bluuebunny/crossref_metadata_2025_split huggingface dataset:
Unsymmetrisch substituierte Phosphinoschwefeldiimide – NMR-Untersuchungen über die Konfiguration in Lösung/ Unsymmetrically Substituted Phosphino Sulfur Diimides – NMR Studies on the Configuration in Solution
Authors: Herberhold Max , Frank Stefan M. , Wrackmeyer Bernd 
Published: March 2015

Abstract
The phosphino-substituted sulfur diimides S(N-PtBu2)2 (1), tBu;P(NSN)PRR′ (R = R′ - phenyl (2a), cyclohexyl (2b), isopropyl (2c), ethyl (2d); R = phenyl, R′ = tert-butyl (2e)) and tBu2P(NSN)tBu (3) were studied in solution by 1H, 13C and 31P NMR spectroscopy**. The coupling constants 4J(31P31P) of the compounds containing different phosphino groups, 2a-e, depend both on the nature of the solvent and the temperature. The NMR results are interpreted in accord with a rapid Z/E⇄ E/Z interconversion at room temperature and the predominance of a single configurational isomer at low temperatures. There is no indication for the presence of the “symmetrical” configurations, Z/Z or E/E respectively, in solution in appreciable amounts. 15N NMR data are also reported for a series of sulfur diimides.
Darstellung von Dichalkogenostibanen des Typs RSb(ER′)2 (R = CH3, C2H5; E = S, Se; R = CH3, C6H5)/ Preparation of Dichalcogenostibanes of the Type RSb(ER′)2 (R = CH3, C2H5; E = S, Se; R′ = CH3, C6H5 )
Authors: Breunig Hans Joachim , Güleç Sabahittin 
Published: March 2015

Abstract
Dichalcogenostibanes of the type RSb(ER′)2 (R = CH3 ,C2H5; E = S. Se; R′ = CH3. C6H5) and trialkylstibanes R3Sb have been prepared by redistribution reactions of stibanes of the type R2SbER′.
Synthese und Eigenschaften von tert-Butyltriiodsilan/ Synthesis and Properties of tert-Butyltriiodosilane
Authors: Baudler Marianne , Arndt Uwe , Grenz Detlef 
Published: March 2015

Abstract
tert-Butyltriiodosilane (1) has been prepared in its pure form by heating tert-butylsilane (2) with iodine. Compound 1 has been characterized by elemental analysis as well as by spectroscopic methods.
Synthesis and Activity of Juvenile Hormone Analogues (JHA)
Authors: Rodriguez Juan B. , Gros Eduardo G. , Stoka Angel M. 
Published: March 2015

Abstract
From geranylacetone and by the use of a variety of reagents, twelve analogues of the juvenile hormone III were synthesized. The compounds (5-16) have an isoprenic structure bearing at the extreme of the chain functional groups as carbonate, carbamate, thiolcarbonate, thiolcarbamate, carbonyloxyimino and thiol carbonyloxyimino. Compounds 5-9 present the normal unsaturated isoprenic chain while compounds 10-16 have a monoepoxide function. All the compounds were tested for their respective juvenile hormone activity for Triatoma infestans and Rhodniusprolixus. The most active compounds were those having a thiol carbonate group independently of the oxidation state of the molecule. The synthetic procedures and the biological results are discussed.
The Crystal Structure of Potassium Nickel Arsenate; KNiAsO4
Authors: Buckley A. M. , Bramwell S. T. , Day P. , Harrison W. T. A. 
Published: March 2015

Abstract
The crystal structure of potassium nickel arsenate. KNiAsO4 has been determined by high resolution powder neutron diffraction at 30 K. The unit cell of KNiAsO4 is rhombohedral. space group R3̄, with hexagonal cell constants, a = 4.97208(2) (Å). c = 28.52606(10) (Å). The compound is isomorphous with NaNiAsO4.
Elektronenreiche Olefine, 2 Struktur und Elektrontransfer-Reaktivität des cyclisch σ/π-hyperkonjugierten Carbosilans 3,3,6,6-Tetrakis(trimethylsilyl)-1,4-cyclohexadien
Authors: Hausen Hans-Dieter , Bessenbacher Christian , Kaim Wolfgang 
Published: March 2015

Abstract
Crystal and molecular structure analysis of the title compound 1, a most electron rich carbosilane, exhibits a shallow boat conformation for the cyclohexadiene ring which is shielded by four bulky Me3Si groups. Multiple hyperconjugative interaction occurs between the two non-conjugated olefinic π systems and the four rather long (192 pm) carbon-silicon o bonds which form an angle of about 34° with the assumed π axis. The HOMO destabilization caused by this unique structural arrangement explains the energetically facile formation and subsequent reactivity of the cation radical 1+ which was found to undergo oxidative desilylation to the aromatic 1,4-bis(trimethylsilyl) benzene precursor in the single electron transfer reaction with TCNE.
Tetrakis[bis(trimethylsilyl)methyl]dialan(4), eine Verbindung mit Aluminium—Aluminium-Bindung
Authors: Uhl Werner 
Published: March 2015

Abstract
The reaction of chloro-bis[bis(trimethylsilyl)methyl]alane (1) with potassium yields the title compound 2.2 crystallizes in the triclinic space group P1̄ and shows an aluminium -aluminium bond length of 266.0(1) pm. The core of the molecule is almost planar.
Die Kristallstruktur von N,N,N'-tris(trimethylsilyl)benzamidin sowie die Synthese und Kristallstruktur von DichIorantimon-N,N'-bis(trimethylsilyl)benzamidinat
Authors: Ergezinger Christina , Weller Frank , Dehnicke Kurt 
Published: March 2015

Abstract
N,N,N'-Tris(trimethylsilyl)benzamidine, [C6H5-C(NSiMe3)N(SiMe3)2], reacts with antimony trichloride in CH2Cl2 solution to form monomeric dichloroantimony-N,N'-bis(trimethylsilyl)- benzamidine, [SbCl2(NSiMe3)2C-C6H5]. Both benzamidine derivatives have been character­ized by crystal structure determinations. [C6H5-C(NSiMe3)N(SiMe3)2]: space group P21/c, Z = 4, 2278 observed independent refle­xions, R = 0,038. Lattice dimensions (19 °C): a = 1521,0(1); b = 656.7(1); c = 2163,0(1) β = 94,21(1)°. The compound forms monomeric molecules with CN distances of 126,6 pm, and 141,0 pm, respectively, corresponding to C=N̄-SiMe3 and C-N(SiMe3)2 moieties. [SbCl2(NSiMe3)2C-C6H5]: space group P21/c, Z = 4, 2707 observed independent reflexions, R = 0,027. Lattice dimensions (19 °C): a = 1212,7(1); b = 962,1(1); c = 1728,9(1) pm; β = 98,02(1)°. The compound forms monomeric molecules in which the antimony atom is surrounded by two chlorine atoms, and by the N atoms of the benzamidine chelate, forming a distorted trigonal bipyramidal arrangement, which is a consequence of the steric effect of the lone pair on the Sb atom.
The Reactions of Hydroxyl Radicals with 1,4-and 1,3-Cyclohexadiene in Aqueous Solution
Authors: Pan Xian-Ming , Bastian Eugenie , Sonntag Clemens von 
Published: March 2015

Abstract
The reactions of radiolytically generated hydroxyl radicals and H atoms with 1,4- and 1,3-cyclohexadiene were studied by pulse radiolysis and product analysis. Hydrogen abstraction from these substrates by the OH radical yields the cyclohexadienyl radical (ε (310 nm) = 4400 dm3 mol-1 cm-1 from the reaction of the H atom with benzene) with an efficiency of 50% (0.29 ,μmol J-1) in the case of 1,4-cyclohexadiene and 25% (0.15 ,μmol J-1) in the case of 1,3-cyclohexadiene as determined by pulse radiolysis. The remaining OH radicals add to the olefin. In 1.4-cyclohexa- diene the yield of the resulting adduct radicals has been determined in a steady-state 60Co-γ-irradiation experiment by reducing it with added 1.4-dithiothreitol (DTT) to 4-hydroxycyc- lohexene. There are two sites of OH radical attack in the case of 1.3-cyclohexadiene, and only the alkyl radical is reduced quantitatively by DTT (G(3-hydroxycyclohexene) = 0.15 ,μmol J-1). From material balance considerations it is concluded that the allylic radical must be formed with a G value of 0.28 ,μmol J-1 but largelv escapes reduction by DTT (G(4-hvdroxycyclohexene) = 0.03 ,μmol J-1). H atoms add preferentially to the double bonds of 1,4- and 1,3-cyclohexadiene (78% and 93%, respectively), while the O.- radical (the basic form of the OH radical) undergoes mainly H- abstraction (92% and 83%, respectively). The radicals formed in these systems decay bimolecularly (2k = 2.8 x 109 dm3 mol-1 s-1). In their combination reactions the cyclohexadienyl radicals form the four possible dimers in propor­tions such that the dienyl radical moiety shows a 2:1 preference to react from its central (1a) rather than from a terminal carbon atom (1b). Cyclohexadienyl radicals and the OH- and H-adduct radicals also cross-tcrminate by disproportionation and dimerization. Material balance has been obtained for the 1,4-cyclohexadiene system in N2O-Saturated solution (10-2 mol dm-3) at a dose rate of 0.14 Gy s-1, the products (G values in ,μmol J-1) being: benzene (0.085), 4-hydroxycyclohexene (0.25), cyclohexadienyl-dimers (0.144). cvclohexadienyl-OH-adduct- dimers (0.02), OH-adduct-dimers (0.02). Some of the 4-hydroxycyclohcxene is formed in an H-abstraction reaction by the OH-adduct radical from 1,4-cyclohexadiene.
Darstellung des Stibinoschwefeldiimid-Achtrings tBuSb(NSN)2SbtBu und einiger seiner Carbonylmetall-Derivate / Synthesis of the Eight-Membered Stibino-Sulfur Diimide Ring tBuSb(NSN)2SbtBu and Some of its Carbonylmetal Derivatives
Authors: Herberhold Max , Schamel Klaus 
Published: March 2015

Abstract
The first antimony-sulfur-nitrogen heterocycle, tBuSb(NSN)2SbtBu (1b)**, has been prepared from the reaction of tBuSbCl2 with the salt K2SN2. It forms stable chelate complexes of the type (CO)4M[tBuSb(NSN)2SbtBu] (M = Cr (3b), Mo (4b), W (5b)). The pentacarbonylchromium complex (CO)5Cr[tBuSbCl2] reacts with K2SN2 to give the mononuclear derivative (CO)5Cr[tBuSb(NSN)2SbtBu] (2b) containing the eight-membered ring 1b, whereas the corre-sponding complexes (CO)5Cr[R2SbCl] (R = tBu, Ph) are converted into binuclear sulfur diimide derivatives (CO)5Cr[R2Sb(NSN)SbR2]Cr(CO)5 (R = tBu (6b). Ph (7b)). The new stibino-sulfur diimides 1b-7b have been characterized by IR and NMR (1H and 13C) spectroscopy.
Diolefinbis(trimethyIphosphine)cobalt(0) Compounds: Stable Organometallic Radicals with Distorted Ground State Structures
Authors: Klein Hans-Friedrich , Helwig Michael , Koch Udo , Lull Goetz , Tadic Marko , Krüger Carl , Hofmann Peter 
Published: March 2015

Abstract
Diolefincobalt(O) complexes Co(L2)(PMe3)2 {L2 -[CH2 = CHSi(OMe)2]2O (1), [CH2 =CHSi(OEt)2]2O (2), (CH2 =CHCH2)2SiMe2 (3), [(CH2 =CHCH2)2N]2CH2 (4)} have been synthesized from Co(C5H8)(PMe3)3 and diolefins at ambient temperatures. Reactions with allyl ethers or with allyltin or allylphosphorus compounds involve transfer of allyl groups to the cobalt, while allylamine simply replaces cyclopentene (C5H8) to give Co(CH2 =CHCH2NH2)(PMe3)3 (5). Cationic cobalt(I) complexes containing olefin ligands as in 1-4 could not be obtained under conditions where norbornadiene readily gave [Co(C7H8)(PMe3)3 ]BF4 (6). Paramagnetic 4 shows a magnetic moment μeff = 2.0 μв (between 3.6 and 293 K), corresponding to one unpaired electron per cobalt atom. Compound 4 crystallizes in the space group P21/c with Z = 4, a = 14.986(4), b = 17.223(5), c = 15.436(3) Å,β = 117.98(2)°, V = 3518.4 Å3 . Each cobalt atom is η4-coordinated to a diolefin involving the smaller of two possible chelating rings. The Co-C distances range only from 2.029(6) to 2.058(6) Å for the olefin ligands, whereas Co-P bond lengths at each cobalt differ significantly: Co1-P1 2.188(2), Co1-P2 2.248(2); Co2-P3 2.185(2), Co2-P4 2.258(2) Å. This feature of two significantly different Co-L bond lengths is hitherto seen in all structurally characterized (bisolefin)CoL2 complexes (L = PMe3, CH3CN) and can be rationalized by molecular orbital calculations (Extended Hückel) on the 17 electron model system (PH3)2Co(C2H4)2.
Strukturen und Schwingungsspektren neuer Wolframatophosphate / Structures and Vibrational Spectra of Novel Tungstophosphates
Authors: Fuchs Joachim , Palm Rosemarie 
Published: March 2015

Abstract
A solution of Na2WO4 • 2H2O and Na2HPO4 (3:1) was acidified with acetic and perchloric acid, respectively, and yielded mixtures of crystals. These were mechanically separated under a microscope according to the appearance of the crystals and the pure phases were subjected to vibrational (IR and Ra) and X-ray investigations. The compounds have the formulae Na20P6W18O79 ·nH2O (I) with n = 41,32 and 12, and Na12P4W14O58 · 42H2O (II), respectively. By carrying out secondary reactions one obtains two more phases of (II) with less water of crystallization (36 and 34 H2O) as well as a hydrolysis product of (I), the compound Na20P5W18O75(OH)3-42H2O (III). The structures of (I) (41-hydrate), (II) (36-hydrate) and (III) were discussed. Besides centrally bound phosphate groups their anions also contain peripherally bound phosphate groups. These compounds can now be identified by the characteristic features of their vibrational spectra
Isomere vierkernige Molybdän—Wolfram—Schwefelclusterdithiophosphinate / Isomeric Tetranuclear Molybdenum—Tungsten — Sulfurclusterdithiophosphinates
Authors: Deeg Axel , Keck Helmut , Kruse Andreas , Kuchen Wilhelm , Wunderlich Hartmut 
Published: March 2015

Abstract
A mixture of three isomeric clusters of composition Mo3WS4(Et2PS2)6 (3) is obtained by reacting equimolar quantities of Mo3S4(Et2PS2)4, W(CO)3(CH3CN)3 and [Et2P(S)]2S2 in toluene'. Some NMR-spectroscopic data and the magnetic properties of these isomers are reported. Isomer 3a consists of a distorted cubane Mo3WS4, each metal of which is coordinated by six S atoms: three of them belonging to the cubane, one to a bridging and two to a chelating ligand Et2PS2
-. The crystal structure of isomer 3b is reported. In 3b only three of the metals in the core are coordinated in this manner while the fourth is surrounded by three S of the cubane and three S of bridging ligands. 3b crystallizes in the orthorhombic space group Pbca, Z = 8. lattice parameters a = 2184,4(8), b = 2264,4(9). c = 2388.2(8) pm. The crystal structure was refined to R = 0.05 using 5398 observed reflections. By HPLC 3b can be separated into two isomers. 3b1 and 3b2, both differing in the type of metal. Mo or W. bonded to the three bridging ligands
Nd7,33Ta8O28CI6 — ein Zwischenprodukt des thermischen Abbaus von Nd2Ta2O7Cl2: Präparation, Struktur und magnetische Eigenschaften / Nd7,33Ta8O28Cl6 — an Intermediate Product of the Thermal Decomposition of Nd2Ta2O7Cl2: Preparation, Crystal Structure and Magnetic Properties
Authors: Schaffrath U. , Gruehn R. 
Published: March 2015

Abstract
Single crystals of the new oxochlorotantalate Nd7.33Ta8O28Cl6, could be obtained only by chemical transport reactions (T2 → T1; T2 - 1000 °C, T, = 900 °C) with mixtures of Cl2/TaCl5 as transport agent. NdTaO4 was chosen as the starting material. A direct preparative route to Nd7.33Ta8O28Cl6 from binary and ternary components, however, was not successful. Nd7.33Ta8O28Cl6 , crystallizes in the space group Cmmm with a = 10.3381(8) Å, b = 18.865(1) Å, c - 3.9152(3) A; Z = 1. The structure was refined to R - 4.42%, R w = 2.76%. Main building units are pairs of edge-sharing TaO6 -octahedra which are connected with threefold capped trigonal prisms around Nd. Especially remarkable is one Nd position with an occupation factor of 0.833. The relationship of this new structure type with Nd2Ta2O7Cl2 is considered. Furthermore, we have measured the magnetic susceptibilities of both Nd-compounds in a temperature range from 3,6 to 251,3 K. The results are compared with calculated data.
Achtfachkoordination von Cadmium(II) und sekundäre Metall—Ligand-Bindungen in [Cd(NO3)2(C12H22N6)] und [Cd(C12H22N6)2(BF4)2 / Eight-Coordination of Cadmium(II) and Secondary Metal —Ligand Bonds in [Cd(NO3) 2(C12H22N6)] and [Cd(C12H22N6) 2(BF4)2
Authors: Strasdeit Henry , Pohl Siegfried 
Published: March 2015

Abstract
[Cd(NO3)2(C12H22N6)] (1), [Cd(C12H22N6)2](BF4)2 (2), and [Cd(C12H22N6)2](ClO4)2 (3) are obtained from methanolic solutions by reaction of 2,5,8,10,13,16-Hexaazapentacyclo[ 8.6.1.125.0918.0l3,7]octadecane (C12H22N6) with Cd(NO3)2-4H2O, Cd(BF4)2, and Cd(ClO4)2 · 6H2O, respectively. 1 crystallizes in the monoclinic space group C2/c with a = 10.346(1), b =18.162(1), c - 10.462(1) Å, β = 112.95(1)°, and Z = 4. 2 is monoclinic, space group P21/n, a = 16.958(1), b = 10.653(1), c = 18.747(1) Å, β= 112,66(1)°, and Z = 4. The X-ray structures of 1 and 2 were refined to R(Rw) = 0.028 (0.029) and 0.060 (0.057), respectively. The compounds contain discrete [Cd(NO3)2(C12H22N6)] and [Cd(C12H22N6)2]2+ complexes, respectively. The Cd atoms are eight-coordinated with four primary and four longer, secondary metal -ligand bonds. In both complexes the hexaamine has an axially symmetrical configuration and acts as a tetradentate ligand. The N03 ligands are aniso-bidentate. Mean bond lengths are (Cd -N)prim 2.308(3), (Cd-N)sec 2.676(3), (Cd-0)prim 2.331(2), (Cd-0)sec 2.593(3) Å for 1, and (Cd-N)prim 2.374 (ligand 1), 2.438 (ligand 2), (Cd-N)sec 2.746 (ligand 1), 2.702 Å (ligand 2) for2. In water the neutral complex 1 dissociates and behaves as an 1:2 electrolyte. 13C and 113Cd NMR data and the conductivity of solutions of 2 or 3 in dimethyl sulfoxide indicate a fast but incomplete exchange of the ligands in [Cd(C12H22N6)2]2+ by solvent molecules
Rhodium(I)-Komplexe mit 2,5-Difurfurylpyrrol-Liganden / Rhodium(I) Complexes with 2,5-Difurfurylpyrrole Ligands
Authors: Lindner Ekkehard , Schneider Horst W. , Fawzi Riad , Englert Ulrich , Hiller Wolfgang 
Published: March 2015

Abstract
The 2.5-difurfurylpyrrole-O.N.O ligands 3a, b [R = CO2C2H5 (a). COCH, (b)] are obtained by reaction of the furanes l a , b with the 2,5-bis(chloromethyl)pyrrole 2 in the presence of SnCl4. Proton abstraction from 3a, b with NaH affords the sodium salts 4a-Na and 4b-Na. Exchange of the chlorine bridges in [μ-ClRh(Diol)]2 (5,5') (Diol = cyclooctadiene, norbornadiene) results in the formation of the 14-electron complexes (Diol)Rh(O.N.O) (6a,6'a). Addition of PPh3, yields the four-coordinated rhodium complexes (Diol)Rh(O.N.O)(PPh3) (7a,7'a). These compounds are also available in a reverse reaction sequence from 5,5', PPh3, and 4a-Na. The mononuclear rhodium complexes RhCl(Diol)(PPh3) (8,8') are isolated as intermediates. In 7a, 7'a the olefinic ligands are replaced by carbon monoxide to give the dicarbonyl rhodium complex (OC)2Rh(O.N.O)(PPh3) (9a) being detectable only in solution. The same result is achieved upon addition of CO to the compound (OC)Rh(O.N.O)(PPh,) (11a) which results bv the reaction of [μ-ClRh(CO)(PPh3)]2 (10) with 4a-Na. Oxidative addition of CH3I or H2 to 6a, 6 a, 7a, 7'a or 11a was not observed. 1H and 31P{1H} NMR investigations indicate that depending on the temperature the O.N.O ligand in the 14-electron rhodium complex 11a acts as tri- (11a-A), bi- (11a-B) and monodentate (IIa-C) ligands. respectively. 11a also reacts with PPh, to form the /ram-bis(phosphane)rhodium complex (PPh3)2Rh(CO)(O.N.O) (12a). 12a and the analogous complexes 12b and trans-(PMe3)2Rh(CO)(O,N.O) (14a) are obtained by action of ClRh(CO)L2 (13) (L = PPh3. PMe3) on 4a-Na and 4b-Na, respectively. The methylene bridges in the O.N.O ligand 3a are not oxidized, neither in the non-complexed (3a) nor in the complexed (12a) state. According to an X-ray structural analysis 14a crystallizes in the monoclinic space group P21/n with Z = 4. In 6a, 6'a, 7a, 7'a, 9a, 11a, 12a, b, and 14a the O.N.O ligand is always nitrogen bonded
N,N'-Bis(trimethylsilyl)benzamidinato-Koniplexe von Titan und Zirkon. Die Kristallstrukturen von [C6H5-C(NSiMe3)2MCl3]2; M = Ti, Zr / N,N'-Bis(trimethylsilyl)benzamidinato Complexes of Titanium and Zirconium. The Crystal Structures of [C6H5-C(NSiMe3)2MCl3 ]2 ; M = Ti, Zr
Authors: Fenske Dieter 
Published: March 2015

Abstract
The N,N'-bis(trimethylsilyl)benzamidinato complexes [C6H5 -C(NSiMe3)2MCl3]2(M = Ti. Zr) have been prepared by the reactions of N,N,N'-tris(trimethylsilyl)benzamidine
[C6H5-C(NSiMe3)N(SiMe3)2] with titanium tetrachloride, and zirconium tetrachloride, respec-tively. The compounds form moisture sensitive, dark red (Ti) and white (Zr) crystals, which were characterized by crystal structure determinations. [C6H5-C(NSiMe3)2TiCl3]2 : space group P21/rc. Z = 2, 4373 observed independent reflexions, R = 0.034. Lattice dimensions (-90 °C): a - 959.0(8); b = 1196.5(8); c = 1770.9(11) pm; β = 93.79(4)°. [C6H5-C(NSiMe3)2ZrCl3]2 : space group P21/n. Z = 2, 3160 observed independent reflexions, R = 0.031. Lattice dimensions (-90 °C): a = 971.6(7); b = 1222.2(9); c = 1792.9(10) pm; β = 93.51(5)°.
Both complexes crystallize isotypically, forming centrosymmetric dimeric molecules via chloro bridges with bond lengths of 242.0 and 253.8 pm (Ti), and of 253.7 and 264.9 pm (Zr). The metal atoms complete their distorted octahedral surroundings with two chlorine ligands and the nitrogen atoms of the chelating amidinato ligand. The N atoms of the amidinato group are in equatorial and axial positions. This accounts for the different metal-nitrogen bond lengths of 207 pm (ax) and 199 pm (eq) in the titanium compound and 219 pm (ax) and 214 pm (eq) in the zirconium complex.
N-Chloronitrenokomplexe des Wolframs: Synthesen und Kristallstrukturen von PPh3Me[Cl5W(NCl)] und (PPh4)3{[Cl5W(NCl)]2Cl} • CCl4 • 4CH3CN / N-Chloro-Nitrene Complexes of Tungsten: Syntheses and Crystal Structures of PPh3Me[Cl5W(NCl)] and (PPh4)3{[Cl5W(NCl)]2Cl} CCl4-4CH3CN
Authors: Gorge Astrid , Patt-Siebel Ute , Müller Ulrich , Dehnicke Kurt 
Published: March 2015

Abstrct
The N-chloro-nitrene complexes PPh3Me[Cl5W(NCl)] and (PPh4)3{ [Cl5W(NCl)]2Cl} • CCl4 • 4CH3CN were prepared by the reaction of [CI4W(NCl)]2 with [PPh3Me]Ci in CH2Cl2 and with [PPh4]Cl in CH3CN. respectively, followed by precipitation with CCl4. Both compounds form red, moisture-sensitive crystals, which were characterized by IR spectroscopy as well as by X-ray structure determinations. PPh3Me[CUW(NCl)]: space group P1̄, Z = 2, a = 862.7(3), b = 1108.4(2), c = 1411.0(5) pm. a = 71.74(3)°, β = 76.78(3)°, y = 77.55(2)° (at 18 °C); 2843 unique observed reflexions, R = 0.042. The compound consists of ions PPh3Me+ and [Cl5W(NCl)]-, in which the tungsten atom has a distorted octahedral environment of five chlorine atoms and the nitrogen atom of the N-chloro-nitrene ligand

with bond distances WN = 169 pm and N-Cl = 160 pm. bond angle WNCl = 175°.
(PPh4)3{[Cl5W(NCl)]2Cl} • CCl4• 4CH3CN: space group P4/n, Z = 2, a = 1298.2(8). c = 2720.4(7) pm (at 17 °C); (1979 unique observed reflexions. R = 0.096). The compound contains cations PPh4
+ and anions {[CI5W(NCl)]2Cl}3-, in which two [Cl5W(NCl)]- ions are bridged by a chloride ion to form the linear unit [Cl5W≡N-Cl ··· Cl -Cl-N≡WCl5]3- with Cl ··· Cl-contactsof 288 and 278 pm
Die Amino- und Azidoborierung von Iminoboranen / The Amino- and Azidoboration of Iminoboranes
Authors: Paetzold Peter , Meier Hans-Ulrich , Schwan Heinrich , Plotho Christoph von 
Published: March 2015

Abstract
Iminoboranes RB=NR" (3a-c; R/R" = iPr/iPr, Bu/tBu, iBu/iBu) are aminoborated by aminoboranes AO(A)N = BR'2 (1a - c ; R' = Et, Bu, 1/2 - CH2-CHMe -CH2-CH2-) or azidoborated by azidoboranes N3=BR'2 (2a-c; R' = Pr. Bu. Ph) to give products

(4a-d) or

(5a-d), respectively. Hypothetical alkyloboration of 3 by 1, 2 can be excluded by applying AO(A)N = 10BBu2 and N3=10BBu2 as boration agents (A = Me3Si)
Die Reaktion von N,N,N'-Tris(trimethylsilyI)benzamidin mit Kupfer(II)chlorid. Kristallstruktur von {C6H5-C(NSiMe3)2CuCl[C6H5-C(NSiMe3)(NHSiMe3)]}/ The Reaction of N,N,N'-Tris(trimethylsilyl)benzamidine with Copper(II) Chloride. Crystal Structure of {C6H5—C(NSiMe3)->CuCl · [C6H5-C(NSiMe3)(NHSiMe3)]}
Authors: Hey Evamarie , Ergezinger Christina , Dehnicke Kurt 
Published: March 2015

Abstract
,N,N'-Tris(trimethylsilyI)benzamidin mit Kupfer(II)chlorid. Kristallstruktur von {C 6 H 5 -C(NSiMe 3) 2 CuCl [C 6 H 5 -C(NSiMe 3)(NHSiMe 3)]} The Reaction of N,N,N'-Tris(trimethylsilyl)benzamidine with Copper(II) Chloride. Crystal Structure of {C 6 H 5 —C(NSiMe 3)->CuCl • [C 6 H 5 -C(NSiMe 3)(NHSiMe 3)]}