Synthese und Kristallstruktur neuer 1,1,1,3,3,3-Hexaamino-1λ5,3λ5- diphosphazenium-Salze/ Synthesis and Crystal Structure of Novel 1,1,1,3,3,3-Hexaamino-1λ5,3λ5- diphosphazenium Salts

1999 ◽  
Vol 54 (11) ◽  
pp. 1363-1370 ◽  
Author(s):  
Kai Landskron ◽  
Wolfgang Schnick
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Temperature Gradient ◽  
Single Crystals ◽  
Room Temperature ◽  
Gauche Conformation ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Acetonitrile Solutions ◽  
Ray Methods

1,1,1,3,3,3-Hexaamino-1λ5,3λ5-diphosphazenium bromide [(NH2)3PNP(NH2)3]Br, nitrate [(NH2)3PNP(NH2)3][NO3], and toluene-4-sulfonate [(NH2)3PNP(NH2)3][CH3C6H4SO3] have been prepared by anion exchange in aqueous solution. Single crystals were obtained from acetonitrile solutions in a temperature gradient between 60 °C and room temperature. The crystal structures were determined by single crystal X-ray methods at room temperature. ([(NH2)3PNP(NH2)3]Br: P1̄̄ , Z = 2, a = 596.2( 1 ),b = 744.5( 1), c = 1114.4( 1) pm, α = 108.78( 1), β = 104.18(1), γ = 90.64(1)°, R 1 = 0.048, wR2 = 0.104; [(NH2)3PNP(NH2)3][NO3]: P1̄̄, Z = 2, a = 550.9( 1), b = 796.3( 1), c = 1115.7( 1) pm, α = 94.45( 1), β= 99.55( 1), γ = 101,53( 1)°, R1 = 0.033, wR2 = 0.095; [(NH2)3PNP(NH2)3][CH3C6H4SO3]: P21/c, Z = 4, a = 804.1(1), b = 596.1(1), c = 3218.7(3) pm, β = 94.59(1)°, R1 = 0.052, wR2 = 0.136). In the solid the three salts consist of discrete [(NH2)3PNP(NH2)3]+ cations and their corresponding anions. The PN4 tetrahedra in [(NH2)3PNP(NH2)3]Br are staggered, while in [(NH2)3PNP(NH2)3][NO3] the eclipsed conformation is preferred. The PN4 tetrahedra of [(NH2)3PNP(NH2)3][CH3C6H4SO3] show gauche conformation.

Synthese, Kristallstruktur und Eigenschaften von 1,1,1,3,3, 3 - Hexaamino - 1λ5,3λ5-diphosphazeniumehlorid [(NH2)3PNP(NH2)3]Cl / Synthesis, Crystal Structure, and Properties of 1,1,1,3,3,3-Hexaamino- 1λ5 ,3λ5-diphosphazenium Chloride [(NH2)3 PNP(NH2)3 ]Cl

1996 ◽  
Vol 51 (12) ◽  
pp. 1732-1738 ◽  
Author(s):  
Stefan Horstmann ◽  
Wolfgang Schnick
Keyword(s):  
Crystal Structure ◽  
Phase Transition ◽  
Temperature Gradient ◽  
Single Crystal ◽  
Single Crystals ◽  
Room Temperature ◽  
Acetonitrile Solution ◽  
Structure And Properties ◽  
X Ray ◽  
Ray Methods

[(NH2)3PNP(NH2)3]Cl has been prepared by a three step synthesis. The last step is the ammonolysis of [Cl3PNPCl3]Cl. Single crystals of 1,1,1,3,3,3-hexaamino-1λ5, 3λ5-diphosphazenium chloride were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. Between room temperature and -100 °C [(NH2)3PNP(NH2)3]Cl is subject to a phase transition. Therefore, the crystal structure was determined by single crystal X-ray methods at room temperature (P1̄, a = 584.7(1) pm, b = 732.1(1) pm, c = 1092.0(2) pm. q = 71.05(3)°, β = 76.36(3)°, γ = 89.83(3)°, Z = 2, R = 4.75 %, wR = 2.47 %). The cation [(NH2)3PNP(NH2)3]+ is built up by two corner sharing PN4 tetrahedra. Remarkably short P-N bonding distances have been observed and both PN4 tetrahedra exhibit a significant distortion resulting in two large and four small N-P-N bond angles.

Synthese und Kristallstruktur des Komplexsalzes [Au(tBu2PH)2][HCl2] / Synthesis and Crystal Structure of the Complex Salt [Au(tBu2PH)2][HCl2]

2012 ◽  
Vol 67 (6) ◽  
pp. 543-548 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Peter Mayer ◽  
Hubert Schmidbaur
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Room Temperature ◽  
Complex Salt ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Large Complex

The synthesis and the characterization of the complex salt [Au(tBu2PH)2][HCl2] (2) resulting from the reaction of hydrogen tetrachloridoaurate(III) hydrate with tBu2PH in dichloromethane at room temperature is reported. Single crystals of 2 have been analyzed by X-ray crystallography: monoclinic, P21=c, Z = 12, a = 12:0805(3), b = 12:3729(4), c = 46:7506(13) Å ; ß = 90:948(2)°; V = 6986:9(3) Å3; T = 173(2) K. The hydrogen bihalide anions [HCl2]- fill the interstices between the large complex cations [Au(tBu2PH)2]+ in the crystal.

Synthese und Kristallstruktur von [(Cl3Si)2N]2TiCl2 -ein perchloriertes N-Silyl-titanamid /Synthesis and Crystal Structure of [(Cl3Si)2N]2TiCl2 -a Fully Chlorinated N-Silyl Titanium Amide

1997 ◽  
Vol 52 (7) ◽  
pp. 819-822 ◽  
Author(s):  
Bernd Schwarze ◽  
Wolfgang Milius ◽  
Wolfgang Schnick
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Room Temperature ◽  
Titanium Atom ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ray Methods ◽  
Cl Atoms

Abstract The chlorinated titanium amides [(Cl3Si)2N]2TiCl2 (1) and (Cl3Si)2NTiCl3 have been syn­thesized selectively from hexachlorodisilazane lithium and TiCl4. The crystal structure of 1 was determined by single crystal X-ray methods at room temperature (P212121, a = 1232.4(2), b = 1265.5(2), c -1469.1(2) pm, Z = 4). The central titanium atom of 1 is bound to two nitrogen atoms and two Cl atoms and is weakly coordinated further by two Cl atoms of the trichlorosilyl groups.

Neue Tetraaminophosphonium-Salze durch Anionenaustausch in flüssigem Ammoniak

1999 ◽  
Vol 54 (8) ◽  
pp. 1019-1026 ◽  
Author(s):  
Kai Landskron ◽  
Stefan Horstmann ◽  
Wolfgang Schnick
Keyword(s):  
Complex System ◽  
Temperature Gradient ◽  
Hydrogen Bonds ◽  
Single Crystals ◽  
Room Temperature ◽  
Liquid Ammonia ◽  
Acetonitrile Solution ◽  
X Ray ◽  
Cscl Type ◽  
Ray Methods

[P(NH2)4]Br and [P(NH2)4][NO3] have been prepared by anion exchange in liquid ammonia. Single crystals of [P(NH2)4]Br were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature while attempts to grow single crystals of [P(NH2)4][NO3] yielded [P(NH2)4][NO3](OP(NH2)3). Both crystal structures were determined by single crystal X-ray methods at room temperature ([P(NH2)4]Br: P4/nbm, a = 809.2(1), c = 468.1(1) pm, Z = 2, R1 = 0.042, wR2 = 0.077; [P(NH2)4][NO3](OP(NH2)3): Pna21, Z = 4, a = 1023.4(1), b = 1704.7(1), c = 618.0(1) pm, R1 =0.025, wR2 = 0.067. In the solid [P(NH2)4]Br forms a tetragonally distorted variant of the CsCl type of structure. [P(NH2)4][NO3](OP(NH2)3) consists of [P(NH2)4]+cations, [NO3]- anions, and OP(NH2)3 molecules which are interconnected by a complex system of hydrogen bonds.

Synthese und Kristallstruktur von [H2NMe2]+[(Me2NH)2 TiCl4]-/Synthesis and Crystal Structure of [H2NMe2]+[(Me2NH)2TiCl4]-

1998 ◽  
Vol 53 (2) ◽  
pp. 239-241 ◽  
Author(s):  
Regina Bettenhausen ◽  
Wolfgang Milius ◽  
Wolfgang Schnick
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Room Temperature ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ionic Salt ◽  
Ray Methods ◽  
Cl Atoms

Abstract The title compound has been synthesized as a green solid by the reaction of MeCl2 SiNHSiMe3 and Ti(NMe2)4 in CH2Cl2. The crystal structure was determined by single crystal X-ray methods at room temperature (C2/c, a = 1825,7(4), b = 909,9(2), c = 1116,1(2) pm, β = 125,09(3)°, Z = 4,R1= 0,047, wR2 = 0,147) to be an ionic salt [H2NMe2]+[(Me2NH)2TiCl4]- . The central titanium(III) atom of the anion is bound to four Cl atoms and weakly coordinated by two Me2NH ligands.

Über die Kristallstruktur von KSc2 F7 / The Crystal Structure of KSc2 F7

1985 ◽  
Vol 40 (6) ◽  
pp. 726-729 ◽  
Author(s):  
Klaus Güde ◽  
Christoph Hebecker
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Unit Cell ◽  
Space Group ◽  
X Ray ◽  
Monoclinic Unit Cell ◽  
R Value ◽  
Ray Methods

Abstract Single crystals of KSc2F7 have been prepared from a mixture of KF and ScF3 . The samples were investigated by X-ray methods. KSc2F7 crystallizes orthorhombically with a = 10.643(2), b = 6.540(1), c = 4.030(1) Å. These data indicate a close crystallographic connection to the monoclinic unit cell of KIn2F7 [1], But in contrast to KIn2F7 , KSc2 F7 crystallizes in space group No. 65. Cmmm - D192h. The R-value for 341 observed independent reflections is 0.060.

Synthese und Kristallstruktur von [VCl2(15-Krone-5)]+[VOCl4]- / Synthesis and Crystal Structure of [VCl2(15-Crown-5)]+[VOCl4]-

1990 ◽  
Vol 45 (10) ◽  
pp. 1393-1397 ◽  
Author(s):  
Gerlinde Frenzen ◽  
Werner Massa ◽  
Thilo Ernst ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Crown Ether ◽  
Single Crystals ◽  
Structure Determination ◽  
Acetonitrile Solution ◽  
Tetragonal Symmetry ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ether Molecule

[VCl2(15-crown-5)]+[VOCl4]- has been prepared by the reaction of VCl4 with 15-crown-5 in acetonitrile solution in the presence of water, forming black-brown single crystals. They were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1530 observed unique reflexions, R = 0.052. Lattice dimensions at -120°C: a = 1128.5(4), b = 1063.3(3), c = 1680(1) pm. The compound forms ions, in which the cation contains vanadium(+III), which is seven coordinate by the five oxygen atoms of the crown ether molecule and by two chlorine atoms in axial positions of a pentagonal bipyramide. The [VOCl4]- anion contains vanadium (+V) with approximately tetragonal symmetry

Die Kristallstruktur von SrHg(SeCN)4 · 4 Pyridin / The Crystal Structure of SrHg(SeCN)4 · 4 Pyridine

1984 ◽  
Vol 39 (5) ◽  
pp. 582-585 ◽  
Author(s):  
Klaus Brodersen ◽  
Manfred Cygan ◽  
Hans-Ulrich Hummel
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Experimental Error ◽  
Space Group ◽  
X Ray ◽  
Ray Methods

Single crystals of SrHg(SeCN)4 · 4 pyridine are prepared by reaction of K2Hg(SeCN)4 with SrCl2 in CH3OH/C2H5OH in the presence of pyridine.The crystal structure was solved with X-ray methods (Mr = 1024.1, space group P4̄n2, Z = 2, a = 9.552(2) Å, c = 17.610(7) Å, V = 1606.7 Å3, λ(AgKα) = 0.5583 Å, dc = 2.12 g cm-3, μ(AgKα) = 57.40 cm-1, F(000) = 943.7, T = 298 K. Final R = 0.043 for 1050 independent reflections).The structure consists of nearly tetrahedral Hg(SeCN)4-units. The SeCN-group is linear within the experimental error. The N-atoms of SeCN and pyridine contribute to the Archimedean antiprismatic coordination of strontium

Über das Erdalkalimetall-Lanthanoid-Kupfer-Oxomolybdat (Cu0,22Mg0 ,78)BaNd2Mo4O16/The Alkaline Earth Rare Earth Copper-Oxomolybdate (Cu0.22Mg0.78)BaNd2Mo4O16

1995 ◽  
Vol 50 (4) ◽  
pp. 577-580 ◽  
Author(s):  
H. Szillat ◽  
Hk. Müller-Buschbaum
Keyword(s):  
Crystal Structure ◽  
Rare Earth ◽  
Single Crystals ◽  
Alkaline Earth ◽  
Three Dimensional ◽  
Space Group ◽  
X Ray ◽  
Ray Methods

Single crystals of (Cu0.22Mg0.78)BaNd2Mo4O16 have been prepared by crystallization from melts and investigated by X-ray methods. The compound crystallizes monoclinically, space group C62h - C12/c1, Z = 4, a = 5.351(1), b = 12.891(2), c = 19.391(4) Å,β = 90.899(14)° and is isotypic to CuKHo2Mo4O16. The crystal structure is dominated by BaO10 and NdO8 polyhedra forming a three-dimensional polyhedra network, which is filled by axially distorted (Cu,Mg)O6 octahedra and MoO4 tetrahedra.

The Vibrational Spectra and Crystal Structure of Acenaphthylene

1973 ◽  
Vol 51 (3) ◽  
pp. 402-404 ◽  
Author(s):  
A. Bree ◽  
R. A. Kydd ◽  
V. V. B. Vilkos ◽  
R. S. Williams
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Raman Spectra ◽  
Vibrational Spectra ◽  
Room Temperature ◽  
Infrared And Raman Spectra ◽  
Depolarization Ratio ◽  
X Ray

A study of the polarized infrared and Raman spectra of acenaphthylene single crystals has been made. These results, together with Gordon and Yang's preliminary X-ray work, suggest that the molecules pack in some disordered arrangement in the solid at room temperature. Most of the A1 fundamentals were identified in the Raman solution spectrum from their low depolarization ratio, and a few tentative assignments of nontotally symmetric fundamentals were made.

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