available pyrido[1,2-a]pyrazines of type 1 are versatile building blocks for ring transformation reactions.W ith heterocyclic quinones such as quinoline-2,5,8-triones 4a-c, a highly regioselective [4+2]-cycloaddition reaction takes place in the first step, followed by a ring transformation cascade.T he 1,6-diazaanthracene-2,9,10-triones 5a-e, which possess an additional bipyridine substructure, could be isolated as main products.In order to modify the starting products of type 1, a metal-catalyzed cross-coupling reaction with acetylenic benzoic esters 9a,b has been performed.T he modified pyridopyrazines 10a,b which were obtained in good yields could be transformed by analogy to 1a,b into ring-fused heterocyclic quinones 12a,b.
Redetermination of Bis(η4-1,3-cyclohexadiene)monocarbonyliron
Authors: Reiß Guido J.
Published: August 2018

The crystal structure of bis(η4-1,3-cyclohexadiene)monocarbonyliron has been redetermined by X-ray data. The compound crystallizes in the enantiomorphic, orthorhombic space group P212121 with one complete molecule in the asymmetric unit. For concordance to the originally reported structure, which was determined under ambient conditions, the redetermination has been carried out at room temperature and at low temperature (T = 293 K: a = 7.618(2), b = 8.522(2), c = 17.138(4) Å, V = 1112.6(5) Å3, R1 = 0.0226, wR2 = 0.0539; T = 120 K: a = 7.509(2), b = 8.417(3), c = 16.778(6) Å, V = 1060.3(6) Å3, R1 = 0.0242, wR2 = 0.0533). The redetermination proved this complex to have non-crystallographic C2v point group symmetry. Correlation effects to the atomic coordinates and displacement parameters introduced problems during the structure refinement caused by pseudo-symmetry of the molecule. All bond lengths, angles, and torsion angles appear in this revised crystal structure in the normal range for π-coordinated diene transition metal complexes.
Spectroscopic Studies on Bis(3,5-di-t-butyl-1,2-benzoquinone 1-oximato)copper(II) and its Mixed-Ligand Complexes. Copper(II)-Radical Ferromagnetic Coupling
Authors: Kasumov Veli T. , Taş Eşref , Yakar Yasin , Köksal Fevzi , Köşeoğlu Rahmi
Published: August 2018

Bis(3,5-di-t-butyl-1,2-benzoquinone 1-oximato)copper(II), Cu(ox)2, and its mixed-ligand complexes, Cu(ox)Lx [Lx = 8-hydroxyquinolinato (L1), N-Phenyl-salicylaldimine (L2), N-phenyl- 3,5-di-t-butylsalicylaldiminato (L3) and N-(2-hydroxyphenyl)-3,5-di-t-butylsalicyl-aldiminato (L4)], were prepared and their spectral behavior as well as redox-reactivity towards PPh3, (m-ClC6H4)3P, (m-CH3C6H4)3P and PPh2-(CH2)4-PPh2 studied by analytical and spectroscopic (IR, UV-vis, ESR) techniques and magnetic measurements. Cu(ox)2 and Cu(ox)L4 complexes prepared in air show μef values of 2.84 and 3.33 μB, respectively, and are consistent with an S= 1 and S= 3/2 ground states. Both compounds are formulated as copper(II)-radical complex exhibiting intramolecular ferromagnetic coupling between the orthogonal dx
2
-y
2 magnetic orbital of the CuII ion and that of the π-radical ligand.
Octahedral Complexes of Fe(III) with Phosphorylic Ligands Closely Related to β-Diketones
Authors: Trush Elizaveta A , Ovchynnikov Vladimir A , Domasevitch Konstantin V , Swiatek-Kozlowska Jolanta , Zub Vera Ya , Amirkhanov Vladimir M
Published: August 2018

Iron(III) coordination compounds of the general formula FeL3 (where L1 = {CCl3C(O)NP(O)-[N(C2H5)2]2
-}-N,N'-tetraethyl-N''-trichloroacetylphosphorictriamide anion, and L2 = {CCl3- C(O)NP(O)[N(CH2CH2)2O]2}--dimorpholido-N-trichloroacetylphosphoricamide anion) have been synthesized and characterized by means of IR, UV-VIS, ESR spectroscopy, and X-ray analysis. The complexes have a molecular structure with the phosphoryl ligands coordinated to the metal ioninabidentatemanner via phosphoryl and carbonyl oxygen atomswith formation of six membered chelate rings. The coordination around the Fe(III) atoms is distorted octahedral, to give fac-isomers in both structures.
Synthesis and Structure of the First Transition Metal Complex with Methanesulfonylhydrazine as a Ligand
Authors: Ienco A. , Mealli C. , Dodoff N. I.
Published: August 2018

The article reports the first transitionmetal complex of methanesulfonylhydrazine, a molecule known for important pharmacological and chemical applications. The complex [ZnCl2(MSH)2], MSH = CH3SO2NHNH2, has been synthesized and its structure characterized by means of X-ray analysis. The coordination geometry is pseudo-tetrahedral and the ligand MSH adopts a conformation that was found by previous ab initio calculations to be a transition state and not a stationary point for the free ligand.
Der (2-Phenyl-2-trimethylsilyl)ethyl-(PTMSE)-Ester – eine neutral spaltbare Carboxyschutzgruppe/The (2-Phenyl-2-trimethylsiylyl)ethyl (PTMSE) Ester – a Carboxy Protecting Group Cleavable under Neutral Conditions
Authors: Wagner Michael , Kunz Horst
Published: August 2018

(2-Phenyl-2-trimethylsilyl)ethyl (PTMSE) esters of aminoacids and peptides are stable under the conditions of hydrogenolytic cleavage of benzoxycarbonyl(Z) and benzyl ester groups, base-induced removal of Fmoc groups, palladium(0)-catalyzed removal of allyloxycarbonyl (Aloc) and even acidolytic cleavage of Boc groups. PTMSE esters are also stable under the conditions of peptide condensation reactions. The PTMSE ester is selectively cleaved by treatment with tetrabutylammonium fluoride (TBAF) trihydrate in dichloromethane, i. e. under almost neutral conditions, within a few minutes and, therefore, considered a valuable novel carboxy protecting group.
Bis(triphenylphosphoranylidene)ammonium Dicyanoaurate(I)
Authors: Liau Ruei-Yang , Ehlich Hendrik , Schier Annette , Schmidbaur Hubert
Published: August 2018

Partially 13C-labeled alkali dicyanoaurates M[Au(CN)2] were prepared and investigated by NMR and IR spectroscopy in aqueous solution. For the range of concentration investigated the data obtained under standard conditions provided no evidence for anion association. The salt [Ph3PNPPh3][Au(CN)2] was also prepared and the crystal structure of the dichloromethane solvate determined. There is no anion aggregation in the crystal, and short contacts of the anions are only discernible with the solvent molecules. A literature survey of crystal structure data for dicyanoaurate(I) salts (almost 35 entries) show that inter-anionic contacts are only observed in structures with small cations or with cations exerting a directional influence.
Die neuen Oxobismutate(III) Cs6Bi4O9, K9Bi5O13 und A2Bi4O7 (A = Rb, Cs) / The New Oxobismutates(III) Cs6Bi4O9, K9Bi5O13 and A2Bi4O7 (A = Rb, Cs)
Authors: Emmerling Franziska , Röhr Caroline
Published: August 2018

The title compounds were synthesized at a temperature of 700 °C via oxidation of elemental Bi with the hyperoxides AO2 or via reaction of the elemental alkali metals A with Bi2O3. Their crystal structures have been determined by single crystal x-ray diffraction. They are dominated by two possible surroundings of Bi by O, the ψ-trigonal-bipyramidal three (B) and the ψ-tetrahedral four (T) coordination. Cs6Bi4O9 (triclinic, spacegroup P1̄, a = 813.82(12), b = 991.60(14), c = 1213.83(18) pm, α = 103.658(2), β = 93.694(3), γ = 91.662(3)°, Z = 2) contains centrosymmetric chain segmentes [Bi8O18]12- with six three- (T) and two four-coordinated (B) Bi(III) centers. K9Bi5O13 (monoclinic, spacegroup P21/c, a = 1510.98(14), b = 567.59(5), c = 2685.6(2) pm, β = 111.190(2)°, Z = 4) is a mixed valence compound with isolated [BivO4]3- tetrahedra and chains [BiIII
4O9]6- of two T and two B coordinated Bi. In the compounds A2Bi4O7 (A = Rb/Cs: monoclinic, C2/c, a = 2037.0(3) / 2130.6(12), b = 1285.5(2) / 1301.9(7), c = 1566.6(2) / 1605.6(9) pm, β = 94.783(3) / 95.725(9)°, Z = 8) ribbons [Bi4O6O2/2]2- are formed, which are condensed to form a three-dimensional framework.
Crystal Structure and Magnetic Properties of (2,2'-Dipyridyl)-(2-acetylphenolato)copper(II) Perchlorate
Authors: Elmali A. , Elerman Y. , Svoboda I.
Published: August 2018

The mixed-ligand dinuclear complex (2,2'-dipyridyl)-(2-acetylphenolato)copper(II) perchlorate was synthesized and its crystal structures determined. The structure consists of a dimeric unit involving a planar Cu2O2 group. The coordination sphere of the Cu atom can be described as an alongated octahedron where the basal plane is formed by the two N atoms of the 2,2'-dipyridyl molecule and the two O atoms of the acetophenon anion. Two apical Cu - O contacts complete the 4+2 coordination of the Cu atoms. They correspond to one of the O atoms of the perchlorate anion and to the O atom of the second unit. Magnetic susceptibility data obey the Curie-Weiss law with θ = -8.1(2) K. The decreasing of the effective magnetic moment from 1.94(8) μB at 300 K to 1.86(8) μB at 70 K and the negative Weiss constant indicate weak antiferromagnetic interactions between the two copper atoms in the dimeric units.
Ternary Antimonides YbTSb (T = Ni, Pd, Pt, Cu, Ag, Au) – Synthesis, Structure, Homogeneity Ranges, and 121Sb Mössbauer Spectroscopy
Authors: Mishraa Ratikanta , Pöttgen Rainer , Hoffmann Rolf-Dieter , Fickenscher Thomas , Eschen Marcus , Trill Henning , Mosel Bernd D.
Published: August 2018

The ternary antimonides YbTSb (T = Ni, Pd, Pt, Cu, Ag, Au) were synthesized by reaction of the elements in sealed tantalum tubes in a high-frequency furnace. The structures of YbCuSb (NdPtSb type), YbAgSb (TiNiSi type), and YbAuSb (NdPtSb type) were confirmed on the basis of X-ray powder diffraction data. Those of the nickel, palladium, and platinum based antimonides (cubic MgAgAs type) were refined from single crystal X-ray data. The nickel based antimonide has a pronounced homogeneity range YbNixSb. The structures of five crystals have been investigated. The cubic lattice parameter increases with increasing nickel content from 613.13(6) pm(x = 0.17) to 621.25(5) pm (x = 0.63). Full occupancy of the palladium and antimony sites was observed for YbPdSb while the platinum compound shows some platinum vacancies leading to the composition YbPt0.969(7)Sb for the investigated crystal. A new, hightemperature modification of YbPdSb was obtained by rapidly quenching an arc-melted sample: TiNiSi type, Pnma, a = 725.6(2), b = 458.3(1), c = 785.4(2) pm, wR2 = 0.1255, 421 F2 values, 20 variables. The antimonides YbTSb (T = Ni, Pd, Pt, Cu, Ag, Au) show single 121Sb Mössbauer signals at isomer shifts ranging from -7.34 to -7.82 mm/s. The crystal chemistry and chemical bonding of these antimonides is discussed.
Isomerisation of Alkenes Bearing Stannyl and Boryl Groups at the C=C Bond
Authors: Wrackmeyer Bernd , Kerschl Susanna , Klaus Uwe
Published: August 2018

Alkenes bearing organometallic substituents such as boryl and stannyl groups isomerise slowly in the absence of UV irradiation. In addition to cis/trans isomerisation the boryl and stannyl group may also exchange places. This is shown for (Z)-2-chloro(dimethyl)stannyl-3-diethylboryl- pent-2-ene 5b (conversion into (Z)-3-chloro(dimethyl)stannyl-2-diethylboryl-pent- 2-ene 7b) and 3,4-diethyl-1,1,2,5-tetramethyl-1,2-dihydro-1,3-stannaborole8b (conversion into 3,5-diethyl-1,1,2,4-tetramethyl-1,2-dihydro-1,3-stannaborole 9b). Zwitterionic structures, involving a bridging boryl group with π-σ delocalisation, the stabilising effect exerted by a stannyl group in β-position with respect to a positively charged centre, and migration of a stannyl group, are suggested in oder to explain the isomerisation. The heterocycle 9b was prepared independently from the reaction of 7b with lithium diisopropylamide.
Molecular Complexes, 13. Weak Arene Complexes of Nitroaromatics. 1H NMR Studies of Conformations and Polar Effects. syn-anti Selectivity of 5-Nitrofurfural
Authors: Stamm Helmut , Strumm Hanns-Otto , Jäckel Hannelore , Beijer Barbro , Schilling Gerhard , Bethke Sabine
Published: August 2018

The refined 1H NMR method (AUS concept, CCl4) provided association constants K and approximate complex shifts IK for complexes of nitroaromatics A with aromatic hydrocarbons D. 5-Nitrofurfural (1) and benzene (B) or toluene (T) form syn-1B or syn-1T, respectively; a proton dependence of K indicates about 10% anti complexes. The dimer T2 of T additionally yields some 1T2 since IK values are 29-34% higher than for 1B. With naphthalene (N) or phenanthrene all protons of 1 provide the same K. Picrylacetone (2) and B form 2B and at least one 2BB adduct; published parameters of 2B and 2BB are inconsistent. 2 and N or M (1,3,5-trimethylbenzene) form only 1:1 complexes. All results are in accord with CH2COMe standing perpendicular to picryl. 2,4-Dinitrophenylacetone (3) in a rather flat conformation coordinates with a single stacking N centred over C-6; 3 yields two isomeric stacking complexes 3B and at least one edge-on 3B complex. 2-Chloro-5-nitropyridine (5) forms stacking complexes under repulsion of D by the ring N. In contrast to 1 and 4-nitrobenzaldehyde (6) 1,4-dinitrobenzene (7) and T form only a 1:1 complex that is stabilized by dipole-dipole attraction. Equal and unequal shielding of proton pairs (ortho or meta) in complexes of type 6B is discussed.
Zur Kenntnis von Calciumtetrahydrogen-hexaoxo-diperiodattetrahydrat CaH4I2O10 · 4 H2O: Kristallstruktur, Schwingungsspektren und thermische Analyse / On Calciumtetrahydrogen-hexaoxo-diperiodatetetrahydrate CaH4I2O10 · 4 H2O: Crystal Structure, Vibrational Spectroscopy and Thermal Analysis
Authors: Haeuseler H. , Botova M.
Published: August 2018

By crystallisation from a strongly acidic aqueous solution calciumtetrahydrogen-hexaoxo-diperiodatetetrahydrate CaH4I2O10 ∙ 4 H2O has been obtained. In the structure of this compound (S.G. C2/c, Nr. 15), Z = 4, a = 1986,6(4), b = 564,2(1), c = 1149,4(20) pm, β = 120,62(3)°) centrosymmetric H4I2O10
2− anions in the form of edge-sharing octahedra form layers via hydrogen bonds originating from the acidic, trans-configurated OH groups of the anions. IR and Raman spectra are analysed with respect to the hydrogen bond system and the internal vibrations of the periodate anion. The dehydration of the compound takes place via Ca(IO4)2 ∙ 5 H2O and Ca(IO4)2 ∙2H2O leading at 143°C to the anhydrous metaperiodate Ca(IO4)2 which decomposes above 248°C to Ca(IO3)2.
Mg5Pd10Si16 und Mg5Pt10Si16, Magnesium-Platinmetall-Silicide mit Tetraedern und gekappten Tetraedern aus Silicium-Atomen / Mg5Pd10Si16 and Mg5Pt10Si16, Magnesium Platinum Metal Silicides with Si4 Tetrahedra and Si12 Truncated Tetrahedra
Authors: Lorenz Peter , Jung Walter
Published: August 2018

The ternary silicides Mg5Pd10Si16 and Mg5Pt10Si16 have been prepared by reaction of magnesium with the binary platinum-metal silicides in sealed tantalum containers (Pt-compound: 1200°C, 3 d, up 20 °/h, down 5 °/h; Pd-compound: 1000°C, 2 d, up and down 50 °/h). In the case of the Pd-compound contact with the tantalum had to be avoided by using a boron nitride crucible. The isotypic compounds crystallize in the cubic space group F4̄3m with 4 formula units per unit cell. The crystal structures were determined from single crystal data, lattice constants from Guinier patterns. The following data were obtained: a = 1258.81(8) pm for Mg5Pd10Si16 and a = 1256.94(9) pm for Mg5Pt10Si16. Short distances in the three-dimensional platinum-metal silicon network indicate strong, covalent Pd(Pt)-Si-bonding (d(Pd-Si) = 240.2 to 256.1 pm; d(Pt-Si) = 237.1 to 258.5 pm). In addition, homonuclear bonding seems to be important, resulting in the formation of Si4-tetrahedra (d(Si-Si) = 250.4 pm (Mg5Pd10Si16) and 255 pm (Mg5Pt10Si16)), empty Si12-polyhedra with the shape of truncated tetrahedra (d(Si- Si): 234.5 and 248.2 pm (Mg5Pd10Si16); 236 and 248.2 pm (Mg5Pt10Si16)), and Mg-centered Pd(Pt)10-clusters with the shape of adamantane (d(Pd-Pd) = 282.3 pm; d(Pt-Pt) = 284.5 pm). Furthermore, Mg4-tetrahedra with Mg-Mg-distances of 360 pm are formed. The structure may be described by an expanded cubic “close” packing of MgPd(Pt)10-units in which the Si4-tetrahedra occupy the octahedral holes while the Si12-polyhedra and the Mg4-tetrahedra reside in one half of the tetrahedral holes each.
Polyol-Metall-Komplexe, 43 [1]. Galactarato-Komplexe mit Aluminium und Kupfer(II) / Polyol Metal Complexes, 43 [1]. Galactarato Complexes with Aluminium and Copper(II)
Authors: Klüfers Peter , Kramer Gernot , Piotrowski Holger , Senker Jürgen
Published: August 2018

Na6[Al6(Gal1,6A21,2,5,6H−4)4(OH)8] ∙ 21 H2O (1) crystallizes from alkaline aqueous solutions of galactaric acid (Gal1,6A2) and aluminium nitrate. Crystal structure analysis (P1̄, a = 9.09950(10), b = 15.1996(2), c = 21.9667(3) Å , α = 96.6190(5), β = 90.5307(4), γ = 103.5658(5)°, V = 2931.66(6) Å3, Z = 2) and solid state 27Al NMR spectroscopy reveal rings of six edge-sharing AlO6 octahedra, the O-atoms stemming from four galactarato and eight hydroxo ligands. The potassium homologue K6[Al6(Gal1,6A21,2,5,6H−4)4(OH)8] ∙ 23 H2O (2) is not isotypic (P21/c, a = 9.7604(6), b = 22.0843(17), c = 30.1534(17) Å , β = 95.970(7)°, V = 6464.4(7) Å3, Z = 4), but the anion structure is the same. Pure polyolato coordination of entirely deprotonated galactarate has been found in Na4[Cu(Gal1,6A2H−6)]] ∙ 12 H2O (3). In 3, a coordination polymer is formed by the copper atoms and the erythro-bis-diolate ligand (P1̄, a = 5.9711(2), b = 9.5319(3), c = 9.7794(3) Å , α = 99.883(2), β = 100.807(2), γ = 105.9182(11)°, V = 510.90(3) Å3, Z = 1).
Synthesis and Characterisation of Na5[CoO2]CO3
Authors: Sofin Mikhail , Peters Eva M. , Jansen Martin
Published: August 2018

Na5[CoO2]CO3 was prepared via the azide/nitrate route. Stoichiometric mixtures of the precursors (Co3O4, NaN3, NaNO3 and Na2CO3) were heated in a special regime up to 500 °C and annealed at this temperature for 50 h in silver crucibles. Single crystals have been grown by subsequent annealing of the powder at 500 °C for 2000 h in silver crucibles, which were sealed in glass ampoules under dry Ar. According to the X-ray analysis of the crystal structure (P4/mmm, Z = 1, a = 4.6467(4), c = 8.2577(6) Å ). Na5[CoO2]CO3 is isostructural with Na5[NiO2]CO3 and contains Co1+, which is coordinated by two oxygen atoms forming a dumb-bell. Na5CoCO5 decomposes at 600 °C to Na3CoO2 and Na2CO3.
Metal Directed One-Pot Syntheses: Mono-, Di- and Tetra-Nuclear Clusters [1]
Authors: Saalfrank Rolf W. , Reimann Uwe , Hampel Frank , Goebel Cornelia , Herbst-Irmer Regine
Published: August 2018

Upon reaction of HL1 1 (picoline-tetrazolylamide) with cobalt(II) acetate under aerobic conditions or with copper(II) acetate, the mono-nuclear complex [CoIII(L1)3] 3 and the di-nuclear complex [Cu2(L1)4] 4 were generated. In 3 and 4, (L1)− exclusively coordinates across its nitrogen donors. However, when HL2 5 (picoline-tetrazolylthioamide) was reacted with copper- or nickel acetate, the di-nuclear cluster [Cu2(L2)4] 6 and the tetra-nuclear cluster [Ni4(L2)8] 7, respectively, were isolated. Contrary to 3 and 4, in 6 and 7, (L2)− also coordinates across sulfur.
New Coordination Polymers Based On Transition Metal Squarates And Pyrazine Ligands
Authors: Näther Christian , Greve Jan , Jeß Inke
Published: August 2018

Three new coordination polymers have been prepared by hydrothermal reaction of squaric acid, pyrazine and the metal halides FeCl2 · 4H2O, CoBr2 and NiBr2. In their crystal structures the metal atoms are coordinated by four water molecules and two pyrazine ligands within slightly distorted octahedra. The pyrazine ligands connect the metal atoms via μ-N,N’-coordination to linear chains which are connected via hydrogen bonding. The squarate dianions are not coordinated to the metal atoms and are located between the chains. The thermal behaviour of all compounds was investigated using TG-DTA-MS measurements. A complex behaviour for all compounds is found and the decomposition temperatures increase from Fe to Ni. From these investigations there are no hints for the occurrence of stoichiometric intermediate compounds.
Synthesis of 2-Phenylisothiazol-3(2H)-One 1,1-Dioxides: Inhibitors of Human Leukocyte Elastase
Authors: Gütschow Michael , Pietsch Markus , Taubert Kathleen , Freysoldt Tonia H. E. , Schulze Bärbel
Published: August 2018

A series of 2-phenylisothiazol-3(2H)-one 1,1-dioxides 14a - q were synthesized by oxidation of isothiazolium perchlorates 12. The inhibition of the serine proteases cathepsin G, chymotrypsin and human leukocyte elastase (HLE) by 14 was investigated. Some 4,5-diphenyl substituted derivatives ( 14i - k) were found to inhibit HLE in a time-dependent manner and exhibited kobs/[I] values > 500 M−1s−1. 14k (kobs/[I] = 2400 M−1s−1), was the most potent HLE inhibitor of this series. Kinetic investigations led to the conclusion that 2-phenylisothiazol-3(2H)-one 1,1-dioxides interact with HLE at the active site as well as at another binding site, resulting in a complex type of inhibition.
A Zwitterionic Platinum Complex with a Carbene Ligand
Authors: Marx Thiemo , Wesemann Lars , Hagen Siegbert , Pantenburg Ingo
Published: August 2018

A new stannaborate complex of platinum is prepared from the reaction of [Bu3MeN]2[trans- (Et3Pt)2Pt(SnB11H11)2] and 1,3-diisopropyl-4,5-dimethylimidazol-2-ylidene (dpdmiy). [trans- (Et3P)2Pt(SnB11H11)(dpdmiy)] has been analyzed by X-ray crystallography and NMR spectroscopy.
Bis(trimethylphosphan)-η5-cyclopentadienyl- tert- butylimidovanadium( III): Reaktionen mit Schwefel, Selen, Tellur und Iod
Authors: Billen Martin , Hornung Gabriele , Wolmershäuser Gotthelf , Preuss Fritz
Published: August 2018

The reaction of [tBuN=VCp(PMe3)2] (1) with S8, Se, Te or I2 have been studied. Via this pathway dinuclear diamagnetic tert-butylimidovanadium(IV) complexes are formed: [(μ-E)(μ- NtBu)2V2Cp2] (E=S, Se, Te), [(μ-η1−E2)(μ-NtBu)2V2Cp2] {E=Se (3), Te}, [(μ-NtBu)2V2Cp2I2]. In addition the vanadium(V) complexes [tBuN=VCp (S5)] (9a) and tBuN=VCpI2 could be isolated. The synthesis of tBuN=VCpF2 is also described. All compounds obtained have been characterized by spectroscopic methods (MS; 1H, 13C, 51V NMR), 3 and 9b by single crystal X-ray diffraction analysis.
Crystal Structure and Magnetic Properties of a New Hetero-Dinuclear CuIIMnII Schiff Base Complex
Authors: Elerman Y. , Elmali A. , Zeyrek C. T. , Svoboda I. , Fuess H.
Published: August 2018

Mn[Cu(L)(O2CMe)2] · H2O (L = N,N’-bis(2-hydroxy-3-methoxybenzylidene)-1,3-diaminopropane) was synthesized and the crystal structure determined. (C23H26CuMnN2O8).H2O, monoclinic, space group P21/c, a = 12.017(3), b = 8.217(3), c = 24.786(4) Å , β = 92.10(2)°, V = 2446(1) Å3, Z = 4. The crystal structure consists of ordered dinuclear units with CuII and MnII ions bridged by two oxygen atoms of the Schiff base ligand. The CuII coordination sphere is a slightly distorted square-plane formed by the N2O2 donor set of the Schiff base ligands. The average Cu-O and Cu-N distances are 1.920(1) and 1.957(4) Å , respectively. The coordination around the MnII ion is a distorted tetrahedron with the donor oxygen atoms of the Schiff base ligands and oxygen atoms of the acetate anions. The Cu ··· Mn separation is 3.327(4) Å . There is also one non-coordinating water molecule in the crystal structure. The χ and χT versus T plots, χ being the molar magnetic susceptibility per CuIIMnII unit and T the temperature, has been measured in the 4.9 - 301 K temperature range. The values of the interaction parameters are J = −28.3 cm−1, gMn = 2.01, gCu = 2.07. This indicates an intramolecular antiferromagnetic interaction between CuII and MnII ions.
Crystal Structure of a New Dimethyl Carbonate/2,4,6-Tris(trifluoromethyl)- 1,3,5-triazine 1:1 Adduct
Authors: Boese O. , Troyanov S. I. , Kemnitz E.
Published: August 2018

The crystal structure of a new 1:1 complex of dimethyl carbonate and 2,4,6-tris(trifluoromethyl)-1,3,5-triazine is reported. A high tendency of sublimation was observed by differential thermal analysis (DTA) and thermogravimetry (TG). Donor-acceptor interactions between dimethyl carbonate and 2,4,6-tris(trifluoro-methyl)-1,3,5-triazine are assumed to be responsible for the complex formation.
Behaviour of Bimetallic Pt-Pd Carbon-Supported Catalysts in Methanol Electrooxidation
Authors: Gökağaç G. , Léger J.M. , Hahn F.
Published: August 2018

Carbon powder supported bimetallic 8w%Pt+8w%Pd/C,8w%Pt+6w%Pd/C, 8w%Pt+4w%Pd/C, 8w%Pt+2w%Pd/C, 8w%Pt/C and 8w%Pd/C samples were prepared, characterised and tested for the electrooxidation of methanol. The particle sizes were found to depend greatly on the composition and the metal content. With pure palladium and samples rich in palladium, the diameter of the bimetallic particles was around 150 nm, but with pure Pt and samples poor in Pd it was much smaller, below 5 nm. The electrocatalytic activity of these catalysts was determined by cyclic voltammetry and polarization curves. Compounds with 33 and 43 at%Pd were the most active catalysts for the methanol oxidation reaction. A good correlation was obtained between electrochemistry and in situ infrared reflectance spectroscopy results.
Synthesis of the Pyrrole-Imidazole Alkaloid Sventrin from the Marine Sponge Agelas sventres
Authors: Breckle Gregor , Polborn Kurt , Lindel Thomas
Published: August 2018

The marine pyrrole-imidazole alkaloid sventrin (1) and the hitherto unknown dehydrooroidin (3) have been synthesized stereoselectively via alkyne intermediates. The pathways start from a 2-azido-4-alkynylimidazole which can be chemo- and stereoselectively reduced to the corresponding amino alkene using NaAlH2(OCH2CH2OMe)2 (Red-Al) or, alternatively, to the amino alkyne. Selective removal of simultaneously present Boc or trityl protecting groups was possible employing either p-TsOH or acetic resp. formic acid.
2-Amino-1,3-dimethylimidazolium 2,2-Dimethyl-4,6-dioxo-1,3-dioxanide. First Structural Characterisation of the Anion of Meldrum’s Acid [1]
Authors: Kuhn Norbert , Al-Sheikh Ahmed , Steimann Manfred
Published: August 2018

2-Amino-1,3-dimethylimidazolium 2,2-dimethyl- 4,6-dioxo-1,3-dioxanide (6) has been obtained from the reaction of 2,2-dimethyl-4,6-dioxo-1,3- dioxan (1, “Meldrum’s acid”) and 2-imino-1,3-dimethylimidazoline (5) in excellent yield. The unit cell of 6 contains two crystallographically independent anions lying on crystallographic mirror planes. The structure of the anion is compared with that of compound 1.
Synthesis, Characterization, Crystal Structure and Magnetic Properties of [(en)CuII(ImH)2](ClO4)2 (en = Ethylenediamine, ImH = Imidazole): A Metalloligand as a Building Block for Heterometal Chains
Authors: Glaser Thorsten , Heidemeier Maik , Hahn F. Ekkehardt , Pape Tania , Lügger Thomas
Published: August 2018

The reaction of Cu(ClO4)2·6H2O, imidazole (ImH), and ethylenediamine (en) in a 1 : 2 : 1 ratio afforded in high yield dark-blue single-crystals of [(en)CuII(ImH)2](ClO4)2, 1, which can be used after deprotonation as a building block for heterometallic ferrimagnetic chains. The structural and electronic properties of 1 were examined by X-ray crystallography, FTIR, ESI-MS, electrochemistry, UV/vis/NIR, EPR, and magnetic susceptibility measurements. The structure of 1 exhibits intermolecular π-π interactions and hydrogen bonds but the magnetic data exclude the presence of intermolecular exchange interactions.
Synthese und Struktur des Ammoniumsesquicarbonat Monohydrates (NH4)4[H2(CO3)3] ·H2O
Authors: Margrafa Günter , Lernera Hans-Wolfram , Bolteb Michael , Wagnera Matthias
Published: August 2018

The ammonium sesquicarbonate monohydrate (NH4)4[H2(CO3)3] · H2O is obtained from the reaction of hexamethyldisilazane with carbon dioxide in tetrahydrofuran in the presence of water. The structure of (NH4)4[H2(CO3)3] · H2O has been determined by X-ray crystal structure analysis.
K4Ti3Te9 – A New Pseudo One-Dimensional Polyanionic Alkali Chalcogenometallate(IV)
Authors: Kolb Andreas , Klepp Kurt O.
Published: August 2018

Lustrous black needle shaped single crystals of K4Ti3Te9 were obtained by reacting K2Te with the corresponding elemental components at 1000 °C. K4Ti3Te9 is monoclinic, mP64, s. g. P21/c (No. 14), Z = 4 with a = 9.052(2), b = 8.088(1), c = 29.465(9) Å , β = 92.35(1)°. The crystal structure was determined from diffractometer data and refined to a conventional R value of 0.035 (2840 Fo’s, 146 variables). The compound contains undulating polyanionic chains built up by severely distorted TiTe6 octahedra sharing opposite faces which run parallel to [100] and are arranged in a hexagonal rod packing. The translation period comprises three octahedra. The most striking feature of this compound is the formation of two ditelluride groups per formula unit with unusually long Te-Te distances of 2.960(2) and 3.025(2) Å, respectively. All other Te-Te distances start at 3.2 Å . The nearest homonuclear neighbours of the two pairs are at 3.215(2) and 3.333(2) Å apart. Ti-Te bond lengths range from 2.700(3) to 2.841(3) Å with an average value of 2.772(4) Å for all three crystallographically independent titanium atoms. The alkali cations are irregularly coordinated by 7 to 9 tellurium atoms.
Crystal Structure and Magnetic Properties of a CeIII –CuII Heterodinuclear Complex
Authors: Elmali Ayhan , Elerman Yalçin
Published: August 2018

Crystal structure and magnetic properties of a heterodinuclear complex, LCu(Me2CO)Ce(NO3)O3 (L = (N,N’-propylene-bis(3-methoxysalicylideneimine)) are reported. (C19H22N2O4)Cu(C3H6O) Ce(NO3)3, monoclinic, space group P21/c, with a = 9.8295(4), b = 19.049(3), c = 15.668(3) Å , β = 94.873(12)◦, V = 2923.2(7) Å3, Z = 4. The central region of the complex is occupied by CuII and CeIII ions which are bridged by two phenolato oxygen atoms of the ligand. The copper ion adopts a square-based 4+1 coordination made, the equatorial N2O2 donors being afforded by the ligand while the axial position is occupied by an oxygen atom of the acetone molecule. The CeIII ion is deca-coordinated. In addition to the two phenolate oxygen atoms, the coordination sphere contains two oxygen atoms of the OMe side arms of L and six oxygen atoms from the three bidentate nitrate ions. The Ce···Cu separation is 3.601(2) Å and the dihedral angle between the CeO(2)Cu and CeO(3)Cu planes is 17.4(1)°. The magnetic susceptibility of the complex was measured over the range 5 - 350 K. The magnetic properties of the investigated compound are dominated by the crystal field effect on the CeIII site, masking the magnetic interaction between the paramagnetic centers.
6-Phenyldibenzo[b,d]phosphinine
Authors: Koe Pieter de , Bickelhaupt Friedrich
Published: August 2018

The title compound (2b) was obtained in 7 steps from 2-phenylbenzhydrol (5). The phenyl substituent of 2b confers thermal stability to the [5]phosphaphenanthrene system by steric protection; in addition, conjugative interaction is revealed by the UV spectrum. The analogy to the corresponding arenes is briefly discussed.
Synthesis and Structure of YbIrIn5
Authors: Zaremba Vasyl’ I. , Rodewald Ute Ch. , Pöttgen Rainer
Published: August 2018

The new ternary indium-rich compound YbIrIn5 was synthesized from the elements via an indium flux technique. A mixture with the starting composition 1:1:7 was heated at 1300 K in a tantalum tube for 6 h and cooled to room temperature at a rate of 5 K/h. The structure was refined from X-ray single crystal diffractometer data: HoCoGa5 type, P4/mmm, a = 461.96(7), c = 740.21(15) pm, wR2 = 0.0616, 222 F2 values, and 12 variable parameters. The iridium atoms have eight indium neighbors in square prismatic coordination at Ir-In distances of 274 pm. The square prisms are condensed via common edges forming layers which are separated by the ytterbium and further indium atoms. Ytterbium has a cuboctahedral indium coordination. The cell volume is suggestive for divalent or intermediate-valent ytterbium.
Crystal Structure and Optical Properties of 4-[4-(Dimethylamino)- styryl]-1-methyl-pyridinium Lead Tribromide
Authors: Papavassiliou George C. , Mousdis George A. , Terzis Aris , Raptopoulou Caterina P.
Published: August 2018

The title compound crystallizes in the centrosymmetric space group I2/a. When pumped by 458 and 1064 nm laser radiation the compound gives rise to a broad luminescence band at ca. 668 and 671 nm, respectively.
Note: Synthesis of the Dinuclear Halogeno-Bridged Complexes [Re2(μ-X)2(CO)6(CH3CN)2], (X = Cl, Br)
Authors: Carballo Rosa , García-Martínez Emilia , Pereiras-Gabián Gumersindo , Vázquez-López Ezequiel M.
Published: August 2018

Complexes [Re2(μ-X)2(CO)6(NCCH3)2] (X = Cl, Br) have been easily prepared in high yield by refluxing of fac- [ReX(CO)3(NCCH3)2] in toluene. The crystal and molecular structure of the bromine derivative have been determined by X-ray analysis. The molecule consists of two fac-Re(CO)3 fragments bridged by two bromine atoms. The acetonitrile molecules reside above and below the Re2Br2 plane.