| 1 | Author
| Dirk Niepmann3, Rainer Pöttgen3, KristinM. Poduskab, FrancisJ. Disalvob, Henning Trillc, BerndD. Moselc | Requires cookie* | | Title
| Structure and Properties of the Stannides CeAuSn, Ce3Rh4Sn13, and Ce3Ir4Sn13  | | | Abstract
| Intermetallic Compounds, Cerium, M össbauer Spectra CeAuSn, Ce.^RluSnn, and Ce3lr4Sni3 were prepared by reaction of the elements in an arc-melting furnace and subsequent annealing at 970 K for two weeks. The three stannides were investigated by X-ray powder and single crystal techniques. CeAuSn crystallizes with the NdPtSb type, space group P6?,mc: a = 472.7(2), c = 771.6(3) pm, xvR2 = 0.0230,208 F 2 values, 11 variable parameters, and BASF = 0.40(2). The gold and tin atoms form a pronounced two-dimensional [AuSn] polyanion which consists of slightly puckered Au3Sn3 hexagons. ,19Sn Mössbauer data at 78 K show one signal at an isomer shift of 6 = 1.90(7) mm/s subjected to unresolved quadrupole splitting of zAEq = 0.55(2) mm/s. Ce3Rh4Sni3 and Ce3lr4Sni3 adopt the cubic Yb3Rh4Sni3 type structure, space group Pm3n: a = 970.51(3) pm, wR2 = 0.0721, 267 F 2 values (Ce3Rh4Sni3) and a = 972.29(6) pm, wR2 = 0.0850, 267 F 2 values (Ce3lr4Sni3) with 14 variable parameters for each refinement. Striking structural motifs in C eiR luSnis are condensed distorted trigonal [RhSnö] prisms with Rh-Sn distances of 266 pm. The polyhe dral network leaves two different cages which are occupied by cerium (6c position) and tin (2a position) atoms. The Sn2 atoms show occupancy parameters of only 92% (C esR luSnn) and 76% (Ce3lr4Sni3) and an extremely large displacement parameter indicating a rattling of these atoms within the icosahedral S n ^ cages. Magnetic susceptibility measurements of Ce3Rh4 Sni3 show paramagnetic behavior down to 2 K with an experimental magnetic moment of 2.45(2) /iß/Ce. No magnetic ordering is observed. Magnetization measurements show a moment of 0.78(2) ^ß/C e at 2 K and 5.5 T. Resistivity data reveal only a very weak tem perature dependence. The two crystallographically different tin sites are resolved in the ll9Sn Mössbauer spectrum which shows a signal at S = 2.12(1) mm/s subject to quadrupole splitting of 1.54(1) mm/s, superimposed by a singlet at 6 = 2.47(1) mm/s. The Seebeck coefficient of Ce^RluSnn is within a few ß V /K of zero over the temperature range of 10 -300 K. | | |
Reference
| (Z. Naturforsch. 56b, 1—8 [2001]; received November 3 2000) | | |
Published
| 2001 | | |
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| default:Reihe_B/56/ZNB-2001-56b-0001.pdf | | | Identifier
| ZNB-2001-56b-0001 | | | Volume
| 56 | |
4 | Author
| Gabriele Wagner3, Rudolf Herrmann3, Bj0m Pedersenb, Wolfgang Schererb, PaulJ. Scheuer | Requires cookie* | | Title
| Synthesis and Structure of Chiral Silatranes Derived from Terpenes  | | | Abstract
| Starting with the chiral pool compounds (—)-menthone, (—)-limonene, (—)-/3-pinene, and (—)-carvone, new homochiral triethanolamine derivatives were obtained and converted to chi ral silatranes. These silatranes were characterized by crystal structure analyses and NMR techniques. Conformational analyses in the solid terpene residues determine the direction of the ring | | |
Reference
| (Z. Naturforsch. 56b, 25—38 [2001]; received August 8 2000) | | |
Published
| 2001 | | |
Keywords
| Silatranes, Terpenes, Chiral Pool | | |
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| default:Reihe_B/56/ZNB-2001-56b-0025.pdf | | | Identifier
| ZNB-2001-56b-0025 | | | Volume
| 56 | |
6 | Author
| E. Kavlakoglu3, A. Eimali3, Y. Elerman3, R. Werner6, H. Svobodac, Fuessc | Requires cookie* | | Title
| Crystal Structure and Magnetic Properties of a Linear Trinuclear Ni(II) Complex  | | | Abstract
| Linear Trinuclear Nickel(II) Complex, Super-Exchange Interactions, Antiferromagnetic Coupling [Ni3(C2H 3 0 2)2(CH3 0 H)2L2] [L = l,3-bis(5-chlorosalicylideneamino)propan-2-ol dianion, (C2H3 0 2)_ = acetate, (CH3OH) = methanol] was synthesized and its crystal structure was determined. It crystallizes in the monoclinic spaceeroup P2i /n with a = 12.694(2), b = 13.281 (4), c = 15.420(3) Ä, ß = 111.25(2)°, V = 2422.9(9) A ? ,Z = 2 . The molecule is a "linear" trinuclear complex with nearly octahedral coordination of each nickel ion. Adjacent nickel(II) ions are bridged by the phenolic oxygen atoms of the ligands and the oxygen atoms of the acetato ligands. The coordination sphere of the terminal nickel(II) ions is completed by the oxygen atom of the methanol. Adjacent nickel(II) centers are separated by 3.043(1) A and weakly antiferromagnetically coupled (J\ = -3 .4 cm -1). The terminal nickel(II) centers are separated by 6.086(1) A and very weakly antiferromagnetically coupled (J2 = -0 .3 cm -1) which follows from temperature-dependent magnetic susceptibility measurements in the temperature range 4.5 to 318 K. The magnetic moment rises from 2.99 hb at 4.5 K to 5.42 /iß at 318 K. In the X(T) curve no characteristic maximum was observed. | | |
Reference
| (Z. Naturforsch. 56b, 43—48 [2001]; received July 4 2000) | | |
Published
| 2001 | | |
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| default:Reihe_B/56/ZNB-2001-56b-0043.pdf | | | Identifier
| ZNB-2001-56b-0043 | | | Volume
| 56 | |
7 | Author
| JenniferA. Aitken, MercouriG. Kanatzidis | Requires cookie* | | Title
| New Information on the Na-Ti-Se Ternary System  | | | Abstract
| Molten Salt Fluxes, Polychalcogenide, Polyselenide Na2Ti2Se9 was first discovered in the quaternary system Na/Ti/P/Se, but it can be prepared rationally by dissolving Ti in a Na2Se.v flux at 375 °C. The silverish dark red crystals are air-and water-stable. A new method for synthesizing Na4TiSe4 is also reported. Na2Ti2Seg crystallizes in space group P2, with a = 12.785(4), b = 14.848(4), c = 13.961(4) A, ß = 94.556(4)°, R 1 = 0.0592 and wR2 = 0.1336. The structure is similar to that of KsNaTi6Se27. It contains infinite one dimensional chains which run parallel to the c-axis and contain Ti + centers bonded to Se22~ and Se2-species. The l/oo[Ti2(Se2)4Se]2~ chains pack together in a hexagonal pattern. All of the titanium atoms are surrounded by a pentagonal bipyramid of selenium atoms. The selenium atoms bridge the Ti centers in two different ways. Na2Ti2Seg is a semiconductor with a band gap, Eg, of ~ 1.02 eV. The Raman spectra are also reported. | | |
Reference
| (Z. Naturforsch. 56b, 49—56 [2001]; received August 22 2000) | | |
Published
| 2001 | | |
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| default:Reihe_B/56/ZNB-2001-56b-0049.pdf | | | Identifier
| ZNB-2001-56b-0049 | | | Volume
| 56 | |
8 | Author
| G. C. Papavassiliou, G. A. Mousdis, I. B. Koutselas | Requires cookie* | | Title
| Some Organic-Inorganic Hybrid Compounds Based on «ö-Thiuronium Cations and Lead Halide Anions  | | | Abstract
| Using 1-chlorodecane (C10H21CI), benzyl chloride (C6H5CH2CI), a,a'-dichloro-p-xylene (CICH2C6H4CH2CI), 4-phenylbenzyl chloride (C6H5C6H4CH2CI), 2-bromomethyl-naphthal-ene (CioHyC^Br), 4-bromomethyl-7-methoxycoumarin (CioHzO^C^Br), 2-bromomethyl-anthraquinone (CuH TC ^C ^Br), 9-chloromethyl-anthracene (C14H9CH2CI), thiourea and halides as starting materials, the organic-inorganic hybrid compounds [CioH2iSC(NH2)2]2Pbl4, [C6H5CH2SC(NH2)2]4Pb3l,o, [(H sN h C S C ^ C ö H tC ^ S Q N H jh k sP b ls, [C6H5C6H4CH2S-C(NH2)2]PbI3, [C,oH7CH2SC(NH2)2]Pbl3, [CioH yChC^SQNHzhlPbL, [C^HyOjCHzSC-(NH2)2]PbI3, [C,4H9CH2SC(NH2)2]Pbl3, and [C M H gO ^SQ N H z^hPbB ^ were prepared and characterized analytically and spectroscopically. | | |
Reference
| (Z. Naturforsch. 56b, 57—61 [2001]; received September 11 2000) | | |
Published
| 2001 | | |
Keywords
| Organic-Inorganic Hybrids, Low-Dimensional Semiconductors, Fluorescence | | |
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| default:Reihe_B/56/ZNB-2001-56b-0057.pdf | | | Identifier
| ZNB-2001-56b-0057 | | | Volume
| 56 | |
11 | Author
| ProfW. Sonderdruckanforderungen, Siebert, Herrn, Prof, M. Dr | Requires cookie* | | Title
| Synthese und Struktur von benzylsubstituierten Derivaten des Dinickel-Tripeldeckerkomplexes //-J75,i75-(2,3-Dihydro-l,3-diborolyl)  | | | Abstract
| -(i/3-aIlyI)(7/4-l,5-hexadien)dinickel Synthesis and S tructure o f B enzyl S ubstituted D erivatives of the D inickel T riple-D ecker C om plex ,w-?75,?75-(2 ,3 -D ih y d ro -l,3 -diborolyl)-(?73-allyl)(774-l ,5 -hexadiene)dinickel W alter Siebert, Stefan H uck und H an s Pritzkow Nickel, //-775,?75-(2 ,3-Dihydro-l,3-diborolyl)(?73-allyl)(?74-l,5-hexadiene)dinickel, Polydecker Complexes Hydroboration of phenyl-and mesitylethyne with in situ formed HBC12 leads to an isome ric mixture of l,l-bis(dichloroboryl)-2-phenylethane (4a) and l,l-bis(dichloroboryl)-l-pheny-lethane (4b) (ratio 3 : 1) and regioselectively to l,l-bis(dichloroboryl)-2-mesitylethane (4c). Treatment of 4a/b and 4c with BI3 gives the corresponding tetraiodo compounds 5, which undergo redox reactions with butyne-2 to form the l,3-diiodo-4,5-dimethyl-2,3-dihydro-l,3-diborole derivatives 6a/b and 6c. Reactions of the diiodo-l,3-diboroles with AlMe3 or LiMe result in the formation of the very air-sensitive pentaorganyl-l,3-diboroles la, lc and the hexaorganyl-l,3-diborole lb. The mixture of la/b as well as lc react with bis(?/3-allyl)nickel to give black products, which are chromatographed on silica with hexane as eluent. The brown solids were recrystallized from pentane to give the light-brown crystals of i M-j/5,7;5-[2-benzyl-l,3 ,4 ,5 -tetramethyl-2 ,3-dihydro-l,3-diborolyl](/73-allyl)(»74-l,5-hexadiene)dinickel (2a, 34%) and //-?/5,»75-[2-(2 ,4 ,6-trimethyl-benzyl)-l,3 ,4 ,5-tetramethyl-2,3-dihydro-l,3-diborolyl](?73-allyl)(?74-l,5-hexadiene)dinickel (2c, 43%). lb does not react with Ni(C3H5)2 to form any triple-decker. The compositions of the new compounds follow from spectroscopic and analytical data, and from X-ray structure analyses of 6a and of 2a. The structure of the ?74-l,5-hexadiene-?73-allyl-dinickel triple-decker 2a finally disproved the alternative tris(allyl)dinickel arrangement. | | |
Reference
| (Z. Naturforsch. 56b, 73—78 [2001]; eingegangen am 4. September 2000) | | |
Published
| 2001 | | |
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| default:Reihe_B/56/ZNB-2001-56b-0073.pdf | | | Identifier
| ZNB-2001-56b-0073 | | | Volume
| 56 | |
12 | Author
| M. Ichael Schur, C. Hristian, N. Äther, W. Olfgang, B. Ensch | Requires cookie* | | Title
| Synthesis and Crystal Structure of Mn2(C2H5NH2)2Sb2S5 Exhibiting a Reversible Phase Transition  | | | Abstract
| Thioantimonates, Solvothermal Synthesis, Chalcogenides The reaction of elemental manganese, antimony and sulfur with ethylamine under mild solvothermal conditions yielded a thioantimonate(III) with composition Mn2(EA)2Sb2S5 (EA = C2H5NH2) that is a new member of a series of polymeric manganese thioantimo-nates(III). The structure of the title compound consists of layers of a neutral mesh-like Mn2Sb2S5 framework. The ethylamino ligands coordinated to the Mn centres separate the sheets and fill the voids within the layers formed by the interconnection of Mn2Sb2S4 hetero-cubane like building blocks. Below 273 K a reversible phase transition occurs, which is accom panied by a doubling of the crystallographic a-axis. | | |
Reference
| (Z. Naturforsch. 56b, 79—84 [2001]; received September 14 2000) | | |
Published
| 2001 | | |
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| default:Reihe_B/56/ZNB-2001-56b-0079.pdf | | | Identifier
| ZNB-2001-56b-0079 | | | Volume
| 56 | |
15 | Author
| M. =. Cr, Mo, W., Norbert Kuhn, Martin Göhner, Manfred Steimann | Requires cookie* | | Title
| Über Komplexe des Typs {(PhC=C)3P}3M(CO)3 (M = Cr, Mo, W) On Complexes of the Type {(PhC=C)3P}3M(CO)3 (  | | | Abstract
| The tris(alkinyl)phosphine complexes {(PhC=C)3P}3M(CO)3, M = Cr (3a), Mo (3b), W (3c), are obtained from P(C=CPh)3 and (C6H 15N3)M(CO)3 (C6H 15N3 = 1,3,5-trimethyl-1,3,5-triazacyclohexane) as stable yellow solids in good yields. While IR data indicate significant acceptor properties of the phosphane ligands, the X-ray structure analysis of 3c also allows the discussion of weak donor interactions. | | |
Reference
| (Z. Naturforsch. 56b, 95—99 [2001]; eingegangen am 22. September 2000) | | |
Published
| 2001 | | |
Keywords
| Chromium, Molybdenum, Tungsten | | |
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| default:Reihe_B/56/ZNB-2001-56b-0095.pdf | | | Identifier
| ZNB-2001-56b-0095 | | | Volume
| 56 | |
16 | Author
| M. H. Vastijová3, J. K. Ohout3, J.W B Uchlerb, H.W K Atzenm Eierb, J. Kožíše, C. D. Id Ie Rje | Requires cookie* | | Title
| Crystallographic and Spectroscopic Evidence of O-Bonding in 3d-MetaI Dicyanomethanidonitrite Complexes  | | | Abstract
| The coordination of the dicyanomethanidonitrite group through the nitroso oxygen atom in the tetrakis(pyridine) complexes [M{ONC(CN)2}2(py)4], M = Ni, Co, Cu, and in the bis(pyridine) complex [Cu{ONC(CN)2}2(py)2] was proved by X-ray crystallography of the Ni11 complex and re-evaluated infrared spectra. The Ni11 and Co11 complexes exhibit almost octahedral structures composed of four pyridine nitrogen atoms and two oxygen atoms of dicyanomethanidonitrite ions. Both copper(II) complexes display a considerable axial distor tion of the pseudooctahedral arrangement. In the bis(pyridine) Cu11 complex the ONC(CN)2 groups are involved in the bridging function by use of the oxygen and nitrile nitrogen atoms. | | |
Reference
| (Z. Naturforsch. 56b, 100—104 [2001]; received July 1 2000 Dicyanomethanidonitrite Complexes) | | |
Published
| 2001 | | |
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| default:Reihe_B/56/ZNB-2001-56b-0100.pdf | | | Identifier
| ZNB-2001-56b-0100 | | | Volume
| 56 | |
17 | Author
| MarkusV. Ettelb | Requires cookie* | | Title
| Orthoamide  | | | Abstract
| , LV [1]. C7H7N30 6 -Tris(diformylamino)methan ("Formylaalen") -ein Orthoameisensäureamid-Derivat mit sechs Formylgruppen O rthoam ides, LV [1]. C7H 7N 30 6 -T ris(diform ylam ino)m ethane ("F orm ylaalen ") -an O rthoform ic A cid A m id e D erivative w ith Six Form yl G roups W illi K antlehnera b, G eorg Z ieglerb, M ichael C iesielsk ib, O liver Scherrb The preparation of tris(diformylamino)methane (3), a hitherto unknown derivative of or thoformic acid, is described. In the presence of a Lewis acid the orthoamide 3 formylates activated aromatic compounds. | | |
Reference
| (Z. Naturforsch. 56b, 105—107 [2001]; eingegangen am 25. September 2000 Orthoformic Acid Amide Derivate) | | |
Published
| 2001 | | |
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| default:Reihe_B/56/ZNB-2001-56b-0105.pdf | | | Identifier
| ZNB-2001-56b-0105 | | | Volume
| 56 | |
19 | Author
| SvenH. Oll | Requires cookie* | | Title
| Wechselwirkungen in Molekülkristallen  | | | Abstract
| , 167 [1, 2]. Kristallzüchtung und Strukturbestimmung von cr-Donator/Akzeptor-Komplexen zwischen 1,4-Dioxan und den Polyiod-Molekülen I2,1 2C=CI2, (IC)4S sowie (IC)4NR (R = H, CH3) Interaction in M olecular Crystals, 167 [1, 2]. C rystallization and Structure D eterm ination o f a -D onor/A cceptor C om p lexes b etw een 1,4 -D ioxan e and the P oly iodine M olecules I2,1 2C=CI2, (IC)4S and (IC)4N R (R = H, C H 3) Hans B ock Donor/Acceptor Complexes, 1,4-Dioxane and Polyiodine Compounds, Selforganization Phenomena With 1,4-dioxane as the constant donor, five new donor/acceptor complexes with the polyiodi ne compounds I-I, I2C=CI2, tetraiodothiophene and two tetraiodopyrrole derivatives could be crystallized and their structures determined despite their decomposition in air. They provide interesting facets for selforganisation on crystallization: The 1,4-dioxane addition causes at best small structural changes of the polyiodine compounds. All adducts crystallize in chains of alternating donors and acceptors, which also staple separatedly. The direction of the con tacts O -I depends on the incorporation of the 1,4-dioxane molecules into the iodine acceptor layers. The structural results correlate with those obtained for donor/acceptor complexes with organosulfur donors and, therefore, add to the rationalization of intermolecular interactions. | | |
Reference
| (Z. Naturforsch. 56b, 111—121 [2001]; eingegangen am 9. August 2000) | | |
Published
| 2001 | | |
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| default:Reihe_B/56/ZNB-2001-56b-0111.pdf | | | Identifier
| ZNB-2001-56b-0111 | | | Volume
| 56 | |
20 | Author
| AthanassiosK. Boudalisa, Vassilios Nastopoulos3, Ans Terzisb, CatherineP. Raptopouloub, SpyrosP. Perlepes3 | Requires cookie* | | Title
| Reaction between Yttrium Nitrate and 2,2':6,2"-Terpyridine (terpy) in MeCN: Preparation, Crystal Structures and Spectroscopic Characterization of [Y (N 03)3(terpy)(H20 )] and [Y(N03)3(terpy)(H20 )] * terpy * 3 MeCN  | | | Abstract
| The reaction of Y(NC>3)3 5H2O and 2,2':6',2"-terpyridine (terpy) in MeCN leads to [Y(N0 3)3(terpy)(H20)] (1) and [Y(N0 3)3(terpy)(H2 0)] terpy-3MeCN (2) in good yields de pending on the isolation conditions. The structures of both complexes were determined by single-crystal X-ray crystallography. The Y m atom in 1 is 9-coordinate and ligation is pro vided by one terdentate terpy molecule, two chelating nitrates, one monodentate nitrate and one terminal H2O molecule; the coordination polyhedron about the metal may be viewed as a tricapped trigonal prism. The Y ni atom in 2 is 10-coordinate and its coordination sphere consists of three nitrogen atoms from the terdentate terpy, six oxygen atoms from the three chelating nitrates (one of them being "anisobidentate") and one oxygen atom from a terminal H2O molecule; the polyhedron about the metal may be viewed as a distorted sphenocorona. The interstitial terpy is strongly hydrogen-bonded to the O atom o f the coordinated H2O molecule to form [Y(N0 3)3(terpy)(H2 0)j -terpy pairs. The new complexes were characterized by IR and 'H NMR spectroscopies. The Y in/N0 3 -/terpy chemistry is compared to the already well-developed Lnin/N0 3 _ /terpy chemistry (Ln = lanthanide). | | |
Reference
| (Z. Naturforsch. 56b, 122—128 [2001]; received August 8 2000) | | |
Published
| 2001 | | |
Keywords
| 2, 2':6', 2"-Terpyridine Complexes, Yttrium Nitrate Complexes | | |
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| default:Reihe_B/56/ZNB-2001-56b-0122.pdf | | | Identifier
| ZNB-2001-56b-0122 | | | Volume
| 56 | |
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