U. Patt‐Siebel scite author profile

et al. 1988

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

S₅N₅[SnCl₅(CH₃CN)]; Synthese, IR-Spektrum, ¹¹⁹Sn-Mößbauer-Spektrum und Kristallstruktur / S₅N₅[SnCl₅(CH₃CN)]; Synthesis, IR Spectrum , Mössbauer Spectrum and Crystal Structure

Ruangsuttinarupap

et al. 1986

S5N5[SnCl5(CH3CN)] is prepared by the reaction of SnCl2 with trithiazyl chloride in acetonitrile suspension. The compound is characterized by its IR spectrum, the 119Sn Mössbauer spectrum and by an X-ray crystal structure determination (1851 observed, independent reflexions, R = 0.024). S5N5[SnCl5(CH3CN)] crystallizes in the monoclinic space group P21/n with Z = 4 and the lattice dimensions a = 758.8; b = 1574.6; c = 1429.1 pm; β = 97.65°. The compound consists of planar S5N5® cations with the azulene-like structure, and anions [SnCl5(CH3CN)]e in which the tin atom has a distorted octahedral coordination. The bond angle Sn-N ≡ C (168°) is surprisingly small.

Die Kristallstruktur von [Cl₃PNPCl₃][VOCl₄]

Zinn

Zeitschrift anorg allge chemie

et al. 1990

Die Titelverbindung wurde aus VOCl3 und [Cl3PNPCl3]Cl in CH2Cl2 hergestellt und durch das IR‐Spektrum und eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe Pbca, Z = 8, 689 beobachtete unabhängige Reflexe, R = 10% (hoher R‐Wert wegen Verwachsung von zwei Kristallindividuen). Gitterabmessungen bei −72°C: a = 981,0(5), b = 1578,9(8), c = 1974(1) pm. Die Verbindung besteht aus Cl3PNPCl3+‐Ionen (Bindungswinkel PNP 138(2)°) und Anionen VOCl4− mit annähernd tetragonal‐pyramidaler Struktur (Bindungslänge VO = 161(2) pm; Bindungswinkel OVCl im Mittel 101,0(9)°).

Dichlorcyclopropenon als stabiler Komplexligand. Die Kristallstruktur von [NbOCl₃·OC₃Cl₂]₄ / Dichlorocyclopropenone as Stable Complex Ligand. The Crystal Structure of [NbOCl₃·OC₃Cl₂]₄

Thullen

et al. 1988

The reaction of tetrachlorocyclopropene with NbOCl3 yields NbCl5·OC3Cl2 (1); 1 is also formed by partial hydrolysis of C3Cl3+NbCl6- (2), which is prepared from C3Cl4 and NbCl5. [NbOCl3·OC3Cl2]4 (3) was obtained by hydrolysis of 1 in form of pale-yellow, moisture sensitive, non-explosive crystals, and characterized by its IR spectrum and an X-ray crystal structure determination (1871 independent observed reflexions, R = 0.048). Crystal data: space group P1̄. Z = 2. a = 993.7(4), b = 1090.5(5). c = 1097.4(3) pm, α = 69.51(3), β = 70.47(3), γ = 66.51(4)° (at -17 °C). 3 consists of centrosymmetrical tetramers; the four Nb atoms form a square and are linked via almost linear oxo groups with alternating short and long NbO bonds with mean bond lengths of 175 and 208 pm. In trans position of each of the short NbO bonds a dichlorocyclopropenone molecule is attached via its oxygen atom with an NbO distance of 223 pm.

PPh₃Me[MoBr₅(CH₃CN)]. IR‐Spektrum, magnetisches Verhalten und Kristallstruktur

Schmidt

Pebler

Zeitschrift anorg allge chemie

et al. 1987

Das aus Molybdäntetrabromid und Acetonitril gebildete MoBr4(CH3CN)2 reagiert mit Triphenylmethylphosphoniumbromid in Dibrommethan zu PPh3Me[MoBr5(CH3CN)]. Beide Addukte werden durch ihre IR‐Spektren charakterisiert. Die Auswertung der Messung der magnetischen Suszeptibilität von PPh3Me[MoBr5(CH3CN)] im Temperaturbereich von 4,2 bis 290 K ergibt die Curie‐Weiss‐Parameter μcw = 2,65 B.M. und Θ = −44 K. Die Kristallstruktur von PPh3Me[MoBr5(CH3CN)] wurde mittels Röntgenbeugung bestimmt (2426 beobachtete Reflexe, R = 8,2%). Kristalldaten: a = 1064,9, b = 2172,1, c = 1330,4 pm; β = 119,92º, Raumgruppe P21/c, Z = 4. Im Kristall sind PPh3Me+‐ und [MoBr5(CH3CN)]−‐Ionen abwechselnd zu Schichten senkrecht zu a gepackt. Im Anion ist das Mo‐Atom verzerrt oktaedrisch koordiniert. Der Bindungsabstand des Br‐Atoms in trans‐Stellung zum N‐Atom ist deutlich kürzer als die übrigen MoBr‐Abstände.