Notizen: Kristallstruktur von 1,1-Dichlor-3,5-diphenyl-4-H-1,2,4,6-λ4-selenatriazin, SeCl2C2N3H(C6H5)2 / Crystal Structure of 1,1-Dichloro-3,5-diphenyl-4-H-1,2,4,6-λ4-selenatriazine, SeCl2C2N3H(C6H5)2

1989 ◽  
Vol 44 (7) ◽  
pp. 857-859 ◽  
Author(s):  
Dieter Fenske ◽  
Christina Ergezinger ◽  
Kurt Dehnicke

The title compound has been prepared as a byproduct of the reaction of Se2Cl2 with Ν,Ν,N′-Tris(trimethylsilyl)benzamidine in CH2Cl2 solution. [SeCl2(HNC2N2Ph2)]2 was characterized by an X-ray structure determination. Space group P21/n, Z = 2, 2979 observed independent reflexions, R = 0.032. Lattice dimensions (-65 °C): a = 1050.1(4), b = 1018.9(4), c = 1402.1(6) pm; β = 99.78(3)°. The compound forms centrosymmetric dimeric molecules with SeCl2Se bridges (bond lengths 241.6(1) and 339.3(1) pm), the selenium atoms being members of nearly planar [xxx] selenatriazine rings with Se—N bond lengths of 182.2(2) and 181.5(2) pm.

1991 ◽  
Vol 46 (12) ◽  
pp. 1625-1628 ◽  
Author(s):  
Stefan Vogler ◽  
Werner Massa ◽  
Kurt Dehnicke

The reaction of tungsten hexachloride with Se4N2 leads to [WCl4(NSeCl)]2, which reacts with pyridine to form [WCl4(NSeCl)Py], and with tetraphenylphosphonium chloride to form PPh4[WCl5(NSeCl)], which was characterized by an X-ray structure determination. Space group P21, Z = 2, 1657 observed unique reflections, R = 0.074, wR = 0.061. Lattice dimensions at —80 C: a = 710.7(1), b = 2217.9(4), c = 953.6(2) pm; β = 111.93(3) . The [WCl5(NSeCl)]- ion possesses an almost linear WNSe group with bond lengths WN = 188 pm, corresponding to a double bond, and NSe = 200 pm.


1988 ◽  
Vol 43 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Dieter Fenske ◽  
Eberhard Böhm ◽  
Kurt Dehnicke ◽  
Joachim Strähle

Abstract The title compound has been prepared by the reaction of N-trimethylsilyl-iminotriphenylphos-phorane with copper(II) chloride in boiling CCl4 /C2H5OH, and forms moisture sensitive crystals, which are green in transmittance and black in reflexion. [Me3SiNPPh3 · CuCl2 ] 2 was characterized by its IR spectrum as well as by a crystal structure determination (4197 observed, independent reflexions, R = 0.049). The lattice dimensions are at 20 °C: a = 1102.7. b = 1407.3. c = 1560.2 pm; β = 94.27°; space group P21/n with two formula units in the unit cell. The complex consists of centrosymmetric, dimeric molecules with a planar Cu2 Cl2 ring (Cu-CI bond lengths 229 and 231 pm). A terminally bonded CI atom (Cu-CI = 221 pm) and the N atom of the Me3SiNPPh3 ligand (Cu-N = 198.5 pm) complete the coordination number four of the nearly planar surroundings of the Cu atoms.


1991 ◽  
Vol 46 (10) ◽  
pp. 1287-1292 ◽  
Author(s):  
Rüdiger Staffel ◽  
Ulrich Müller ◽  
Andreas Ahle ◽  
Kurt Dehnicke

The title compound was prepared from sodium polyselenide and 12-crown-4 in DMF solution in the presence of cerium(III)chloride in the form of black needles. The crystal structure determination by X-ray diffraction shows a partially disordered structure, in which the anionic units Se82- · Se7 and Se82- · Se6 are present in the ratio 0.72/0.28. These units are associated to layers parallel to (100); the layers alternate with pseudohexagonal layers of [Na(12-crown-4)2]+ ions. Space group P1̅, Z = 2, 3903 observed unique reflections, R = 0.114, wR= 0.084. Lattice dimensions at -65°C: a = 1247.9(3), b = 1367.8(8), c = 1660(1) pm, α = 94.65(5), β = 98.94(3), γ = 91.10(3)°.


2011 ◽  
Vol 66 (11) ◽  
pp. 1087-1091 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo

Colorless and transparent single crystals of Ba2H3I were obtained by reacting Ba with dried and sublimed NH4I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules at 1100 K for 13 h. The crystal structure of the title compound was determined and refined by means of single-crystal X-ray diffraction. Ba2H3I crystallizes in a stuffed anti-CdI2 structure isotypic to Sr2H3I in the space group P3̄m1 (no. 164) with the lattice parameters a = 451.86(12) and c = 811.84(23) pm. The structural results for Ba2H3I are consistent with bond lengths and coordination geometries of related binary and ternary hydrides


1978 ◽  
Vol 33 (6) ◽  
pp. 610-613 ◽  
Author(s):  
Siegfried Pohl

Abstract The crystal structure of the title compound was determined from single crystal X-ray data. The compound crystallises in the orthorhombic space group Pnma. In contrast to the solution where fluctuating P-Te bonds have been established by NMR analyses the crystals contain isolated molecules with fixed P-Te bonds (bond length: 235.4 pm). The four-membered phosphorus nitrogen ring exhibits significant deviations from planarity. The P-N bond lengths were found to be 168.3 and 175.0 pm, respectively


1995 ◽  
Vol 50 (1) ◽  
pp. 66-70 ◽  
Author(s):  
Inge Pabst ◽  
Peter Sondergeld ◽  
Mirjam Czjzek ◽  
Hartmut Fuess

The title compound has been prepared in two different ways: First, by boiling single crystals of [(C2H5)4N]HgCl3 in a mixture of n-hexane/n-octane [4:1] at T = 350 K, and second, in a synthesis from stoichiometric quantities of the components. X-ray structure analysis gave the stoichiometry [(C2H5)4N]2Hg3Cl8, monoclinic, space group P21, a = 7.538(3), b = 19.909(6), c = 10.274(3) Å, β = 95.13(1)°, V = 1535.7(9) A3, Z = 2. The basic [Hg3Cl8]2--units form broken zig-zag chains along [100]. The Hg–Cl distances within the [Hg3Cl8]2- clusters range from 2.315(3) to 2.755(4) Å. This is a new coordination type for halomercurates.


1989 ◽  
Vol 44 (9) ◽  
pp. 1003-1006 ◽  
Author(s):  
Kurt Merzweiler ◽  
Dieter Fenske ◽  
Eva Hartmann ◽  
Kurt Dehnicke

The title compound has been prepared by the reaction of N,N,N′-tris(trimethylsilyl)benzamidine with tantalum pentachloride in CH2Cl2 suspension, forming amber-coloured, moisturesensitive crystals, which were characterized by an X-ray structure determination. Space group P 21/n, Z = 2, 4895 observed independent reflexions, R = 0.059. Lattice dimensions (-65°C): a = 1165.2(6), b = 1335.4(6), c = 1629.0(7) pm, β = 93.23(4)°. The complex forms centrosymmetric molecules dimerized via chloro bridges TaCl2Ta with TaCl bond lengths of 247.2(2) and 277.1(2) pm, the longer one being in trans-position to the imido group, which can be formulatedas [xxx] (bond lengths Ta=Ν = 183.5(8), C=N = 134(1) pm, bond angle TaNC = 162.7(7)°).


1986 ◽  
Vol 41 (7) ◽  
pp. 839-844 ◽  
Author(s):  
H .-D. Hausen ◽  
G. Rajca ◽  
J. Weidlein

AbstractThe title compound, Cl2PN2CCl, has been synthesized by the reaction of PCl5 with Me3Si -N = C = N - SiMe3 (Me - CH3) in a 1:1 molar ratio. The colourless com pound is trimericin benzene solution and in the solid state and has a structure with a highly puckered 12-membered P3N6C3-ring skeleton of low symmetry. The X-ray structure determination shows a monoclinic space group P 21/a with 4 trimeric units per cell.


1990 ◽  
Vol 45 (11) ◽  
pp. 1593-1596 ◽  
Author(s):  
Wolfgang Hiller ◽  
Alfred Zinn ◽  
Kurt Dehnicke

The title compound has been prepared by the reaction of CuCl, with hexakis(trimethylsilyl)-benzdiamidine, in boiling acetonitrile in the presence of traces of water, as brown crystals, which were characterized by their IR spectrum as well as by an X-ray structure determination. Space group C 2/c, Z = 4, 2668 observed unique reflexions, R = 0.036. Lattice dimensions at –65 C: a = 879.5(2), b = 2441.1(3), c = 1241.4(3) pm, β = 95.24(3)°. In the structure four copper atoms surround an oxygen atom in a slightly distorted tetrahedral fashion; the chlorine atoms bridge adjacent copper atoms, and each copper atom is thus bound to three chlorine atoms. The nitrogen atoms of the acetonitrile complete the slightly distorted trigonal bipyramid around the copper atoms.


1989 ◽  
Vol 44 (10) ◽  
pp. 1325-1328 ◽  
Author(s):  
Klaus Hösler ◽  
Frank Weller ◽  
Kurt Dehnicke

The chlorothionitrene complex [Cl4Mo(NSCl)]2 reacts with N,N,N′-tris(trimethylsilyl)benzamidine in THF solution to form the heterocyclic complex [MoCl2(NSN) · 2 THF]2, which contains the [NSN]4-unit. The compound is characterized by IR spectroscopy and by an X-ray structure determination (Space group P2,/c, Z = 2, 1504 observed unique reflexions, R = 0.044. Lattice dimensions at 19°C: a = 1176.0(1), b = 1108.6(4), c = 1227.3(3) pm, β = 118.25(1)°). The compound forms centrosymmetric molecules [(THF)2Cl2Mo(NSN)2MoCl2(THF)2], in which the molybdenum atoms are members of a nearly planar Mo(NSN)2Mo eight-membered ring with bond lengths MoN 180.2 and 175.2 pm; NS 157.5 and 160.6 pm; the bond angle NSN is 108.3°, corresponding to a NSN4- unit.


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