bluuebunny/crossref_metadata_2025_split huggingface dataset:
Konformation und Vernetzung von (CuCN)6‐Ringen in polymeren Cyanocupraten(I) [Cu2(CN)3—] (n= 2, 3)
Authors: Pretsch Thorsten , Brüdgam Irene , Hartl Hans 
Published: February 2004

AbstractDie Alkalimetall‐tricyano‐dicuprate(I) Rb[Cu2(CN)3] · H2O (1) und Cs[Cu2(CN)3] · H2O (2) wurden hydrothermal aus CuCN und RbCN bzw. CsCN, die Dialkylammonium‐tricyano‐dicuprate(I) [NH2(Me)2][Cu2(CN)3] (3), [NH2(iPr)2][Cu2(CN)3] (4), [NH2(Pr)2][Cu2(CN)3] (5) und [NH2(sekBu)2][Cu2(CN)3] (6) durch Umsetzungen von Dimethylamin, Diisopropylamin, Dipropylamin bzw. Di‐sek‐butylamin mit CuCN und NaCN in Gegenwart von Ameisensäure erhalten. Die Kristallstrukturen dieser sechs Verbindungen enthalten (CuCN)6‐Ringe unterschiedlicher Konformation, die in Abhängigkeit von der Größe und Form der beteiligten Kationen zu Schichten (1) oder dreidimensionalen, teilweise zeolithartigen Netzwerken (2bis6) verbunden sind. Kristalldaten s. Abstract.
Complexes of 2, 6‐Bis(hydroxymethyl)pyridine with Different Copper(II) Salts Involving the Anions Chloride, Perchlorate, Nitrate and Acetate. Synthesis and Crystal Structures of the Complexes
Authors: Winter S. , Seichter W. , Weber E. 
Published: February 2004

AbstractComplexes of 2, 6‐bis(hydroxymethyl)pyridine (dhmp) with different CuII salts [CuCl2·6H2O, Cu(ClO4)2·6H2O, Cu(NO3)2·3H2O, Cu(CH3COO)2·H2O] are prepared (1—5, respectively), studied by IR, and their crystal structures reported. Dependent on the anion kind, influences on the distortion of the co‐ordination polyhedron, the distribution of donor sites, the formation of a mono‐ or binuclear complex, and the resultant packing structure of the complex are observed, although in no case the counterions of the used CuII salts or water of hydration were found in the co‐ordination sphere. Crystal structures of 1—5 indicate hexaco‐ordination of the CuII ions with N2O4‐environment and show that 1—4 are mononuclear 2:1 (L:M) complexes, but 5 is a binuclear 4:2 complex. Crystallization of Cu(ClO4)2·6H2O with dhmp yielded two different complexes (2/3). In 3, one of the dhmp components is mono‐deprotonated and acts as an anionic ligand. The same behavior is found in 5. Whereas in the neutral ligand complexes 1, 2 and 4 the basal planes are occupied by O donors, and N atoms are in the axial positions of the octahedrons, in 3 and 5 the bases are formed by two O and two N donor atoms, and O atoms are in the axes. Moreover, complex 3 shows the N atoms in trans position, but 5 in cis position. The packing of the cationic complex units is typical of strong and weak H bond interactions involving the counterions and hydroxylic or aromatic hydrogen atoms to yield complex network structures.
Alkali Metal Di‐tert‐butylphenylsilanides — tBu2PhSiM (M = Li, Na, K) — Syntheses, Structures, and Reactivity
Authors: Lerner H.‐W. , Scholz S. , Bolte M. , Wagner M. 
Published: February 2004

AbstractThe alkali metal silanides tBu2PhSiM (M = Li, Na, K) are quantitatively accessible from the reaction of tBu2PhSiBr with alkali metals in heptane, tetrahydrofuran, and benzene at moderately elevated temperature. In contrast to the polymer structure of unsolvated tBu2PhSiNa, the solvated di‐tert‐butylphenylsilanides tBu2PhSiNa(THF), tBu2PhSiK(C6H6), tBu2PhSiK(THF), and tBu2PhSiK(THF)2 possess a novel feature in their crystal structures with a dimeric arrangement of tBu2PhSiM units via π interaction between the tBu2PhSi group and the alkali metal centers. The alkali metal siloxides tBu2PhSiOM (M = Li, Na, K) can be synthesized almost quantitatively from tBu2PhSiM (M = Li, Na, K) with N2O in tetrahydrofuran at —78 °C. Single crystals of the silanol tBu2PhSiOH have been obtained from the protolysis of tBu2PhSiONa with (NH4)2SO4.
Phosphanimin‐ und Phosphaniminato‐Komplexe von Beryllium. Kristallstrukturen von [BeCl2(HNPPh3)2], [BeCl(HNPPh3)2(Py)]Cl und [Be3Cl2(NPPh3)4]
Authors: Neumüller Bernhard , Dehnicke Kurt 
Published: February 2004

AbstractTetraphenylphosphonium‐hexachlorodiberyllat, (Ph4P)2[Be2Cl6], reagiert mit Lithiumphosphaniminat, [LiNPPh3]6, in Dichlormethan unter Bildung des dreikernigen Berylliumphosphaniminats [Be3Cl2(NPPh3)4] (3). Als Nebenprodukt erhält man den Phosphaniminkomplex [BeCl2(HNPPh3)2] (1), der mit Pyridin in den ionischen Komplex [BeCl(HNPPh3)2(Py)]Cl (2) umgewandelt wird. Dagegen reagiert das silylierte Phosphanimin Me3SiNP(p‐Tolyl)3 (5) weder mit BeCl2 noch mit (Ph4P)2[Be2Cl6] unter Bildung von Phosphaniminaten des Berylliums. Aus CH2Cl2‐Lösung läßt sich lediglich das Aminophosphoniumsalz [(C7H7)3PNH2]Cl (4) isolieren. Die Verbindungen 1‐5 werden durch Kristallstrukturanalysen und durch IR‐Spektroskopie charakterisiert.1·C7H8: Raumgruppe C2/c, Z = 4, Gitterkonstanten bei 193 K: a = 1408, 9(2); b = 1750, 9(2); c = 1633, 2(2) pm; β = 106, 50(1)°; R1 = 0, 0385. Die Molekülstruktur von 1 weist kurze Be—N‐Abstände von 169, 8(3) pm auf.2·Py: Raumgruppe P1¯, Z = 4, Gitterkonstanten bei 193 K: a = 969, 5(1); b = 2077, 1(2); c = 2266, 4(2) pm; α = 72, 24(1)°; β = 87, 16(1)°; γ = 77, 42(2)°; R1 = 0, 0776. 2 hat die Struktur eines Ionenpaars, in dem die NH‐Atome der Phosphanimin‐Liganden Wasserstoffbrückenbindungen mit dem Chloridion ausbilden. Die HNPPh3‐Moleküle realisieren kurze Be—N‐Bindungen von 169, 0(6) pm, der Be—N‐Abstand des Pyridinliganden beträgt 182, 5(6) pm.3·3CH2Cl2: Raumgruppe P1¯, Z = 2, Gitterkonstanten bei 193 K: a = 1333, 2(2); b = 1370, 2(2); c = 2151, 8(3) pm; α = 107, 14(1)°; β = 91, 39(1)°; γ = 105, 15(1)°; R1 = 0, 0917. Die Struktur des dreikernigen Moleküls 3 entspricht der eines Be2+‐Ions, das durch die N‐Atome zweier Chelatliganden {ClBe(NPPh3)2}— tetraedrisch koordiniert ist.4·CH2Cl2: Raumgruppe P21/c, Z = 4, Gitterkonstanten bei 193 K: a = 1206, 6(2); b = 1798, 0(2); c = 1096, 2(1) pm; β = 97, 65(1)°; R1 = 0, 0535. 4 bildet dimere Einheiten, in denen die NH2‐Gruppen der [(C7H7)3PNH2]+‐Kationen mit den Chloridionen zentrosymmetrische Achtringe bilden.5: Raumgruppe P21/n, Z = 4, Gitterkonstanten bei 193 K: a = 1074, 3(2); b = 2132, 2(3); c = 1075, 5(2) pm; β = 110, 68(1)°; R1 = 0, 0664. 5 bildet Moleküle mit Abständen PN von 154, 6(3), SiN von 168, 8(3) pm und einem SiNP‐Winkel von 134, 4(2)°.
Festkörper‐NMR‐Untersuchungen an Natriumoxothiophosphaten(V)
Authors: Pompetzki M. , van Wüllen L. , Jansen M. 
Published: February 2004

AbstractNatriummonothiophosphat(V) Na3PO3S ist dimorph. Die metastabile Hochtemperaturmodifikation β‐Na3PO3S kristallisiert hexagonal mit den Gitterkonstanten a = 8, 996(4) und c = 5, 216(2)Å. 31P‐Festkörper‐NMR‐Experimenten zufolge weist α‐Na3PO3S bei 20 °C im Gegensatz zu den Ergebnissen der verfeinerten Kristallstruktur eine nichtaxialsymmetrische Umgebung für die Phosphorkerne auf. Diese Diskrepanz wird unter der Annahme geordneter und fehlgeordneter Strukturmodelle diskutiert. Bei 490 °C hingegen ist der Tensor der chemischen Verschiebung für die Phosphorkerne in α‐Na3PO3S axialsymmetrisch. Offenbar wird die Verzerrung der Phosphorumgebung durch die thermische Bewegung der Atome aufgehoben. Die Anzahl kristallographischer Lagen für Natrium und Phosphor in Na3PO2S2 und Na3POS3 läßt sich anhand von Festkörper‐NMR‐Spektren in exakter Übereinstimmung mit ihren Kristallstrukturen bestimmen.
Structural Isomers of Bis(diphenylarsino)methane‐dichloroplatinum(II)
Authors: Babai Arash , Deacon Glen B. , Meyer Gerd 
Published: February 2004

AbstractFrom a range of preparative methods, three geometric isomers of bis(diphenylarsino)methane‐dichloroplatinum(II) have been isolated, viz. cis‐PtCl2(dpam), trans, trans‐Pt2Cl4(dpam)2 and cis, trans‐Pt2Cl4(dpam)2. Their structures were determined by single‐crystal X‐ray diffraction.
Syntheses, Characterization and X‐Ray Structures of the first Copper(I) and Silver(I) Complexes with ATT (ATT = 6‐Aza‐2‐thiothymine)
Authors: Ghassemzadeh Mitra , Pooramini Mostafa Mohammad , Tabatabaee Maasoomeh , Heravid Majid M. , Neumüller Bernhard 
Published: February 2004

AbstractThe reaction of copper(I) chloride with 6‐aza‐2‐thiothymine (ATT, 1) and triphenylphosphane in methanol/chloroform gives [(ATT)CuCl(PPh3)] (2) as a neutral complex. [(ATT)Ag(NO3)(PPh3)2]·MeOH (3) can be obtained by the reaction of 1 with silver(I) nitrate and triphenylphosphane in methanol/chloroform in excellent yields and the single crystals of 3 can be obtained from acetonitril solution.Both complexes were characterized by infrared spectroscopy, elemental analyses as well as by X‐ray diffraction studies. Crystal data for 2 at —80 °C: space group I2/a with a = 1859.3(1), b = 1143.2(1), c = 2208.2(1) pm, β = 104.84(1)°, Z = 8, R1 = 0.0355 and for 3 at —80 °C: space group P21/c with a = 1344.1(1), b = 1553.6(1), c = 1977, 3(3) pm, β = 105.26(1)°, Z = 4, R1 = 0.0436.
Reactions of Ru3(CO)12 with Diphosphenes — A New Route to 50‐Electron Ru3P2nido‐Clusters
Authors: Freytag Matthias , Edelmann Frank T. , Ernst Ludger , Jones Peter G. , Schmutzler Reinhard 
Published: February 2004

AbstractThe reaction of the symmetric diphosphene 2, 4, 6‐(CF3)3‐C6H2‐P=P‐C6H2‐2, 4, 6‐(CF3)3 4 with Ru3(CO)12 led to the 50‐electron Ru3P2 nido‐cluster Ru3(CO)9[μ‐P‐C6H2‐2, 4, 6‐(CF3)3]2 5, which in solution at room temperature displays hindered rotation of the aromatic rings about the C(aryl)—P bonds. The structure of 5 was determined by X‐ray crystal structure analysis; its Ru3P2 centre forms a distorted square pyramid with one ruthenium atom at the apex. One of the two C6H2(CF3)3 groups is also appreciably distorted. Temperature‐dependent 19F NMR studies of the [A3M3X]2 spin system (A = M = CF3, X = 31P) of 5 indicated a rotational barrier ΔG≠ of 82.3 kJ mol‐1 at 141 °C. The same Ru3P2 core was obtained by the reaction of the unsymmetric diphosphene Mes*‐P=P‐Mes 11 with Ru3(CO)12; hindered rotation about the C(aryl)—P bonds was also observed, in this case.
Synthesis, Spectral and Magnetic Properties, and Crystal Structures of Copper(II) Pyridinecarboxylate Adducts with N‐Heterocyclic Ligands
Authors: Segl'a Peter , Palicová Martina , Miklos Dusan , Koman Marian , Melník Milan , Korabik Maria , Mrozinski Jerzy , Glowiak Tadeusz , Sundberg Markku R. , Lönnecke Peter 
Published: February 2004

AbstractSynthesis and characterization of seven new complexes [Cu(2‐MeSnic)2(CH3OH)]2 (where 2‐MeSnic is 2‐methylthionicotinate), [Cu(2‐MeSnic)2L2]2 (where L is pyridine — py, ethylnicotinate — Etnic and butylnicotinate — Bunic), [Cu(2‐MeSnic)2L2(H2O)2] (where L is py and nicotinamide — nia) and [Cu(2‐MeSnic)2(N‐Menia)2(H2O)2]·2H2O (where N‐Menia is N‐methylnicotinamide) are reported. The characterization were based on elemental analysis, infrared, electronic and EPR spectra, and magnetic susceptibility measurements over a temperature range of 1.8 — 300 K or 70 — 300 K. Three complexes of different type were studied by X‐ray analysis. The molecule of [Cu(2‐MeSnic)2(CH3OH)]2 has dimeric paddle‐wheel cage structure with a tetragonal pyramidal arrangement around CuII. The dimer results from the fact that carboxyl groups of four 2‐MeSnic anions function as bridging in a syn‐syn arrangement. On the other hand [Cu(2‐MeSnic)2(py)2]2 forms dimers with hexacoordinated CuII atoms in highly distorted coordination octahedra, each with two oxygen atoms of bridging carboxyl groups in an anti‐anti arrangement of two 2‐MeSnic anions, with two oxygen atoms of one asymmetrically chelating 2‐MeSnic anion and with two nitrogen atoms of two pyridine ligands. The temperature independent EPR spectrum for this complex exhibits an axial signal which corresponds to almost isolated S = 1/2 magnetic ions. Magnetic data for the dimer show a weak antiferromagnetic interaction between the two metal ions with J = —0.65 cm—1. The CuII atom in complex [Cu(2‐MeSnic)2(py)2(H2O)2] is hexacoordinated in an elongated centrosymmetrical tetragonal‐bipyramidal arrangement (4 + 2). Based on the molecular structure the electronic, infrared, electron paramagnetic resonance spectra and magnetic properties are discussed and stereochemistry as well as the mode of ligand coordination in new solid complexes under study have been determined.
Vibrational Spectra and Magnetic Properties of Eu3[BN2]2 and LiEu4[BN2]3
Authors: Somer Mehmet , Gül Cem , Müllmann Ralf , Mosel Bernd D. , Kremer Reinhard K. , Pöttgen Rainer 
Published: February 2004

AbstractEu3[BN2]2 and LiEu4[BN2]3 were synthesized from a stoichiometric mixture of EuN, BN, europium metal and Li3N, EuN and BN (ratio: 1:4:3) in sealed niobium ampoules at 1475 and 1275 K, respectively. Temperature dependent susceptibility measurements of Eu3[BN2]2 and LiEu4[BN2]3 show Curie‐Weiss behavior with experimental magnetic moments of 8.03(5) and 8.5(1) μB/Eu atom, respectively, compatible with divalent europium. Both nitridoborates order ferromagnetically at TC = 32.0(5) K (Eu3[BN2]2) and 22.0(5) K (LiEu4[BN2]3). The saturation magnetizations of 5.73(5) μB/Eu atom at 5 K and 7 T for Eu3[BN2]2 and 4.2 μB/Eu atom at 5 K and 2 T for LiEu4(BN2)3 are smaller than the maximum value of 7 μB. 151Eu Mössbauer data of Eu3[BN2]2 at 4.2 K show an isomer shift of —11.4(1) mm/s and an experimental line width of 3.1(2) mm/s. Full magnetic hyperfine field splitting with 26.2(3) T at the europium nuclei is detected. Vibrational spectra of Eu3[BN2]2 are interpreted on the basis of discrete [BN2]3— units with symmetry D∞h by taking into account the existence of two crystallographically independent [BN2]3— anions and their dynamic coupling in the unit cell (factor group splitting).
Dithiolylium‐Chlorooxomolybdate(V): Synthese und Kristallstruktur von (C3Cl3S2)[MoOCl4] und (C3Cl3S2)[Mo2O2Cl7]
Authors: Beck Johannes , Koch M. 
Published: February 2004

AbstractDurch Umsetzung von 3, 4, 5‐Trichlor‐1, 2‐dithiolyliumchlorid mit MoOCl3 in Dichlormethan unter solvothermalen Bedingungen bei 65 °C entstehen nebeneinander das grüne Tetrachlorooxomolybdat(V) (C3Cl3S2)[MoOCl4] und das braun‐gelbe Heptachlorodioxodimolybdat(V) (C3Cl3S2)[Mo2O2Cl7]. Die Kristallstrukturen beider Substanzen enthalten annähernd planare (C3Cl3S2)+‐Ionen mit einer S—S‐Bindungslänge von 203 pm. Das diskrete [MoOCl4]—‐Ion in der Struktur von (C3Cl3S2)[MoOCl4] hat die Form einer quadratischen Pyramide mit einer Grundfläche aus Chloratomen, aus der das zentrale Molybdänatom um 58 pm in Richtung des Sauerstoffatoms auf der Pyramidenspitze herausgerückt ist. Das [Mo2O2Cl7]—‐Ion in der Struktur von (C3Cl3S2)[Mo2O2Cl7] hat die Form eines flächenverknüpften Oktaederdoppels. Es besteht formal aus einem [MoOCl4]—‐Ion und einem MoOCl3‐Molekül, die durch eine symmetrische und zwei asymmetrische Chlorobrücken verknüpft sind. Die Molybdänatome in den so verknüpften Oktaedern bilden bei einem Abstand von 357 pm keine Bindung aus.
The Stereochemical Activity of the Lone Pair in [Bi(NO3)3{(iPrO)2(O)PCH2P(O)(OiPr)2}2] — Comparison of Bismuth, Lanthanum and Praseodymium Nitrate Complexes
Authors: Mehring Michael , Mansfeld Dirk , Schürmann Markus 
Published: February 2004

AbstractFive coordination compounds of bismuth, lanthanum and praseodymium nitrate with the oxygen‐coordinating chelate ligand (iPrO)2(O)PCH2P(O)(OiPr)2 (L) are reported: [Bi(NO3)3(L)2] (1), [La(NO3)3(L)2] (2), [Pr(NO3)3(L)2] (3), [La(NO3)3(L)(H2O)] (4) and [Pr(NO3)3(L)(H2O)] (5). The compounds were characterized by means of single crystal X‐ray crystallography, 1H and 31P NMR spectroscopy in solution, solid‐state 31P NMR spectroscopy, IR spectroscopy, DTA‐TG measurements (1, 2 and 4), conductometry and electrospray ionization mass spectrometry (ESI‐MS). In addition, DFT calculations for model compounds of 1 and 2 support our experimental work. In the solid state mononuclear coordination compounds were observed for 1—3, whereas compounds 4 and 5 gave one‐dimensional hydrogen‐bonded polymers via water‐nitrate coordination. Despite of the similar ionic radii of bismuth(III), lanthanum(III) and praseodymium(III) for a given coordination number the bismuth and lanthanide compounds 1—3 are not isostructural. The bismuth compound 1 shows a 9‐coordinate bismuth atom whereas lanthanum(III) and praseodymium(III) atoms are 10‐coordinate in the lanthanide complexes 2—5. The general LnO10 coordination motif in compounds 2—5 is best described as a distorted bi‐capped square antiprism. The BiO9 polyhedron might be deduced from the LnO10 polyhedron by replacing one oxygen ligand with a stereochemically active lone pair. The one‐to‐one complexes 4 and 5 dissociate in solution to give the corresponding one‐to‐two complexes 2 and 3, respectively, and solvated Ln(NO3)3. In contrast to the lanthanides, the one‐to‐two bismuth complex 1 is less stable in CH3CN solution and partially dissociates to give solvated Bi(NO3)3 and (iPrO)2(O)PCH2P(O)(OiPr)2.
Aminotroponiminate and a Related Diimine as Ligands for Tungsten Complexes
Authors: Kirin Vladimir , Roesky Peter W. 
Published: February 2004

AbstractReaction of N‐isopropyl‐2‐(isopropylamino)troponimine, {(i‐Pr)2ATI}H, with fac‐[W(CO)3(NCMe)3] yield the complex tungsten‐tetracarbonyl‐N, N'‐diisopropyl‐1, 2‐diimino‐3, 5‐cycloheptadiene (1), in which the ligand is tautomerized from the enamino to the imino isomer. As a result of the rearrangement the conjugate 10 π electron system of the ligand is destroyed. Further, treatment of compound 1 with an excess of KH in THF leads to the ionic complex [K(THF)2][{(i‐Pr)2ATI}W(CO)4] (2). In the presence of diglyme the corresponding complex [K(diglyme)2][{(i‐Pr)2ATI}W(CO)4] (3) is obtained. All compounds have been characterized by spectroscopic methods. Complex 1 has also been investigated by single crystal X‐ray diffraction.
Synthesis and Structure of the Clusters [Hg2(μ—SePh)2(SePh)2(PPh3)2] and [Hg3Br3(μ—SePh)3] · 2 DMSO
Authors: Schulz Lang Ernesto , Müller Dias Marcelo , Santos dos Santos Sailer , Vázquez‐López Ezequiel M. , Abram Ulrich 
Published: February 2004

AbstractThe compounds [Hg2(μ—SePh)2(SePh)2(PPh3)2] (I) and [Hg3Br3(μ—SePh)3] · 2 DMSO (II) are formed by reactions of [Hg(SePh)2] with PPh3 in THF(I) or with HgBr2 in DMSO (II) at room temperature. X—ray crystallography reveals that the cluster I consists of a distorted square built by each two Hg and Se atoms. The Hg atoms have almost tetrahedral co‐ordination environments formed by selenium atoms of two (μ‐—SePh) ligands and Se and P atoms of terminal —SePh and PPh3 ligands. The compound II is a six‐membered ring with alternating Hg and Se atoms in the chair conformation. Two DMSO molecules occupy positions below and above the [Hg3Se3] ring with the oxygen atoms directed to the centre of the ring.
Stabilization of Discrete [Cu(C2O4)2(H2O)2]2— Dianions in the Solid State by an Extensive Hydrogen Bonded Network
Authors: Keene Tony D. , Hursthouse Michael B. , Price Daniel J. 
Published: February 2004

AbstractThe dominant species in aqueous copper(II) solutions containing a high concentration of oxalate (ox) is trans‐[Cu(ox)2(H2O)2]2—, yet the ability of the oxalate anion to bridge metal ions means that very few examples of this isolated anion are seen in solid state structures. The structure of [pipH2]2+[Cu(ox)2(H2O)2]2— · 2H2O (pip = piperazine) (1) comprises discrete ions held in a complex 3‐dimensional hydrogen bonded network.
Hydrothermal Synthesis of Rare Earth Iodates from the Corresponding Periodates: II1). Synthesis and Structures of Ln(IO3)3 (Ln = Pr, Nd, Sm, Eu, Gd, Tb, Ho, Er) and Ln(IO3)3 · 2H2O (Ln = Eu, Gd, Dy, Er, Tm, Yb)
Authors: Douglas Paul , Hector Andrew L. , Levason William , Light Mark E. , Matthews Melissa L. , Webster Michael 
Published: February 2004

AbstractSingle crystals of lanthanide iodates have been quickly grown by decomposition of the corresponding periodates under hydrothermal conditions. Single crystal X‐ray diffraction showed that two structure types form with the elements from Pr‐Yb, an anhydrous form for Pr, Nd, Sm, Eu, Gd, Tb, Ho, Er and a dihydrate for Eu, Gd, Dy, Er, Tm, Yb. A detailed structure study is presented for one representative of each of these types, along with structure type and lattice parameters for the other materials.Tb(IO3)3: Space group P21/c, Z = 4, lattice dimensions at 120 K: a = 7.102(1), b = 8.468(1), c = 13.355(2)Å, β = 99.67(1)°; R1 = 0.034.Yb(IO3)3 · 2H2O: Space group P1¯, Z = 2, lattice dimensions at 120 K: a = 7.013(1), b = 7.370(1), c = 10.458(2)Å, α = 95.250(5), β = 105.096(5), γ = 109.910(10)°; R1 = 0.024.
The System LiSO3CF3/RbSO3CF3: Phase Diagram, Solid State NMR Investigations, and Ionic Conductivity
Authors: Pompetzki M. , van Wüllen L. , Jansen M. 
Published: February 2004

AbstractIn the system LiSO3CF3/RbSO3CF3 four different quasi‐ternary phases occur: Li0.7Rb0.3SO3CF3, Li0.55Rb0.45SO3CF3, LiRb2(SO3CF3)3, and Li0.2Rb0.8SO3CF3. These have been identified, and characterized by means of X‐ray powder diffractometry and DSC. LiSO3CF3 is trimorphic, LiRb2(SO3CF3)3 is dimorphic and RbSO3CF3 exists in four different modifications. The cation dynamics has been studied using 7Li‐NMR line shape analysis and 7Li‐spin lattice relaxation (T1) measurements. The pure and mixed trifluoromethylsulfonates in the system LiSO3CF3/RbSO3CF3 are solid electrolytes. Their ionic conductivities below 475 K increase with the rubidium content. Above this temperature, the conductivity of β‐LiRb2(SO3CF3)3 exceeds the one of δ‐RbSO3CF3.
Novel Layered Structures Formed by Iodocuprate Clusters Stabilized by Dialkylsulphide Ligands
Authors: Paulsson Heléne , Berggrund Malin , Fischer Andreas , Kloo Lars 
Published: February 2004

AbstractFrom solutions of copper iodide and dodecyldimethylsulphonium iodide in acetonitrile, single crystals of [Cu4I4(DodecylMeS)4] (1) and [Cu3I4(DodecylMeS)3](DodecylMe2S) (2) could be obtained. Both compounds crystallize in the triclinic crystal system, space group P1¯ (1: a = 957.23(1), b = 967.25(2), c = 3818.38(6) pm, α = 90.3837(6)°, β = 86.4687(7)°, γ = 75.0996(7)°, 2: a = 874.23(1), b = 979.29(1), c = 4388.75(4) pm, α = 90.4472(3)°, ß = 94.7088(3)°, γ = 116.1162(3)°). 1 consists of tetrahedral Cu4 clusters, which are capped by four iodide ions over the tetrahedral faces. 2 contains trigonal Cu3 clusters, which are coordinated by four iodide ions, one centered over the plane, three bridging over the edges of the Cu3 triangle. In both compounds, the S atoms of (DodecylMeS) ligands coordinate to the Cu atoms. In 2, a (DodecylMe2S) cation is also present.
[PbAsSiiPr3]6 — the First Structurally Characterized Compound with Chemical Bonds between Lead and Arsenic
Authors: von Hänisch Carsten , Nikolova Donna 
Published: February 2004

AbstractThe compound [PbAsSiiPr3]6 (1) could be obtained by the reaction of PbCl2 with iPr3SiAs(SiMe3)2 in THF at 0 °C. Central structural motif is a hexagonal prism built by six lead and six arsenic atoms. The average Pb—As bond length is 281 pm. The cluster crystallizes in the monoclinic space group C2/c, the lattice constants are: a = 4460.8(9) b = 2296.6(5), c = 2734.4(6) pm, β = 117.57(3)°. The thermogravimetric analysis in vacuum shows the tendecy of 1 to decompose under formation of elementary lead and volatile arsenic compounds.
Ein Metaarsenat(V) Anion neuartiger Konstitution in AgAsO3
Authors: Curda J. , Peters E.‐M. , Jansen M. 
Published: February 2004

AbstractAgAsO3 wurde durch Festkörperreaktion zwischen Ag2O und As2O3 oder As unter erhöhtem Sauerstoffdruck erstmals dargestellt (T = 500 °C, p(O2) = 2 kbar, 1—2 Tage). Nach den Ergebnissen der Einkristallröntgenstrukturanalyse (Pca21; a = 1948.8(3), b = 660.0(1), c = 1266.1(3) pm; Z = 24; 4741 unabh. Reflexe; R1 = 0.044) liegt gemäß [(AsO6/2)(AsO2/1O2/2)2] ein neuartiges Polyanion vor, das Arsen nebeneinander in oktaedrischer und tetraedrischer Koordination enthält. Es weist damit Struktureinheiten wie As2O5 auf, die darüber hinaus in ähnlicher Weise verknüpft sind.