Synthese und Kristallstruktur des Dichloroselenonitren-Komplexes (PPh4)2[WCl5(NSeCl2)] / Synthesis and Crystal Structure of the Dichloro-selenonitrene Complex (PPh4)2[WCl5(NSeCl2)]

1992 ◽  
Vol 47 (3) ◽  
pp. 301-304 ◽  
Author(s):  
Stefan Vogler ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Structure Determination ◽  
Selenium Atom ◽  
Tungsten Atom ◽  
Chlorine Atoms ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Octahedral

The title compound has been prepared by the reaction o f [WCl4(NSeCl)]2 with PPh4Cl in CH2Cl2 solution. It forms red crystals, which were characterized by an X-ray structure determination. Space group P21/c, Z = 4, 3856 observed unique reflections, R = 0.073. Lattice dimensions at 25 °C: a = 2266.0(5), b = 1121.0(2), c = 2013.0(4) pm, β = 109.66(3)°. The structure consists o f PPh4+ ions and anions [WCl5(NSeCl2)]2-, in which the tungsten atom is surrounded in a distorted octahedral way by five chlorine atoms and by the nitrogen atom of the (NSeCl2)3- ligand. The W = N = SeCl2 group is characterized by WN and SeN double bonds; the selenium atom has a pseudo trigonal-bipyramidal coordination with the N atom and two lone pairs in equatorial and the chlorine atoms in axial positions.

Synthese und Kristallstruktur von N,N′-Bis(trimethylsilyl)benzamidinato-dichlorogold, Ph— C(NSiMe3)2AuCl2 / Synthesis and Crystal Structure of N,N′-Bis(trimethylsilyl)benzamidinato-dichlorogold, Ph — C(NSiMe3)2AuCl2

1989 ◽  
Vol 44 (9) ◽  
pp. 999-1002 ◽  
Author(s):  
Wolfgang Hiller ◽  
Joachim Strähle ◽  
Alfred Zinn ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Gold Atom ◽  
Chlorine Atoms ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Square Planar

Ph—C(NSiMe3)2AuCl2 has been prepared by the reaction of N,N,N′-tris(trimethylsilyl)-benzamidine with AuCl3 in CH2Cl2 suspension, forming orange-red crystals, which were characterized by an X-ray structure determination.Space group P21/n, Z = 4, 2358 observed independent reflexions, R = 0.028. Lattice dimensions (20°C): a = 695.9(3); b = 1576.1(3); c = 1830.9(3) pm; β = 94.27(3)°. The compound forms monomeric molecules, in which the gold atom is in a square planar arrangement of the two nitrogen atoms of the benzamidinato chelate (Au—N 201.6(7); 203.3(6) pm) and by two chlorine atoms (Au—Cl 227.9(3); 228.5(2) pm).

Über die Darstellung neuer spirocyclischer N,N′-Dimethylsulfamid-substituierter Phosphorverbindungen und Ν,N′-Dimethylsulfamid-verbrückter Diphosphorverbindungen / The Preparation of New Spirocyclic N,N′-Dimethylsulphamide-Substituted Phosphorus Compounds, and of Some N,N′-Dimethylsulphamide-Bridged Diphosphorus Compounds

1990 ◽  
Vol 45 (2) ◽  
pp. 175-183 ◽  
Author(s):  
Peter G. Jones ◽  
Anke Meyer ◽  
Reinhard Schmutzler
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Structure Determination ◽  
Sodium Azide ◽  
Mixed Valence ◽  
Spectroscopic Properties ◽  
Phosphorus Compounds ◽  
Molar Ratio ◽  
X Ray ◽  
Trigonal Bipyramidal

The reactions of 4-chloro-1,3,5,7-tetramethyl-2,2,6,6-tetraoxa-2,6-dithia-1,3,5,7-tetraaza-4λ5-phosphaspiro[3.3]heptane (1) with trimethylsilyl compounds and sodium azide led to a series of spirocyclic N,N′-dimethylsulphamide-substituted phosphoranes (2—5). The nature of the pentaaza-spirophosphorane (4) was confirmed by an X-ray crystal structure determination (C2/c, a = 991.8(4), b = 1185.6(6), c = 1224.9(5) pm,β = 108.64(3)°, Z = 4, R = 0.041 for 1065 unique observed reflections); a crystallographic twofold axis passes through phosphorus and the nitrogen atom of the NMe2 group. The geometry at phosphorus is to a good approximation trigonal bipyramidal. The azido-spirophosphorane (5) undergoes Staudinger-type reactions with phosphorus(III) compounds (PPh3, dppm) to form the mixed-valence phosphorus compounds 6—8. The reaction of N,N′-dimethylsulphamide or N,N′-dimethyl-N,N′-bis(trimethylsilyl)-sulphamide with dichlorophosphines RPCl2 (R = Me, Ph) in a molar ratio 1:2 leads to the formation of the acyclic N,N′-dimethylsulphamide-bridged diphosphorus compounds 9 and 10, respectively. The spectroscopic properties (and, for 4, the X-ray crystal structure) of the products are compared with those of analogous urea-bridged phosphorus compounds.

Synthese und Kristallstruktur des Amido-Palladats (PPh4)2[Pd2Cl4(NH2)2] · CH2Cl2 und des Benzamidin-Palladats PPh4{ [Ph– C(NH2)(NH)]PdCl3} · CH3CN / Synthesis and Crystal Structure of the Amido Palladate (PPh4)2[Pd2Cl4(NH2)2] · CH2Cl2 and of the Benzamidine Palladate PPh4{[Ph—C(NH2)(NH)]PdCl3} · CH3CN

1991 ◽  
Vol 46 (8) ◽  
pp. 992-998 ◽  
Author(s):  
Henning von Arnim ◽  
Werner Massa ◽  
Alfred Zinn ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Ir Spectroscopy ◽  
Acetonitrile Solution ◽  
Chlorine Atoms ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations ◽  
Hcl Gas

Orange crystals of (PPh4)2[Pd2Cl4(NH2)2] have been prepared by the reaction of (PPh4)2[Pd2Cl6] with N,N,N′-tris(trimethylsilyl)benzamidine in boiling acetonitrile in the presence of water, and orange brown crystals of PPh4{[Ph—C(NH2)(NH)]PdCl3} by the reaction of the amidinato complex PPh4[Ph—C(NSiMe3)2PdCl2] with HCl gas in acetonitrile solution. The complexes were characterized by IR spectroscopy as well as by X-ray structure determinations.(PPh4)2[Pd2Cl4(NH2)2] · CH2Cl2: Space group PĪ, Z = 1, 2784 observed unique reflections, R = 0.043. Lattice dimensions at —60 °C: a = 1053.3(4), b = 1081.1(4), c = 1249.2(4) pm, α = 102.90(2)°, β = 110.44(2)°, γ = 102.23(2)°. The compound consists of PPh4+ ions and centrosymmetric anions [Pd2Cl4(NH2)2]2- with bridging chlorine atoms and terminal amido groups.PPh4{[Ph—C(NH2)(NH)]PdCl3} -CH3CN: Space group C2/c, Z = 8, 1183 observed unique reflections, R = 0.033. Lattice dimensions at —60 °C: a = 3106.7(6), b = 1059.0(1), c = 1818.0(4) pm, β = 90.98(2)°. The compound consists of PPh4+ ions, [Ph—C(NH2)(NH)PdCl3]-ions, and included CH3CN molecules. In the anion the benzamidine ligand is bound via the nitrogen atom of the imido group.

scholarly journals Synthese und Kristallstruktur von [Ag(PhN3C6H4N3(H)Ph)]4, einem tetrameren Ag(I)-Komplex mit überbrückenden Bistriazenido-Liganden / Synthesis and Crystal Structure of [Ag(PhN3C6H4N3(H)Ph)]4, a Tetrameric Ag(I) Complex with Bridging Bistriazenido Ligands

1990 ◽  
Vol 45 (5) ◽  
pp. 689-694 ◽  
Author(s):  
Manfredo Hörner ◽  
Antônio Gilberto Pedroso ◽  
Carlos Roberto de Menezes Peixoto ◽  
Johannes Beck
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Coordination Sphere ◽  
Structure Determination ◽  
Silver Atom ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
Trigonal Bipyramidal ◽  
Silver Atoms ◽  
Distorted Trigonal Bipyramidal

[Ag(PhN3C6H4N3(H)Ph)]4 is obtained by the reaction of AgNO3 with [PhN3C6H4N3(H)Ph)]Na in tetrahydrofurane in form of brown crystals. The crystal structure determination (orthorhombic space group Pbcn, a = 1989.7(8), b = 1917.5(3), c = 1767.1(4) pm, Z = 4, 1784 reflections for 200 parameters, final R = 0.059) shows the complex to be isotypic to the previous described copper analogue. The complex is built of a rhombus of four silver atoms and four bridging bistriazenido units. One nitrogen atom of a neutral nitrogen chain completes the coordination sphere of each silver atom to a distorted trigonal bipyramidal environment of two other silver atoms and three nitrogen atoms. The Ag–Ag distances are in the range from 279.9 to 310.3 pm, the Ag–N distances from 217 to 236 pm.

scholarly journals Synthese und Kristallstruktur von [WCl3(N 3S2)(Pyridin)] / Synthesis and Crystal Structure of [WCl3(N3S2)(Pyridine)]

1986 ◽  
Vol 41 (6) ◽  
pp. 796 ◽  
Author(s):  
Heribert Wadle ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Crystal Data ◽  
Pyridine Ligand ◽  
Tungsten Atom ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral ◽  
In Trans ◽  
Moisture Sensitive

[WCl3(N3S2)(pyridine)] was obtained by the reaction of a mixture of S5N5[WCl4(N3S2)] and S4N3[WCl4(N3S2)] with pyridine in dichloromethane. It forms brown, moisture-sensitive crystal plates and was characterized by its IR spectrum and an X-ray crystal structure determination (1404 ob­served reflexions. R = 0.052). Crystal data: ortho­rhombic, space group Pbca. Z = 8, a = 708.3, b = 1275.4, c = 2628.6 pm. The tungsten atom has a distorted octahedral coordination and is part of a planar WN3S2 ring with WN bond lengths of 176 and 186 pm. The pyridine ligand (W−N 232 pm) is in trans position to the shorter WN bond.

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

1986 ◽  
Vol 41 (10) ◽  
pp. 1191-1195 ◽  
Author(s):  
Ute Patt-Siebel ◽  
Somluck Ruangsuttinarupap ◽  
Ulrich Müller ◽  
Jürgen Pebler ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Bond Angle ◽  
Mossbauer Spectrum ◽  
Monoclinic Space Group ◽  
Mössbauer Spectrum ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral

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.

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

Notizen: Eine neue bicyclische Zinn-Selen-Verbindung. Synthese und Kristallstruktur von [{Cp(CO)2Fe}3ClSn3Se4] / A New Bicyclic Tin Selenium Compound. Synthesis and Crystal Structure of [{Cp(CO)2Fe}3ClSn3Se4]

1993 ◽  
Vol 48 (7) ◽  
pp. 1009-1012 ◽  
Author(s):  
Kurt Merzweiler ◽  
Harald Kraus
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Selenium Compound ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Compound Synthesis

[{Cp(CO)2Fe}SnCl3] reacts with Na2Se in THF to form the compound [{Cp(CO)2Fe}3ClSn3Se4] 1. 1 crystallizes in the monoclinic space group P21/n with 4 formula units per unit cell. The lattice constants are α = 1435.2(7), b = 1124.4(4), c = 1972.7(12) pm, β = 94.59(4)°. According to the X-ray structure determination 1 contains a bicyclic Sn3Se4 framework.

Synthesis and Crystal Structure of [(CH2)6N4CH3]2[CoCl4]

2002 ◽  
Vol 55 (9) ◽  
pp. 561 ◽  
Author(s):  
W. Li ◽  
S.-L. Zheng ◽  
C.-R. Zhu ◽  
Y.-X. Tong ◽  
X.-M. Chen
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Hydrogen Bonds ◽  
Three Dimensional ◽  
Title Complex ◽  
Chlorine Atoms ◽  
Synthesis And Crystal Structure ◽  
Methylene Groups ◽  
Self Assembled ◽  
Hydrogen Bonded

The interesting three-dimensional hydrogen-bonded self-assembled network of [(CH2)6N4CH3]+ cations and [CoCl4]2– anions has been prepared and structurally characterized. In the title complex, the quaternization of one hexamethylenetetramine nitrogen atom has been trapped, and further stabilized by the large [CoCl4]2– anions, featuring C–H���Cl hydrogen bonds (3.497–3.709 �) between the methylene groups of [(CH2)6N4CH3]+ cations and the chlorine atoms of the [CoCl4]2– anions.

Multianvil High-Pressure Synthesis And Crystal Structure Of β-YbBO3

2001 ◽  
Vol 56 (8) ◽  
pp. 697-703 ◽  
Author(s):  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Title Compound ◽  
Variable Parameters ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Oxygen Coordination ◽  
Distorted Octahedral ◽  
Pressure Synthesis ◽  
Octahedral Oxygen

β-Ytterbium borate (β-YbBO3) was synthesized under high-pressure in a Walker-type multianvil apparatus at 2.2 GPa and 1400 °C. The title-compound crystallizes in the trigonal calcite structure, space group R3̄̄c. Single crystal X-ray data yielded a = 492.1(2), c = 1630.5(9) pm, wR2 = 0.0344 for 165 F2 values and 11 variable parameters. Within the trigonal planar BO3 groups the B-O distance is 137.8(4) pm. The ytterbium atoms have a slightly distorted octahedral oxygen coordination (Yb-O: 224.4(2) pm)

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