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  • 1
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen von (Ph4P)4[Bi8I28], (nBu4N)[Bi2I7] und (Et3PhN)2[Bi3I11] - Iodobismutate mit isolierten bzw. polymeren Anionen (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2049-2054 
    Details
    ISSN: 0044-2313
    Keywords: Iodobismuthate ; [Bi2I7]-, [Bi3I11]2-, [Bi8I28]4-, crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of (Ph4P)4[Bi8I28], (nBu4N)[Bi2I7], and (Et3PhN)2[Bi3I11] - Bismuth Iodo Complexes with Isolated and Polymeric AnionsSolutions of BiI3 in methanol react with NaI and (nBu4N)(PF6) or (Et3NPh)(PF6) to form anionic bismuth iodo complexes (nBu4N)[Bi2I7] 1 and (Et3PhN)2[Bi3I11] 2. In 1 Bi4I16 units, and in 2 Bi6I24 units are linked by common I-atoms to onedimensional infinite chains. Reaction of BiI3 with (Ph4P)(PF6) in methanol yields (Ph4P)4[Bi8I28] 3. The anions of 1-3 consist of edge-sharing BiI6 octahedra.(nBu4N)[Bi2I7] 1: Space group I2/m (No. 13), a = 1 082.3(5), b = 2 597.1(13), c = 1 206.1(6) pm, β = 93.17(2)°, V = 3 385(3) · 106 pm3;(Et3PhN)2[Bi3I11] 2: Space group P1 (No. 2), a = 1 283.5(6), b = 1 345.9(7), c = 1 546.3(8) pm, α = 83.87(2), β = 74.24(2), γ = 68.26(2)°, V = 2 388(2) · 106 pm3;(Ph4P)4[Bi8I28] 3: Space group P1 (No. 2), a = 1 329.3(4), b = 1 337.0(4), c = 2 193.1(5) pm, α = 104.20(2), β = 99.73(2), γ = 100.44(2)°, V = 3 622(2) · 106 pm3.
    Notes: BiI3 reagiert in methanolischer Lösung mit NaI und (nBu4N)(PF6) bzw. (Et3PhN)(PF6) zu (nBu4N)[Bi2I7] 1 und (Et3PhN)2[Bi3I11] 2 mit Iodobismutatanionen. In 1 liegen unendliche Stränge von über gemeinsame I-Atome verknüpften Bi4I16-Einheiten vor. In 2 bilden verkettete Bi6I24-Einheiten polymere Anionen. Führt man die Umsetzung von BiI3 mit (Ph4P)(PF6) ohne NaI durch, so kristallisiert aus Methanol (Ph4P)4[Bi8I28] 3. Die Anionen von 1-3 bestehen aus kantenverknüpften BiI6-Oktaedern.(nBu4N)[Bi2I7] 1: Raumgruppe I2/m (Nr. 13), a = 1 082,3(5), b = 2 597,1(13), c = 1 206,1(6) pm, β = 93,17(2)°, V = 3 385(3) · 106 pm3;(Et3PhN)2[Bi3I11] 2: Raumgruppe P1 (Nr. 2), a = 1 283,5(6), b = 1 345,9(7), c = 1 546,3(8) pm, α = 83,87(2), b = 74,24(2), γ = 68,26(2)°, V = 2 388(2) · 106 pm3;(Ph4P)4[Bi8I28] 3: Raumgruppe P1 (Nr. 2), a = 1 329,3(4), b = 1 337,0(4), c = 2 193,1(5) pm, α = 104,20(2), β = 99,73(2), γ = 100,44(2)°, V = 3 622(2) · 106 pm3.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956211212
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  • 2
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen kettenförmiger und netzartiger Iodoplumbate (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 259-263 
    Details
    ISSN: 0044-2313
    Keywords: Crystal structures ; iodoplumbate ; polynuclear complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of Polymeric Iodoplumbate Chains and NetsThe iodoplumbates (Me3N—C3H6—NMe3)3 [Pb3I9]2 (2) and (Me3N—C3H6—NMe3)2 [Pb3I10] (3) or (Me3N—C2H4—NMe3)2 [Pb3I10] (1), respectively, are formed in the reaction of PbI2 with NaI and (Me3N—C3H6—NMe3) (PF6)2 or (Me3N—C2H4—NMe3) (PF6)2 in DMF. The anions of 1 and 2 consist of Pb3I11 units sharing common I atoms to form infinite zigzagchains and nets. The polymeric anions in 3 contain chains of face- and edge-sharing PbI6 octahedra.(Me3N—C2H4—NMe3)2 [Pb3I10] (1): Space group P1 (No. 2), a = 950.66(6), b = 1341.2(1), c = 1899.7(2) pm, α = 103.646(8), β = 90.097(5), γ = 107.733(4)°, V = 2234.8(2) · 106 pm3; (Me3N—C3H6—NMe3)3 [Pb3I9]2 (2): Space group C2/c (No. 15), a = 2679.0(4), b = 950.3(2), c = 3090,0(3) pm, β = 90.84(1)°, V = 7866(2) · 106 pm3; (Me3N—C3H6—NMe3)2 [Pb3I10] (3): Space group C2/c (No. 15), a = 2290.5(4), b = 972.4(2), c = 2335.3(4) pm, β = 115.64(1)°, V = 9678(3) · 106 pm3.
    Notes: Die Iodoplumbate (Me3N—C2H4—NMe3)2[Pb3I10] (1) bzw. (Me3N—C3H6—NMe3)3[Pb3I9]2 (2) und (Me3N—C3H6—NMe3)2[Pb3I10] (3) bilden sich bei der Umsetzung von PbI2 mit NaI und (Me3N—C2H4—NMe3)(PF6)2 oder (Me3N—C3H6—NMe3)(PF6)2 in DMF. In 1 und 2 sind die Anionen aus Pb3I11-Einheiten aufgebaut, die über gemeinsame I-Atome zu polymeren Zickzackketten bzw. Netzen verknüpft sind. Die polymeren Anionen in 3 enhalten dagegen Ketten flächen- und kantenverknüpfter Pbl6-Oktaeder.(Me3N—C2H4—NMe3)2[Pb3I10] (1): Raumgruppe P1 (Nr. 2), a = 950,66(6), b = 1341,2(1), c = 1899,7(2) pm, α = 103,646(8), β = 90,097(5), γ = 107,733(4)°, V = 2234,8(2) ·106 pm3; (Me3N—C3H6—NMe3)3[Pb3I9]2 (2): Raumgruppe C2/c (Nr. 15), a = 2679,0(4), b = 950,3(2), c = 3090,0(3) pm, β = 90,84(1)°, V = 7866(2) · 106 pm3; (Me3N—C3H6—NMe3)2[Pb3I10] (3): Raumgruppe C2/c (Nr. 15), a = 2290,5(4), b = 972,4(2), c = 2335,3(4) pm, β = 115,64(1)°, V = 9678(3) · 106 pm3.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230142
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  • 3
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur des ionischen Tellurnitridchlorids [Te3N2Cl5(SbCl5)]+SbCl6- (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1375-1379 
    Details
    ISSN: 0044-2313
    Keywords: Tellurium Nitride Chloride ; Synthesis ; 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 the Ionic Tellurium Nitride Chloride[Te3N2Cl5(SbCl5)]+SbCl6-The title compound has been prepared by the reaction of Te2NCl5 with antimony pentachloride in CH2Cl2 suspension. It is characterized by IR spectroscopy and by a crystal structure determination. Space group P21/c, Z = 4, lattice dimensions at -70°C: a = 1535.6, b = 1259.5, c = 1572.4 pm, β = 109.30°, R = 0.031. The compound forms an ionic pair with the central group of a (TeNCl)2 molecule in which the tellurium atoms are linked by the nitrogen atoms to give a planar Te2N2 four-membered ring. One of the nitrogen atoms is coordinated by a TeCl3+ unit, the other one by an antimony pentachloride molecule. According to the IR spectra a structure like [Te2N2Cl2(TeCl4)2] is proposed for Te2NCl5.
    Notes: Die Titelverbindung wird durch Reaktion von Te2NCl5 mit Antimonpentachlorid in Dichlormethan hergestellt und durch das IR-Spektrum und eine Kristallstrukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, Gitterkonstanten bei -70°C: a = 1535,6; b = 1259,5; c = 1572,4 pm, β = 109,30°; R = 0,031. Die Verbindung bildet ein Ionenpaar, dessen Kation als zentrales Bauelement ein (TeNCl)2-Molekül enthält, in dem die Telluratome mit den Stickstoffatomen zu einem planaren Te2N2-Vierring verknüpft sind. Eines der N-Atome ist mit einem TeCl3+-Ion, das andere mit einem SbCl5-Molekül koordiniert. Aus dem Vergleich der IR-Spektren wird für Te2NCl5 eine Struktur gemäß [Te2N2Cl2(TeCl4)2] vorgeschlagen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230909
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  • 4
    Electronic Resource
    Electronic Resource
    [VCl3(NPPh3)(OPPh3)], ein Phosphaniminato-Komplex von Vanadium(IV) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1023-1026 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complex of Vanadium(IV) ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [VCl3(NPPh3)(OPPh3)], a Phosphorane Iminato Complex of Vanadium(IV)The title compound has been prepared from vanadium tetrachloride and Me3SiNPPh3 in the presence of OPPh3 in CCl4 solution, forming orange-red, moisture sensitive crystals, which were characterized by an X-ray structure determination. Space group Cc, Z = 4, 2 560 observed unique reflections, R = 0.049. Lattice dimensions at 0°C: a = 1 018(1), b = 1 826(2), c = 1 859(2) pm, β = 93.65(9)° [VCl3(NPPh3)(OPPh3)] forms monomeric molecules, in which the vanadium atom is coordinated in a distorted square pyramidal fashion with the (NPPh3)- ligand in apical position. The three chlorine atoms and the oxygen atom of the OPPh3 molecule occupy the basal positions. The phosphorane iminato group V=N=PPh3 is nearly linear (bond angle VNP 161.4°), the bond lengths VN (169 pm) and PN (162 pm) correspond with double bonds.
    Notes: Die Titelverbindung entsteht aus Vanadiumtetrachlorid und Me3SiNPPh3 in Gegenwart von Triphenylphosphanoxid in CCl4. Die orangeroten, feuchtigkeitsempfindlichen Kristalle wurden durch eine röntgenographische Strukturanalyse charakterisiert: Raumgruppe Cc, Z = 4, 2 560 beobachtete unabhängige Reflexe, R = 4,9%. Gitterabmessungen bei 0°C: a = 1 018(1), b = 1 826(2), c = 1 859(2) pm, β = 93,65(9)°. [VCl3(NPPh3)(OPPh3)] bildet monomere Moleküle, in denen das Vanadiumatom eine verzerrte tetragonale Pyramide bildet mit dem (NPPh3)--Liganden in der Apicalposition. Die drei Chloratome und das O-Atom des OPPh3-Moleküls sind äquatorial angeordnet. Die Phosphaniminatogruppe V=N=PPh3 ist mit 161,4° nahezu gestreckt, die Abstände VN und PN entsprechen mit 169 und 162 pm Doppelbindungen.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190612
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  • 5
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen von [Li(thf)4]2[Bi4I14(thf)2], [Li(thf)4]4[Bi5I19] und (Ph4P)4[Bi6I22] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1559-1564 
    Details
    ISSN: 0044-2313
    Keywords: Iodobismutate ; BiI3 ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of [Li(thf)4]2[Bi4I14(thf)2], [Li(thf)4]4[Bi5I19], and (Ph4P)4[Bi6I22]Solutions of BiI3 in THF or methanol react with MI (M = Li, Na) to form polynuclear iodo complexes of bismuth. The syntheses and results of X-ray structure analyses of compounds [Li(thf)4]2[Bi4I14(thf)2], [Li(thf)4]4[Bi5I19], [Na(thf)6]4[Bi6I22] and (Ph4P)4[Bi6I22] are described. The anions of these compounds consist of edge-sharing BiI6 and BiI5(thf) octahedra. The Bi atoms lie in a plane and are coordinated by bridging and terminal I atoms and by THF ligands in a distorted octahedral fashion.[Li(thf)4]2[Bi4I14(thf)2]: Space group P1 (No. 2), a = 1 159.9(6), b = 1 364.6(7), c = 1 426.5(7) pm, α = 114.05(3), β = 90.01(3), γ = 100.62(3)°.[Li(thf)4]4[Bi5I19]: Space group P21/n (No. 14), a = 1 653.0(9), b = 4 350(4), c = 1 836.3(13) pm, β = 114.70(4)°.[Na(thf)6]4[Bi6I22]: Space group P21/n (No. 14), a = 1 636.4(3), b = 2 926.7(7), c = 1 845.8(4) pm, β = 111.42(2)°.(Ph4P)4[Bi6I22]: Space group P1 (No. 2), a = 1 368.6(7), b = 1 508.1(9), c = 1 684.9(8) pm, α = 98.28(4), β = 95.13(4), γ = 109.48(4)°.
    Notes: Lösungen von BiI3 in THF oder Methanol reagieren mit MI (M = Li, Na) zu mehrkernigen Bismutiodokomplexen. Darstellung und Ergebnisse der Kristallstrukturanalyse von [Li(thf)4]2[Bi4I14(thf)2], [Li(thf)4]4[Bi5I19], [Na(thf)6]4[Bi6I22] und (Ph4P)4[Bi6I22] werden beschrieben. Die Anionen der vier Verbindungen bestehen aus kantenverknüpften BiI6- bzw. BiI5(thf)-Oktaedern. In diesen Verbindungen liegen die Bi-Atome in einer Ebene und werden verzerrt oktaedrisch von den verbrückenden und terminalen I-Atomen bzw. THF-Liganden koordiniert.[Li(thf)4]2[Bi4I14(thf)2]: Raumgruppe P1 (Nr. 2), a = 1 159,9(6), b = 1 364,6(7), c = 1 426,5(7) pm, α = 114,05(3), β = 90,01(3), γ = 100,62(3)°.[Li(thf)4]4[Bi5I19]: Raumgruppe P21/n (Nr. 14), a = 1 653,0(9), b = 4 350(4), c = 1 836,3(13) pm, β = 114,70(4)°.[Na(thf)6]4[Bi6I22]: Raumgruppe P21/n (Nr. 14), a = 1 636,4(3), b = 2 926,7(7), c = 1 845,8(4) pm, β = 111,42(2)°.(Ph4P)4[Bi6I22]: Raumgruppe P1 (Nr. 2), a = 1 368,6(7), b = 1 508,1(9), c = 1 684,9(8) pm, α = 98,28(4), β = 95,13(4), γ = 109,48(4)°.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200911
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  • 6
    Electronic Resource
    Electronic Resource
    Funktionalisierte Alkinkomplexe von Wolfram(VI). Synthese und Kristallstrukturen von [WCl4(Et—Se—C≡C—Se—Et)(THF)] und [WCl4(Et—Te—C≡C—Te—Et)(THF)]Professor Gerhard Fritz zum 75. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 388-392 
    Details
    ISSN: 0044-2313
    Keywords: Functionalized Alkyne Complexes of Tungsten ; Synthesis ; IR spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Functionalized Alkyne Complexes of Tungsten(VI). Syntheses and Crystal Structures of [WCl4(Et—Se—C≡C—Se—Et)(THF)] and [WCl4(Et—Te—C≡C—Te—Et)(THF)]The title compounds have been prepared by reactions of [WCl4(SEt2)2] with the alkynes Et—X—C≡C—X—Et (X = Se, Te) in CCl4 solution and subsequent addition of tetrahydrofurane. Both complexes were characterized by crystal structure determinations.[WCl4(Et—Se—C≡C—Se—Et)(THF)]: Space group P21/n, Z = 4, structure determination with 2942 unique reflections, R = 0.038. Lattice dimensions at 20°C: a = 934.2, b = 1639.5, c = 1189.5 pm, β = 96.497°.[WCl4(Et—Te—C≡C—Te—Et)(THF)]: Space group P21/n, Z = 4, structure determination with 4097 unique reflections, R = 0.067, Lattice dimensions at -70°C: a = 899.2, b = 1691.9, c = 1213.3 pm, β = 96.82°.The complexes have monomeric molecular structures with the oxygen atom of the THF molecules in trans-position to the side-on bound alkyne ligands.
    Notes: Die Titelverbindungen werden aus [WCl4(SEt2)2] und den Alkinen Et—X—C≡C—X—Et (X = Se, Te) in CCl4-Lösung nach Zusatz von Tetrahydrofuran erhalten und durch Kristallstrukturanalysen charakterisiert.[WCl4(Et—Se—C≡C—Se—Et)(THF)]: Raumgruppe P21/n, Z = 4, Strukturverfeinerung mit 2942 unabhängigen Reflexen, R = 0,038. Gitterabmessungen bei 20°C: a = 934,2; b = 1639,5; c = 1189,5 pm, β = 96,497°.[WCl4(Et—Te—C≡C—Te—Et)(THF)]: Raumgruppe P21/n, Z = 4, Strukturverfeinerung mit 4097 unabhängigen Reflexen, R = 0,067. Gitterabmessungen bei -70°C: a = 899,2; b = 1691,9; c = 1213,3 pm, β = 96,82°.Beide Verbindungen haben monomere Molekülstrukturen, in denen sich das O-Atom des THF-Moleküls in trans-Position zum seitlich gebundenen Alkinliganden befindet.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210308
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  • 7
    Electronic Resource
    Electronic Resource
    Iodoplumbate mit polymeren Anionen - Synthese und Kristallstrukturen von [Na3(OCMe2)12][Pb4I11(OCMe2)], (Ph4P)2[Pb5I12] und (Ph4P)4[Pb15I34(dmf)6] (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1781-1787 
    Details
    ISSN: 0044-2313
    Keywords: Crystal structures ; iodoplumbate ; polynuclear complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Iodoplumbates with Polymeric Anions - Synthesis and Crystal Structures of [Na3(OCMe2)12][Pb4I11(OCMe2)], (Ph4P)2[Pb5I12], and (Ph4P)4[Pb15I34(dmf)6]Reactions of PbI2 with NaI in polar organic solvents followed by crystallization with large cations yield iodoplumbate complexes with various compositions and structures. [Na3(OCMe2)12][Pb4I11(OCMe2)] 3, (Ph4P)2[Pb5I12] 4 and (Ph4P)4[Pb15I34(dmf)6] 7 contain one-dimensional infinite anionic chains of face- or edge-sharing PbI6 or PbI5L (L = acetone, DMF) octahedra.[Na3(OCMe2)12][Pb4I11(OCMe2)] 3: Space group P1 (No. 1), a = 1120.3(5), b = 1265.3(6), c = 1608.3(8) pm, α = 74.64(4), β = 70.40(4), γ = 85.24(4)°, V = 2071(2) · 106 pm3;(Ph4P)2[Pb5I12] 4: Space group C2/c (No. 15), a = 787.00(10), b = 2812.0(5), c = 3115.9(5) pm, β = 96.240(13)°, V = 6885(2) · 106 pm3;(Ph4P)4[Pb15I34(dmf)6] 7: Space group P21/n (No. 14), a = 2278.8(4), b = 1782.6(3), c = 2616.8(4) pm, β = 114.432(13)°, V = 9678(3) · 106 pm3.
    Notes: Bei Umsetzungen von PbI2 mit NaI in polaren organischen Lösungsmitteln entstehen Iodoplumbatkomplexe unterschiedlicher Zusammensetzungen und Strukturen, die durch Kristallisation mit großen Kationen isoliert werden können.[Na3(OCMe2)12][Pb4I11(OCMe2)] 3, (Ph4P)2[Pb5I12] 4 und (Ph4P)4[Pb15I34(dmf)6] 7 enthalten eindimensional unendliche Anionen, die aus flächen- bzw. kantenverknüpften PbI6- oder PbI5L-Oktaedern (L = Aceton, DMF) aufgebaut sind.[Na3(OCMe2)12][Pb4I11(OCMe2)] 3: Raumgruppe P1 (Nr. 1), a = 1120,3(5), b = 1265,3(6), c = 1608,3(8) pm, α = 74,64(4), β = 70,40(4), γ = 85,24(4)°, V = 2071(2) · 106 pm3;(Ph4P)2[Pb5I12] 4: Raumgruppe C2/c (Nr. 15), a = 787,00(10), b = 2812,0(5), c = 3115,9(5) pm, β = 96,240(13)°, V = 6885(2) · 106 pm3;(Ph4P)4[Pb15I34(dmf)6] 7: Raumgruppe P21/n (Nr. 14), a = 2278,8(4), b = 1782,6(3), c = 2616,8(4) pm, α = 114,432(13)°, V = 9678(3) · 106 pm3.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966221024
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