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.

Synthese und Kristallstruktur von [N(PPh3)2][VCl3(N3S2)]·C7H8 / Synthesis and Crystal Structure of [N(PPh3)2][VCl3(N3S2)]·C7H8

1987 ◽  
Vol 42 (4) ◽  
pp. 410-414 ◽  
Author(s):  
Aida El-Kholi ◽  
Ruth Christophersen ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Subsequent Treatment ◽  
Vanadium Atom ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Chlorine Atoms ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

Abstract [N(PPh3)2][VCl3(N3S2)]·C7H8 is formed by the reaction of VCl2 (N3S2) with excess PPh3 in CH2C12 and subsequent treatment of the reaction mixture with toluene, as well as by the reaction of VCl2(N3S2) with [N(PPh3)2]Cl in CH2Cl2 in the presence of toluene. The compound forms red crystals, which have been characterized by IR spectroscopy. The crystal structure was determined by X-ray diffraction (1433 observed, independent reflexions, R = 0.070). Crystal data: mono-clinic, space group Cc, Z = 4, a = 994.1, b = 2148.0, c = 2055.2 pm, β = 90.03°. The compound consists of [N(PPh3)2]⊕ cations and [VCl3(N3S2)]⊖ anions, in which the vanadium atom is five-coordinated by threee chlorine atoms and two nitrogen atoms, and is part of a planar VN3S2 ring.

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 [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

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).

Notizen: Synthese und Kristallstruktur von [OsCl4(CH3CN)2] · 1/2 CH3CN / Synthesis and Crystal Structure of [OsCl4(CH3CN)2] · 1/2CH3CN

1990 ◽  
Vol 45 (8) ◽  
pp. 1210-1212 ◽  
Author(s):  
Dieter Fenske ◽  
Gerhard Baum ◽  
Hans-Walter Swidersky ◽  
Kurt Dehnicke
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Room Temperature ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Slow Reaction ◽  
Moisture Sensitive

[OsCl4(CH3CN)2] · 1/2CH3CN has been prepared by the reaction of OsCl5 with acetonitrile in a slow reaction at room temperature, forming red, moisture sensitive crystals. The compound was characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1281 observed unique reflexions, R = 0.031. Lattice dimensions at 20 °C: a = 1032.5(5), b = 1356.0(7), c = 975.9(5) pm. The complex has a molecular structure, in which the osmium atom is octahedrally coordinated by four chlorine atoms and by two N-atoms of the ciscoordinated acetonitrile molecules. The included CH3CN molecules are disordered in two positions.

Ionische Phosphaniminato-Komplexe von Schwefel(IV) und Selen(IV ). Die Kristallstrukturen von [S(NPMe3)3]Cl · CH2Cl2, [S(N PPh3)3]S4N5 und [Se(NPMe3)3]Cl · C7H8 / Ionic Phosphorane Iminato Complexes of Sulfur(IV) and Selenium(IV). Crystal Structures of [S(NPMe3)3]Cl ·CH2Cl2, [S(NPPh3)3]S4N5 and [Se(NPMe3)3]Cl · C7H8

1995 ◽  
Vol 50 (10) ◽  
pp. 1455-1463 ◽  
Author(s):  
Frank Kunkel ◽  
Hella Folkerts ◽  
Sigrid Wocadlo ◽  
Hak-Chul Kang ◽  
Werner Massa ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Formula Unit ◽  
Selenium Compound ◽  
Space Group ◽  
Sulfur Dichloride ◽  
Structure Determinations ◽  
Moisture Sensitive

[S(NPMe3)3]Cl · CH2C12 and [S(NPPh3)3]S4N5 were prepared by the reaction of Me3SiNPMe3 or Me3SiNPPh3 with sulfur dichloride and S3N2Cl2, respectively, in CH2Cl2 solutions as colourless, moisture sensitive crystals. The corresponding selenium compound was prepared from SeCl4 and Me3SiNPMe3 in acetonitrile solution; it crystallizes from toluene solutions with one mole of toluene per formula unit. All complexes have been characterized by IR spectroscopy and by crystal structure determinations.[S(NPMe3)3]Cl-CH2Cl2: Space group Pna21, Z = 8 , 3930 observed unique reflections, R = 0.033. Lattice dimensions at -120 °C: a = 1200.9(1), b = 1020.2(1), c = 1790.5(1) pm.[S(NPPh3)3]S4N5: Space group P63, Z = 2, 2586 observed unique reflections, R = 0.054. Lattice dimensions at -100 °C: a = b = 1334.7(2), c = 1652.6(2) pm.[Se(NPMe3)3]Cl · C7H8: Space group C2/c, Z = 8 , 1475 observed unique reflections, R = 0.059. Lattice dimensions at -40 °C: a = 1853.6(8), b = 1159.2(4), c = 2053.2(4) pm. β = 101.92(3)°.All compounds contain cations [E(NPR3)3]+ (E = S, Se) with pyramidal structures. Bond lengths and bond angles are in average: S-N 162.5 pm, S-N-P 120.5° (R = Me), S-N 161.8 pm, S-N-P 119.2° (R = Ph), Se-N 177.8 pm, Se-N-P 120.3°.

Synthesis and Crystal Structure of [Cu2(OAc)4(NCMe)2] · 2MeCN

1998 ◽  
Vol 53 (7) ◽  
pp. 774-776 ◽  
Author(s):  
Mitra Ghassemzadeh ◽  
Kioumars Aghapoor ◽  
Bernhard Neumiiller
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Structural Data ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Centrosymmetric Dimers

T etrakis-μ-acetato-bis(acetonitrile-N )-dicopper( II) bisacetonitrile (1) was syn thesized and characterized by IR spectroscopy and by an X-ray structure determination [Space group P21/n, Z = 2, lattice dimensions at - 70 °C: a = 1064.2(1), b = 1018.4(1), c = 1088.3(1) pm, β = 101.59(1)°, R1 = 0.048]. A ccording to the structural data the blue compound consists of centrosymmetric dimers [Cu2(OAc)4(NCMe)2] and noncoordinated acetonitrile molecules.

Synthese und Kristallstruktur von (PPh4)4[Cu2Se14] / Synthesis and Crystal Structure of (PPh4)4[Cu2Se14]

1990 ◽  
Vol 45 (8) ◽  
pp. 1128-1132 ◽  
Author(s):  
Ulrich Müller ◽  
My-Linh Ha-Eierdanz ◽  
Gertrud Kräuter ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
The Other ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

(PPh4)4[Cu2Se14] has been prepared by the reaction of a lithium polyselenide solution in DMF with CuCl at 120 °C in the presence of PPh4Br. The compound forms black crystals, which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P 21, Z = 2, 2690 observed unique reflexions, R = 0.095. Lattice dimensions at 19 °C: a = 2139.5(9), b = 1611.7(3), c = 1365.1(3) pm, β = 93.54(3)°. The compound consists of PPh4+ and [Cu2Se14]4- ions, in which the two copper atoms are bridged by an Se52- chain. One of the Cu atoms is a member of a CuSe4 ring, the other one of a CuSe5 ring; the coordination at each Cu atom is trigonal-planar.

Komplexe mit dem (NSeMe)2--Liganden. Die Kristallstruktur von [PPh3Me][Cl5W(NSeMe)] / Complexes with the Ligand (NSeMe)2-. The Crystal Structure of [PPh3Me][Cl5W(NSeMe)]

1990 ◽  
Vol 45 (4) ◽  
pp. 427-432 ◽  
Author(s):  
Dieter Fenske ◽  
Andreas Frankenau ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Ir Spectroscopy ◽  
Chlorine Atoms ◽  
Space Group ◽  
Bond Angles ◽  
Bond Lengths ◽  
Moisture Sensitive

[CH3CN—WCl4(NSeMe)] and [PPh3Me][Cl5W(NSeMe)] have been prepared by the reaction of Me3SiSeMe with [CH3CN—WCl4(NCl)] and [PPh3Me][WCl5(NCl)], respectively, as brown, moisture sensitive crystals which were characterized by IR spectroscopy. The crystal structure of [PPh3Me][Cl5W(NSeMe)] was determined: Space group PĪ, Z = 4, 7599 observed unique reflexions, R = 0.046. Lattice dimensions at —70°C: α = 1104.6(6), b = 1489.2(9), c = 1650.6(8) pm, α = 108.37(4)°, β = 90.71(4)°, γ = 93.83(4)°. The compound forms ions [PPh3Me]+ and [Cl5W(NSeMe)]-, in which the tungsten atoms is octahedrally coordinated by five chlorine atoms and by the nitrogen atom of the (NSeMe)2- ligand. The bond lengths WN 171.6(8), NSe 180.6(9) pm and bond angles WNSe 173.6(7)°, NSeC 98.3(5)° (in average of the two independent anions) are in agreement with the proposed formula W ≡ N—Se—Me ↔W = N = Se—Me.

Die isoelektronischen Molekülkomplexe TiCl3(NPPh3) und TiCl3(OSiPh3) / The Isoelectronic Molecular Complexes TiCl3(NPPh3) and TiCl3(OSiPh3)

1994 ◽  
Vol 49 (1) ◽  
pp. 15-20 ◽  
Author(s):  
Thilo Rübenstahl ◽  
Dorothea Wolff von Gudenberg ◽  
Frank Weller ◽  
Kurt Dehnicke ◽  
Helmut Goesmann
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Ir Spectroscopy ◽  
Oxygen Atom ◽  
Structure Analysis ◽  
Titanium Tetrachloride ◽  
Titanium Atom ◽  
Molecular Complexes ◽  
Space Group ◽  
Structure Determinations

AbstractTiCl3(NPPh3) and TiCl3(OSiPh3) have been prepared from titanium tetrachloride and Me3SiNPPh3 and HOSiPh3, respectively. Both complexes were characterized by IR spectroscopy and by crystal structure determinations. TiCl3(NPPh3): Space group R3̄̅, Z = 6, structure analysis with 959 observed unique reflections, R = 0.039. Lattice dimensions at -68°C: a = b = 1370.5(7), c = 1845.9(9) pm. TiCl3(OSiPh3): Space group P21/c, Z = 8, structure analysis with 4549 observed unique reflections, R = 0.049. Lattice dimensions at 19°C: a = 2127.7(2), b = 947.2(1), c = 2136.8(1) pm, β = 105.081(5)°. Both complexes form monomeric molecules in which the titanium atom is tetrahedrally coordinated by three chlorine atoms, the nitrogen atom of the phosphorone iminato ligand and the oxygen atom of the silyloxy group, respectively. The bond lengths TiN of 171.9(4) pm and TiO of 171.0(3) (in average) correspond to double bonds.

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