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  • 1
    Electronic Resource
    Electronic Resource
    [Gd4(C2)](Cl, I)6, an Interstitially Stabilized Heteroleptic Gadolinium SesquihalideDedicated to Professor John D. Corbett on the Occasion of his 70th Birthday (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 494-500 
    Details
    ISSN: 0044-2313
    Keywords: Gadolinium sesquihalide ; interstitial carbon units ; crystal structure ; electronic structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Gd4(C2)](Cl, I)6, ein interstitiell stabilisiertes, heteroleptisches Gadoliniumsesquihalogenid[Gd4(C2)](Cl, I)6 erhält man aus CsI, Gd, GdCl3 und C2I4 in verschweißten Niob-Ampullen bei 1000/800°C in Form von schwarzen, glänzenden Nadeln. Die Kristallstruktur (tetragonal; P4/mbm; Z = 2; a = 1347,5(1); c = 1212,5(1) pm) ist ähnlich wie jene von Na[Mo4]O6 bzw. [Sc4B]Cl6. Trans-kantenverknüpfte [Gd6]-Oktaeder verlaufen parallel [001]. Sie enthalten interstitielle C2-Einheiten, Jedes dritte Oktaeder enthält fehlgeordnete C2-Einheiten, senkrecht zu jenen in den benachbarten [Gd6(C2)]-Oktaedern. Diese sind daher entlang der (pseudo)-C4-Achse gestaucht. Rechnungen zur elektronischen Struktur zeigen, daß insgesamt 13 Elektronen zur Auffüllung aller Metall-Metall-bindenden Zustände für eine „leere“ [Gd4]Cl6-Struktur nötig wären. Die Einlagerung der C2-Dimeren verändert die Bindungsverhältnisse in [Gd4(C2)]X6 (X = Cl, I) erheblich. Die formale Ladung von -6 der C2-Einheit wird durch das Aufsplitten der πg-Zustände reduziert, Gd—Gd und Gd—C-bindende Zustände werden besetzt und bindende dx2-y2-Orbitale kombinieren zu den am niedrigsten liegenden nicht besetzten Zuständen.
    Notes: [Gd4(C2)](Cl, I)6 is obtained from CsI, Gd, GdCl3 and C2I4 in sealed niobium containers at 1000/800°C as black, shiny needles. The crystal structure (tetragonal, P4/mbm, Z = 2, a = 1347.5(1), c = 1212.5(1) pm) is similar to that of Na[Mo4]O6 and [Sc4B]Cl6. It may be regarded as being built from octahedra sharing common trans edges running in the [001] direction. The octahedra contain C2 units as interstitials. Every third octahedron contains a disordered C2 unit perpendicular to those in the two neighboring [Gd6(C2)] octahedra and is therefore compressed in the direction of the (pseudo) C4 axis. Calculations of the electronic structure of an “empty” [Gd4]Cl6 structure reveals a total of 13 electrons necessary to occupy all metal-metal bonding states. The incorporation of a carbon dimer substantially alters the bonding conditions for [Gd4(C2)]X6 (X = Cl, I). The formal charge of -6 of the C2 unit is significantly reduced as πg states split up, Gd—Gd and Gd—C bonding states are occupied and bonding dx2—y2 orbitals combine to form the lowest unoccupied energy states.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220318
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  • 2
    Electronic Resource
    Electronic Resource
    Pyrazolate-Based Oligonuclear Copper and Silver Complexes with N/S Coordination SpheresDedicated to Prof. Dr. Gottfried Huttner on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1441-1447 
    Details
    ISSN: 0009-2940
    Keywords: Pyrazolate complexes ; Bridging ligands ; Copper ; Silver ; N,S-Donor Ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of pyrazole-based potential ligands bearing thioether substituents in 3- and 5-positions of the heterocycle was synthesized [3,5-bis(RSCH2)-pyzH R=Ph (1aH), PhCH2 (1bH), iPr (1cH), tBu (1dH)]. These ligands afford oligonuclear Cu1 and Ag1 coordination compounds [LCu]x (2a-c, L = 1a - c) and [LAg]x (3a-d, L = 1a-d), respectively. The single crystal X-ray analysis of 3c shows the presence of trimeric planar arrays of N,N′-bridging pyrazolates and linear coordinated silver ions, with each two of the trinuclear moieties being linked by two unsupported short intermolecular Ag…Ag contacts [3.041(1) Å]. Molecular-weight determinations for 2a (THF) and 3c (toluene) indicate that hexanuclear entities are preserved in solution. Starting from 1bH the CuII complex [(1b)2Cu2](BF4)2 (4) was synthesized. According to an X-ray crystal structure analysis it consists of dinuclear molecules with two bridging pyrazolates, distorted square planar N2S2 coordination spheres for Cu11 and an axially bridging tetrafluoroborate. Magnetic susceptibility data reveal an antiferromagnetic exchange (J = -206 cm-1) that is among the highest found for doubly pyrazolate bridged dicopper(II) complexes, which is rationalized on the basis of the rather symmetric dinuclear core of 4. The irreversibility of the electrochemical reduction and oxidation processes for the CuII and CuI compounds, respectively, is explained by the inability of the respective coordination framework to adapt to different geometric preferences.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301014
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  • 3
    Electronic Resource
    Electronic Resource
    Dimeric Silver(I) Complexes of Some Isothiazole-Based LigandsDedicated to Prof. Dr. Rolf Gleiter on the occasion of this 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 95-100 
    Details
    ISSN: 0009-2940
    Keywords: Isothiazole complexes ; Dinuclear silver(I) complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of isothiazole-based potential ligands bearing substituents with additional donor sites in the 5-position of the heterocycle was synthesized [3-Me-5-R-C3HNS; R = CH=N(CH2)2py (1), CH=NCH2py (2), CH2N(CH2CH2NEt2)2 (4), (CH2)2SMe (5)]. Upon reaction with AgO3SCF3 they formed complexes [(1)AgOSO2CF3]2 (6), [(2)AgOSO2CF3]2 (7), [(4)Ag]2+2(O3SCF-3)2 (8) and [(5)AgOSO2CF3]2 (9), respectively. 6, 8 and 9 were shown by X-ray structural analyses to consist of dimeric units L2Ag2+2, either discrete (8), coordinated by terminal CF3SO-3 units (6). In 8 and 9 the isothiazole moiety is bonded to the metal center via the ring-N. The coordination potential of the isothiazole heterocycle is discussed.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300115
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  • 4
    Electronic Resource
    Electronic Resource
    Dinuclear Cobalt(II) Complexes of Pyrazole Ligands with Chelating Side ArmsDedicated to Prof. Dr. Walter Siebert on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 605-613 
    Details
    ISSN: 0009-2940
    Keywords: Pyrazolate complexes ; Dinuclear complexes ; Bridging ligands ; Cobalt ; Conformational analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of pyrazole-based potential ligands bearing polydentate amine substituents in the 3- and 5-positions of the heterocycle has been synthesized [3,5-bis(R2NCH2)-pyzH R2N = Me2N(CH2)3NMe (2aH), [Me2N(CH2)3]2N (2bH), (Et2NCH2CH2)2N (2cH)]. Upon reaction with two equivalents of CoCl2 they form complexes LCo2Cl3 (3a-c; L = 2a-c, respectively) which are shown crystallographically to contain a dinuclear metal core bridged by both the pyrazolate unit and a chlorine atom, with each cobalt center carrying a further terminal chlorine atom. Two of the ligand side arms in 3b, c are dangling, thus leading to five-coordination of the cobalt(II) centers in all cases. Addition of two equivalents of NaBPh4 to solutions of 3b, c induced coordination of the formerly dangling side arms to the metal centers by substitution of the terminal chlorine atoms. The resulting compounds [LCo2Cl](BPh4)2 (4b, c, respectively) were characterized by X-ray structure analyses. They can be viewed as dinuclear linked versions of tran-type complexes [(tran = tris(aminoalkyl)amine] with distorted trigonal-bipyramidal coordination spheres around cobalt(II). Conformational analyses employing force-field calculations were carried out for 4b, c in order to rationalize the conformations observed in the solid state with regard to the accessible conformational space.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300511
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  • 5
    Electronic Resource
    Electronic Resource
    1,1-Hydroborierung von Alkinen mit 6-Aza-nido-decaboranen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 947-951 
    Details
    ISSN: 0009-2940
    Keywords: 6-Aza-nido-decaborane ; 9-(1-Alkenyl)-6-phenyl-6-aza-nido-decaborane ; 1,1-Hydroboration of alkynes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,1-Hydroboration of Alkynes with 6-Aza-nido-decaboranes[1]Alkynes AC≡CR′ (R′ = Me, Bu, tBu, SiMe3), that contain a mobile group A, like H or SiMe3, undergo hydroboration by 6-aza-nido-decaboranes RNB9H11 (1a-c, R = H, Ph, PhCH2) and 1,2-migration of the group A, to give the corresponding 9-(1-alkenyl)-6-aza-nido-decaboranes RNB9H10(CH=CR′A) (2a-h). Ethenes AHC=CH2 (A = SiMe3, SnBu3) are hydroborated by 1a, b as well to form products of the type RNB9H10(CH2CH2A) (3a-c). The alkyne Me3SiC=CH undergoes a hydroboration with 1b twice; the formation of (PhNB9H10)2CHCH2SiMe3 (4) proceeds by a 1,1- and a 1,2-hydroboration step, apparently. The crystal structure analysis of (PhCH2)NB9H10[CH=CMe(SiMe3)] (2e; space group Pl) reveals a (Z configuration of the ethene moiety.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280916
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  • 6
    Electronic Resource
    Electronic Resource
    Öffnung des Aza-closo-dodecaboran-Gerüsts durch Basen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1225-1229 
    Details
    ISSN: 0009-2940
    Keywords: 1-Organo-1-aza-closo-dodecaborane(12) ; Trialkylamine-1-organo-1-aza-nido-dodecaborane(12) (1/1) ; Undecahydro-1-organo-1-aza-nido-dodecaborate(1-), 2-hydro-, 2-halogeno-, 2-alkoxy-, 2-amino-, 2-alkyl- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Opening of the Aza-clso-dodecaborane Skeleton by BasesThe aza-closo-borane PhNB11H11 (1a) is opened by the amines NR3 (R = Me, Et) to give the novel aza-nido-dodecaboranes PhNB11H11(NR3) (2a, b). The non-planar open pentagonal face of 2a, b accomodates the N atom, a BHB bridge, and the base-bound B atom, according to NMR spectra and the crystal structure analysis of monoclinic 2b. A similar but more symmetric structure is found when closo-RNB11H11 (1a-c, R = Ph, Me, H) is attacked by anionic bases X- to give nido-RNB11H11X- (3a-j; R/X = Me/H, Me/F, Me/Cl, Ph/OH, H/OMe, Me/OMe, Me/OtBu, Me/NEt2, Me/Me, Me/Bu). The anions are precipitated with cations [K([18]crown-6)], [S(NMe2)3], [N(PPh3)2], [Et2NH2], or [Li(tmeda)2]. The nido-structures of type 2 and 3 are derived from the hypothetical closo-NB12H13.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951281214
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  • 7
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur von Praseodympropionat-trihydrat, Pr(CH3CH2COO)3(H2O)3Professor Gerhard Thiele zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 325-328 
    Details
    ISSN: 0044-2313
    Keywords: Praseodymium ; Propionate ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of Praseodymium Propionate Trihydrate, Pr(CH3CH2COO)3(H2O)3Single crystals of Pr(CH3CH2COO)3(H2O)3 were obtained by dissolving freshly prepared praseodymium hydroxide in diluted propionic acid. The crystal structure (monoclinic, P21/c, Z = 4, a = 1034.2(2) pm, b = 1521.2(3) pm, c = 2086.3(7) pm, β = 102.87(2)°, R1 = 0.0864, wR2 = 0.1196) consists of one-dimensional infinite chains parallel [010]. Pr1 and Pr2 are coordinated by four tridentate-bridging propionate groups. Additionally, Pr1 is coordinated by three “coordination water” molecules, Pr2 by two bidentate propionate groups. There are, in addition, three “crystal water” molecules so that praseodymium propionate trihydrate should be formulated as [(H2O)3Pr1(CH3CH2COO)4Pr2(CH3CH2COO)2] (H2O)3.
    Notes: Einkristalle von Pr(CH3CH2COO)3(H2O)3 wurden durch Auflösen von frisch gefälltem Praseodymhydroxid in verdünnter Propionsäure und anschließendes Eindunsten bei Raumtemperatur an der Luft erhalten. Die Kristallstruktur (monoklin, P21/c, Z = 4, a = 1034,2(2) pm, b = 1521,2(3) pm, c = 2086,3(7) pm, β = 102,87(2)°, R1 = 0,0864, wR2 = 0,1196) wird von eindimensional-unendlichen Ketten längs [010] geprägt. In diesen sind Pr1 und Pr2 von insgesamt vier dreizähnig-überbrückenden Propionatgruppen, Pr1 zusätzlich von drei „Koordinationswasser“-Molekülen, Pr2 stattdessen von zwei zweizähnigen Propionatgruppen koordiniert. Daneben liegen drei „Kristallwasser“-Moleküle vor, so daß das Praseodympropionat-trihydrat gemäß [(H2O)3Pr1(CH3CH2COO)4Pr2(CH3CH2COO)2](H2O)3 formuliert werden sollte.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220220
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  • 8
    Electronic Resource
    Electronic Resource
    Ternäre Bromide und Iodide zweiwertiger Lanthanide und ihre Erdalkali-Analoga vom Typ AMX3 und AM2X5Professor Hanskarl Müller-Buschbaum zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 759-765 
    Details
    ISSN: 0044-2313
    Keywords: Metallothermic Reduction ; Lanthanides ; Alkaline Earth Metals ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Bromides and Iodides of Divalent Lanthanides and Their Alkaline-Earth Analoga of the Type AMX3 and AM2X5Metallothermic reduction of the tribromides and -iodides MX3 (M = Sm, Dy, Tm, Yb) with alkali metals as well as with indium and thallium (A = Cs, Rb, K, In, Tl) results in most cases in ternary compounds with the composition AMX3 and AM2X5, respectively. Analogous compounds with M = Ba, Sr, Ca were synthesized from the binary components. The AMX3 compounds crystallize with the following types of structure: the perovskite-type and its distorted variants, the NaNbO3-II- and the GdFeO3-type, the NH4CdCl3- and the stuffed PuBr3-type. These structure types differ by a gain of condensation of the [MX6] octahedra (three-dimensional connection via corners within the variants of the perovskite-type, double chains of edge- and face-connected octahedra within the NH4CdCl3-type, and layers of corner- and edge-connected octahedra within the stuffed PuBr3-type of structure). This comes along with a reduction of the coordination number of A+ from 12 (“ideal” perovskite) to 8 + 2 (GdFeO3-type), 9 (NH4CdCl3-type), and 8 (stuffed PuBr3-type). Thus, the A/[MX6] size ratio determines which AMX3 type of structure is adopted. If the M2+ ion is large enough, ternary compounds with the composition AM2X5 occur either in addition to the AMX3 compounds or exclusively. They crystallize with the TlPb2Cl5 type of structure (C.N.(M2+) = 7 and 8). All of the AMX3 and AM2X5 compounds are summarized in a structure field diagram.
    Notes: Die metallothermische Reduktion der Tribromide und -iodide MX3 (M = Sm, Dy, Tm, Yb) mit Alkalimetallen sowie mit Indium und Thallium (A = Cs, Rb, K, In, Tl) liefert überwiegend ternäre Verbindungen der Zusammensetzungen AMX3 bzw. AM2X5. Analoge Erdalkaliverbindungen (M = Ba, Sr, Ca) wurden aus den jeweiligen binären Komponenten dargestellt. Die Halogenide AMX3 kristallisieren im Perowskit-Typ und seinen Verzerrungsvarianten, dem NaNbO3-II-bzw. dem GdFeO3-Typ, sowie im NH4CdCl3- oder im aufgefüllten PuBr3-Typ. Diese Strukturtypen unterscheiden sich durch eine zunehmende Verknüpfung der [MX6]-Oktaeder (allseitige Eckenverknüpfung in den Perowskitvarianten, Doppelstränge aus kanten- und flächenverknüpften Oktaedern im NH4CdCl3-Typ und kanten- und eckenverknüpfte Oktaederschichten im aufgefüllten PuBr3-Typ). Sie geht mit einer Verkleinerung der Koordinationszahl des A+-Ions von 12 im idealen Perowskit über 8 + 2 (GdFeO3-Typ) und 9 (NH4CdCl3-Typ) auf 8 (aufgefüllter PuBr3-Typ) einher, so daß das A/[MX6]-Größenverhältnis ausschlaggebend dafür ist, welcher Strukturtyp für die Zusammensetzung AMX3 auftritt. Sind die M2+-Ionen groß genug, treten (zusätzlich oder ausschließlich) Verbindungen vom Typ AM2X5 auf, die im TlPb2Cl5-Typ kristallisieren (C.N.(M2+) = 7 und 8). Alle erhaltenen Verbindungen wurden in einem Strukturfelddiagramm zusammengefaßt.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220502
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  • 9
    Electronic Resource
    Electronic Resource
    Eine Strukturvariante zum NaErCl4/α-NiWO4-Typ für ternäre Selten-Erd-Chloride vom Typ NaMCl4: Synthese und Kristallstruktur von NaLuCl4Professor Wolfgang Jeitschko zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 785-789 
    Details
    ISSN: 0044-2313
    Keywords: Rare Earth Halides ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Structural Variant to the NaErCl4/α-NiWO4 Type for Ternary Rare-Earth Halides NaMCl4: Synthesis and Crystal Structure of NaLuCl4Single crystals of NaLuCl4 (orthorhombic, Pbcn (Nr. 60), Z = 4, a = 618.6(1) pm, b = 1 592.2(2) pm, c = 657.0(1) pm) were grown for the first time from the binary components using the Bridgman technique. The crystal structure may be derived from a hexagonally closest packing of Cl- spheres with one half of all octahedral sites occupied by the cations Na+ and Lu3+, respectively. The close relation of the structure to that of NaErCl4 (α-NiWO4) is discussed. NaScCl4 was found to be isotypic to NaLuCl4.
    Notes: Einkristalle von NaLuCl4 (orthorhombisch, Pbcn (Nr. 60), Z = 4, a = 618,6(1) pm, b = 1 592,2(2) pm, c = 657,0(1) pm) wurden erstmals nach dem Bridgman-Verfahren aus den binären Komponenten gezüchtet. Die Kristallstruktur läßt sich von einer hexagonal-dichtesten Kugelpackung von Cl--Ionen ableiten, in der die Hälfte aller Oktaederlücken mit den Kationen Na+ bzw. Lu3+ besetzt ist. Die enge Verwandtschaft der Struktur mit jener von NaErCl4 (α-NiWO4) wird diskutiert. Mit NaScCl4 konnte ein zweiter Vertreter dieses Strukturtyps dargestellt werden.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220506
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  • 10
    Electronic Resource
    Electronic Resource
    Kristallstrukturen von [TiF3(NPPh3)(HNPPh3)]2 und von HNPPh3Professor H.-G. von Schnering zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1091-1096 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato-Phosphaneimine Complex of Titanium ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures of [TiF3(NPPh3)(HNPPh3)]2 and of HNPPh3The phosphoraneiminato-phosphaneimine complex [TiF3(NPPh3)(HNPPh3)]2 was obtained by the reaction of TiF4 with Me3SiNPPh3 in boiling dichloromethane. It crystallizes from 1,2-dichloroethane as yellow crystals which include four molecules C2H4Cl2 per dimeric formula unit. Space group P21/n, Z = 2, structure solution with 7270 independent reflections, R = 0.060 for reflections with I 〉 2σ(I). Lattice dimensions at -50°C: a = 1417.5, b = 1896.9, c = 1586.6 pm, β = 101.22°. The compound forms centrosymmetric dimeric molecules via μ2-F bridges with TiF distances of 194.6 and 223.3 pm, the longer one being in trans-position to the N atom of the (NPPh3)- ligand. Its TiN bond length of 177.7 pm corresponds with a double bond. The TiN bond length of the HNPPh3 donor molecule of 213.4 pm is typical for a donor acceptor bond.According to the crystal structure determination the phosphaneimine HNPPh3 forms monomeric molecules without intermolecular hydrogen bridges with a PN bond length of 152.4 pm. Space group P21/c, Z = 4, structure solution with 3229 independent reflections, R = 0.062 for reflections with I 〉 2σ(I). Lattice dimensions at -70°C: a = 1460.4, b = 928.9, c = 1096.6 pm, β = 93.35°.
    Notes: Der Phosphaniminato-Phosphanimin-Komplex [TiF3(NPPh3)(HNPPh3)]2 wird aus TiF4 und Me3SiNPPh3 in siedendem Dichlormethan erhalten. Er kristallisiert aus 1,2-Dichlorethan als gelbe Kristalle unter Einschluß von vier Molekülen C2H4Cl2 pro dimere Formeleinheit. Raumgruppe P21/n, Z = 2, Strukturlösung mit 7270 unabhängigen Reflexen, R = 0,060 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -50°C: a = 1417,5; b = 1896,9; c = 1586,6 pm; β = 101,22°. Die Verbindung bildet zentrosymmetrische Dimere, in denen die Titanatome über μ2-F-Brücken mit TiF-Abständen von 194,6 und 223,3 pm verknüpft sind. Die lange Ti—F-Bindung befindet sich in trans-Position zum N-Atom des (NPPh3)--Liganden, dessen TiN-Bindung mit 177,7 pm einer Doppelbindung entspricht. Der vom HNPPh3-Liganden ausgehende Ti—N-Abstand beträgt 213,4 pm.Das Phosphanimin HNPPh3 bildet nach der Kristallstrukturanalyse monomere Moleküle mit einer PN-Bindungslänge von 152,4 pm ohne intermolekulare Wasserstoffbrücken. Raumgruppe P21/c, Z = 4, Strukturlösung mit 3229 unabhängigen Reflexen, R = 0,062 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -70°C: a = 1460,4; b = 928,9; c = 1096,6 pm; β = 93,35°.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220626
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