Molybdännitridtrichlorid-2,3,3-trichloracrylnitril, [MoNCI3 · NC-C2Cl3]2 Synthese, IR-Spektrum und Kristallstruktur / Molybdenumnitridetrichloride-2,3,3-trichloroacrylnitrile, [MoNCl3 · NC—C2Cl3]2 Synthesis, IR Spectrum, and Crystal Structure

1988 ◽  
Vol 43 (12) ◽  
pp. 1616-1620 ◽  
Author(s):  
Abderraouf Khabou ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Bond Length ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Triple Bond ◽  
Crystal Data ◽  
Space Group ◽  
Bond Lengths ◽  
Trans Influence

Abstract [MONCl3 · NC - C2Cl3]2 has been prepared by the reaction of MONCl3 with trichloromethyl isocyanidedichloride, CCl3NCCl2 , in CH2Cl2 suspension. The compound forms redbrown. mois-ture sensitive crystals, which were characterized by their IR spectrum as well as by a crystal structure determination (2482 independent observed reflexions, R = 0.048). Crystal data (-70 °C): Space group P21/c, Z = 2, a = 674.2(2); b = 2128.2(11); c = 786.0(4) pm: β = 102.81(3)°. [MONCl3 • NC-C2Cl3]2 forms centrosymmetric dimeric molecules via chloro bridges with Mo-Cl bond lengths of 240.7 and 276.0 pm. The longer MoCl bond of the MOCl2MO ring is caused by the trans influence of the nitride ligand; the MoN bond length of 167 pm corresponds with a triple bond. The 2,3,3-trichloroacrylnitrile ligand is bonded by its nitrogen atom with a bond length of Mo -N = 216 pm; the Mo-N≡C-C sequence is almost linear with a remarkable short C-C bond of 143.0 pm.

N-TrimethylsilyMminotriphenylphosphoran-Kupfer(II)-chlorid, [Me3 SiNPPh3 · CuCl 2 ]2 Synthese und Kristallstruktur / N-Trimethylsilyl-iminotriphenylphosphorane Copper(II) Chloride, [Me3 SiNPPh3 · CuCl 2] 2 Synthesis and Crystal Structure

1988 ◽  
Vol 43 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Dieter Fenske ◽  
Eberhard Böhm ◽  
Kurt Dehnicke ◽  
Joachim Strähle
Keyword(s):  
Crystal Structure ◽  
Coordination Number ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Title Compound ◽  
Unit Cell ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Bond Lengths ◽  
Moisture Sensitive

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.

Synthese und Kristallstruktur des cyclischen Hydrazido-Komplexes {Fe2Cl4[(NSiMe3)(CPh)]2N2} / Synthesis and Crystal Structure of the Cyclic Hydrazido Complex {Fe2Cl4[(NSiMe3)(CPh)]2N2}

1989 ◽  
Vol 44 (4) ◽  
pp. 495-498 ◽  
Author(s):  
Wolfgang Hiller ◽  
Eva Hartmann ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Title Compound ◽  
Crystal Data ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Data Space ◽  
Moisture Sensitive

The title compound has been prepared by the reaction of FeCl3 with N, N, N′-tris(trimethylsilyl) benzamidine in CH2Cl2 solution as dark red, moisture-sensitive crystals. The complex was characterized by its IR spectrum as well as by an X-ray structure determination.Crystal data: space group P21/n, Z = 2 (1178 observed independent reflexions, R = 0.089). Lattice dimensions (20 °C): a = 1240.2(2), b = 645.7(3), c = 1779.7(3) pm, β = 91.31(2)°. The compound forms centrosymmetric molecules, in which the iron atoms are members of two fused planar heterocycles with the NN group as the com m on edge. The NN bond length (142.5(9) pm) is very close to the NN bond length of hydrazine.

scholarly journals Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2 / Molecular and Crystal Structure of l,r-Dimethylsilylene Titanocene Dichloride, (CH3)2Si(C5H4)2TiCl2

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structure Determination ◽  
Titanocene Dichloride ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Structural Dimensions

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2

scholarly journals Über die Reaktion von Wolframhexachlorid mit Se4N2; Kristallstruktur von PPh4[WCl5(NSeCl)] / On the Reaction of Tungsten Hexachloride with Se4N2; Crystal Structure of PPh4[WCl5(NSeCl)]

1991 ◽  
Vol 46 (12) ◽  
pp. 1625-1628 ◽  
Author(s):  
Stefan Vogler ◽  
Werner Massa ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Structure Determination ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Tetraphenylphosphonium Chloride ◽  
Tungsten Hexachloride

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.

Kristallstruktur und spektroskopische Charakterisierung von Hexamethyl- disilazan-Aluminiumtrichlorid [(H3C)3Si]2NH ∙ AlCl3 / Crystal Structure and Spectroscopic Characterisation of Hexamethyl- disilazane-trichloroalum inum [(H3C)3Si]2NH ∙ AlCl3

2000 ◽  
Vol 55 (8) ◽  
pp. 763-767 ◽  
Author(s):  
Martin Jansen ◽  
Thomas Jäschke
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Bond Length ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Space Group ◽  
Aluminium Trichloride ◽  
Spectroscopic Characterisation

Abstract By reaction of hexamethyldisilazane with aluminium trichloride in hexane hexamethyldisilazane-trichloroaluminum [(H3C)3Si]2NH • AlCl3 is formed. The adduct has been characterized by MS, IR, Raman, 1H, 13C, 27Al, 29Si NMR spectroscopy, and by a crystal structure determination (1425 independent reflections, R = 0.035). The space group is Pbca with a = 1312,6(5), b = 1182,9(5), c = 1964,7(5) pm; Z = 8. [(H3C)3Si]2NH • AlCl3 forms monomeric units which have point symme­try C1 and exhibit an Al − N bond length of 193,9(3) pm.

Notizen: 1,2-Dimethoxyethan-Komplexe von MoNCl3 und WNCl3. Die Kristallstruktur von [MoNCl3 · DME] / 1,2-Dimethoxyethane Complexes of MoNCl3 and WNCl3. The Crystal Structure of [MoNCl3 · DME]

1993 ◽  
Vol 48 (12) ◽  
pp. 1841-1844 ◽  
Author(s):  
Eva Rentschler ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Organic Solvents ◽  
Structure Determination ◽  
Triple Bond ◽  
Trans Position ◽  
Molybdenum Complex ◽  
Structure Solution ◽  
In Trans ◽  
Moisture Sensitive

The complexes [MoNCl3·DME] and [WNCl3·DME] (DME = 1,2-dimethoxyethane) have been prepared by the reaction of the nitride chlorides MNC13 with equimolar amounts of DME in CH2Cl2 suspensions. They form orangered, moisture sensitive crystals, which are soluble in organic solvents. The molybdenum complex has been characterized by a crystal structure determination. Space group Pbca, Z = 8, structure solution with 1781 observed unique reflections, R = 0.031. Lattice dimensions at –60°C: a = 738.6(1), b = 1182.2(1), c = 2314.1(1) pm. [MoNCl3·DME] forms monomeric complexes with chelating DME molecules and Mo–O bond lengths of 215.4(4) and 247.4(4) pm, the longer one being in trans-position of the nitrido ligand. The MoN bond length of 163.3(5) pm suggests a triple bond.

Brom- und Chlorthionitrenkomplexe des Rheniums. Die Kristallstruktur von (PPh4)2 [ReBr4(NS)(NSBr)]·CH2Br2 Bromo- and Chlorothionitrene Complexes of Rhenium The Crystal Structure of (PPh4)2[ReBr4(NS)(NSBr)]·CH2Br2

1986 ◽  
Vol 41 (7) ◽  
pp. 825-830 ◽  
Author(s):  
Hans-Günter Hauck ◽  
Wolfgang Willing ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Ring Cleavage ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Pyridine Complex ◽  
Subsequent Addition

AbstractThe thionitrosyl-halothionitrene com pounds (PPh4)2[ReX4(NS)(NSX)]·2 CH2X2, X = Cl or Br, are obtained by nucleophilic ring cleavage of the Re(N2S2) rings of complexes [ReX4(N2S2)]⊖ with PPh4X in CH2X2. (AsPh4)2[ReCl4(NS)(NSCl)] · CH2Cl2 can also be obtained by the reaction of [ReCl4(NSCl)(POCl3)] with S(NSiMe3)2 and subsequent addition of AsPh4Cl. The pyridine complex [ReBr2(NS)(NSBr)(NC5H5)2] · CH2Br2 forms by bromination of the corresponding chloro compound with Me3SiBr. The IR spectra are reported. The crystal structure of (PPh4)2[ReBr4(NS)(NSBr)] · CH2Br2 was determ ined by X-ray diffraction (4158 independent observed reflexions, R = 0.059). Crystal data: a = 1039.7, b - 1232.5, c - 2158.4 pm, α = 81.59, β = 87.05, γ = 77.06°, Z = 2, space group P1̄. The compound consists of PPh4⊕ ions, CH2Br2 molecules, and anions [ReBr4(NS)(NSBr)]2⊖ in which the rhenium atoms are coordinated by four bromine atoms, one thionitrosyl and one brom othionitrene group. The latter have cis arrangement and ReN bond lengths of 186 pm. W hereas the thionitrosyl group is nearly linear, the R = N = SBr group has an ReNS angle of 165°.

scholarly journals Die Kristallstruktur von PPh3Me[NbOCl4(CH3CN)] / The Crystal Structure of PPh3Me[NbOCl4(CH3CN)]

1984 ◽  
Vol 39 (1) ◽  
pp. 107-110 ◽  
Author(s):  
W. Hiller ◽  
J. Strähle ◽  
H. Prinz ◽  
K. Dehnicke
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Nitrogen Atom ◽  
Bond Length ◽  
Unit Cell ◽  
Trans Position ◽  
Space Group ◽  
X Ray ◽  
Oxo Ligand ◽  
Solvate Molecule

The X-ray structure of PPh3Me[NbOCl4(CH3CN)] at 210 K was solved (space group P1̄, two formula units per unit cell, a = 1173.5(5), b = 1130.1(4), c = 946.8(3) pm, α = 97.70(4), β = 93.57(3), γ = 78.62(3)°, 3688 inde­pendent reflexions, R = 0.025). The material consists of cations [P(C6H5)3CH3]⊕ and anions [NbOCl4(CH3CN)]⊖. The nitrogen atom of the acetonitrile solvate molecule is coordinated to the niobium centre in the trans-position to the oxo ligand; the NbO bond length of 169 pm corresponds to a double bond.

[ η6-C6Me6Fe- η5-C5H5]2Fe2Cl6 · 2 CH2Cl2: Bildung und Kristallstruktur / [η6-C6Me6Fe-η5-C5H5]2Fe2Cl6· 2CH2Cl2: Formation and Crystal Structure

1992 ◽  
Vol 47 (8) ◽  
pp. 1075-1078 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Ir Spectrum ◽  
Title Compound ◽  
The Novel ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

When hexymethylbenzene-cyclopentadienyl-iron reacts with ozone in dichloromethane, the title compound is one of the products. Its crystal structure was determined by X-ray diffraction (R = 0.145 for 1412 unique reflexions). Crystal data: a = 1815.1(8), b = 1314.8(5), c = 1823.0(8) pm, space group Pbca, Z = 8. The sandwich-like [η6-C6Me6Fe-η5-C5H5]+ ions exhibit large thermal motions, and the CH2C12 molecules are disordered in two orientations. The novel [Fe2Cl6]2- ion has the structure of two tetrahedra sharing an edge. Its IR spectrum is reported.

Substitutionsreaktionen an der N-Chlornitrenogruppe des [WCl4(NCl)]2. Die Kristallstrukturen von [CH3CN—WCl4(NSMe)] und [WNCl3 · NC—CH3]4 / Substitution Reactions at the N-Chloronitreno Group of [WCl4(NCl)]2. The Crystal Structures of [CH3CN—WCl4(NSMe)] and [WNCl3 · NC—CH3]4

1989 ◽  
Vol 44 (8) ◽  
pp. 903-910 ◽  
Author(s):  
Astrid Görge ◽  
Ute Patt-Siebel ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Trans Position ◽  
Crystal Data ◽  
Substitution Reactions ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations

[WCl4(NCl)]2 reacts in acetonitrile with the trimethylsilyl compounds Me3SiSR (R = Me, Ph), and Me3SiESiMe3 (E = S, Se), with substitution of the chlorine atom of the N-chloronitreno group W=N–Cl and formation of CH3CN–WCl4(NSR) and CH3CN–WCl4(NEN)WCl4–NCCH3, respectively. Excess Me3SiBr reacts with CH3CN–WCl4(NSMe) to afford CH3CN–WBr4(NSMe). [CH3CN–WNCl3]4 was obtained from CH3CN–WCl4(NCl) and N(SiMe3)3. The products were characterized by their IR spectra. Two X-ray crystal structure determinations were also carried out. CH3CN—WCl4(NSMe) forms twinned crystals, and only non-overlapping reflexions of one of the twin individuals were used for the structure determination (846 unique values, R = 0.055). Crystal data: a = 592.4(2), b = 758.8(2), c = 1203.7(8) pm, β = 95.06(4)°, monoclinic, space group P21/m, Z = 2. The compound is a monomer in which the acetonitrile ligand is situated in the trans position to the W≡N–S̱̅–Me group. The bond lengths (W≡N 174(2), N–S 161(2) pm) and bond angles (WNS 176(1), NSC 102.1(9)°) are in agreement with the proposed formula. Crystal data for [CH3CN–WNCl3]4: a = 1009.5(2), b = 1274.5(2), c = 1287.9(2) pm, β = 108.17(1)°, monoclinic, space group P21/c, Z = 2 (2113 unique reflexions, R = 0.057). The compound forms tetrameric units, in which the W atoms form a square and are linked with one another via N atoms at alternating distances (W=N 171(2), W–N 207(2), W–NCMe 238(2) pm).

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