Cyclothiazeno-oxo-diazidowoIframat(VI) Die Kristallstruktur von (AsPh4)2[W(N3S2)(O)(N3)2]2 / Cyclothiazeno Oxodiazidotungstate(VI) The Crystal Structure of (AsPh4)2[W(N3S2)(O)(N3)2]2

1985 ◽  
Vol 40 (12) ◽  
pp. 1626-1630 ◽  
Author(s):  
Heribert Wadle ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Coordination Number ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Ring System ◽  
Crystal Data ◽  
Improved Method ◽  
Silver Azide ◽  
Tungsten Atom ◽  
Triclinic Space Group

Abstract A new, improved method of synthesis for the cyclothiazeno complex AsPh4[WCl4(N3S2)] consists of the reaction of Na2WO4 with molten trithiazyl chloride (NSCl)3 followed by treatment with AsPh4Cl in CH2C12. Through the reaction with silver azide suspended in CH2C12 in the presence of moisture, black crystalline (AsPh4)2[W(N3S2)(O)(N3)2]2 is obtained. Its IR spectrum and its crystal structure are reported. Crystal data: triclinic, space group P1̄, Z = 1, a - 1018.3, b = 1107.8, c = 1379.1 pm; a = 91.11°, β = 106.74°, γ = 113.91°. Structure determination with 3219 observed reflexions, R = 0.061. The structure consists of AsPh4+ cations arranged to form (AsPh4+)2 pairs and of dimeric anions [W(N3S2)(O)(N3)2]2⊖ in which the tungsten atom s are members of planar cyclothiazeno rings WN3S2 with WN bond lengths of 186 and 222 pm. The oxygen atoms are in positions trans to the longer of these bonds. One of the N atoms of each cyclothiazeno ring is involved in the dimerization resulting in a centrosymmetric W2N2 ring. The azido groups are situated above and below the ring system and complete the coordination number of six for the W atoms with WN distances of 208 and 212 pm

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.

scholarly journals Synthese und Kristallstruktur von (PPh4)2Te4 / Synthesis and Crystal Structure of (PPh4)2Te4

1991 ◽  
Vol 46 (8) ◽  
pp. 1015-1019 ◽  
Author(s):  
Hans Wolkers ◽  
Bernhard Schreiner ◽  
Rüdiger Staffel ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Crystal Data ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cscl Type ◽  
Type Lattice ◽  
Close Contacts

(PPh4)2Te4 has been prepared by the reaction of Na2Te3 with PPh4Cl in DMF solution in the presence of MnCl2 or FeCl2. The compound forms dark red crystals, which were characterized by IR spectroscopy as well as by an X-ray crystal structure determination (6109 observed independent reflections, R = 0.030). Crystal data: triclinic, space group PĪ, Z = 2, a = 1046.7(2), b = 1130.1(2), c = 1967.8(4) pm, α = 93.63(3), β = 90.43(3), γ = 108.89(3)° at —60 °C. The cations are grouped in pairs (PPh4+)2 around inversion centres, each pair being surrounded by eight Te42- ions, arranged as in the CsCl type lattice. The chain-like Te42- ions have no close contacts with one another.

μ-Nitridokomplexe von Wolfram(VI) Die Kristallstruktur von PPh4[W2NCl10]/ μ-Nitrido Complexes of Tungsten(VI) The Crystal Structure of PPh4[W2NCl10]

1985 ◽  
Vol 40 (8) ◽  
pp. 999-1004 ◽  
Author(s):  
Thomas Godemeyer ◽  
Alexander Berg ◽  
Hans-Dieter Groß ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Phosphorus Oxide ◽  
Tungsten Atom ◽  
Triclinic Space Group ◽  
X Ray ◽  
Nitrido Complexes ◽  
Tetraphenylphosphonium Chloride ◽  
Tungsten Hexachloride

AbstractW2NCl9 was obtained as a brilliant red crystal powder from tungsten hexachloride and tris(trimethylsilyl)amine. According to its IR spectrum it has dimeric molecules [W2NCl9]2 with bridging chlorine atoms. Its reaction with tetraphenylphosphonium chloride yields PPh4[W2NCl10], and with phosphorus oxide chloride W2NCl9 ·OPCl3 is obtained; both are soluble in dichlorom ethane. The crystal structure of PPh4[W2NCl10] was determined by X-ray diffraction (2521 observed reflexions. R = 0.065). Crystal data: triclinic, space group P1̄, Z = 2, a = 1125.7, b - 1278.2, c = 1347.8 pm, α = 110.08, β = 94.55, γ = 111.55°. The structure consists of PPh4ⓛ ions which are arranged to (PPh4ⓛ)2 pairs about inversion centres, and of [W2NCl10]⃝ anions. The latter possess an almost linear W NW group (173°) with slightly different WN bond lengths of 179 and 188 pm corresponding to double bonds. Each tungsten atom has an octahedral coordination. The WCl bonds trans to the nitrido ligand are about 9 pm longer than the bonds in the cis positions.

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 Notizen: Synthese und Kristallstruktur von PPh3Me[HSO4]/ Synthesis and Crystal Structure of PPh3Me[HSO4]

1988 ◽  
Vol 43 (8) ◽  
pp. 1069-1071 ◽  
Author(s):  
Fritjof Schmock ◽  
Aida Müller ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Hydrogen Bonds ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Crystal Data ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Silver Sulfate ◽  
By Products

AbstractPPh3Me[HSO4] was prepared by the reaction of (PPh3Me)I with silver sulfate in aqueous solution. OPPh2Me and benzene being the by-products. The title compound was characterized by its IR spectrum as well as by an X-ray structure determination (1730 observed independent reflexions, R = 0.043). Crystal data: a = 910.4(3). b = 1587.8(4), c = 1294.2(6) pm, β = 105.52(3)°. space group P21/c, Z = 4. The structure consists of PPh3Me⊕ cations and of HOSO3⊖ ions that are associated via strong hydrogen bonds to dimeric centrosymmetric units.

Tetrazido-Nitrido-Molybdat(VI); Darstellung, IR-Spektrum und Kristallstruktur von AsPh4[MoN(N3)4] / Tetrazido-nitrido-molybdate(VI); Preparation, IR Spectrum and Crystal Structure of AsPh4[MoN(N3)4]

1980 ◽  
Vol 35 (9) ◽  
pp. 1070-1074 ◽  
Author(s):  
Kurt Dehnicke ◽  
Josef Schmitte ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Ir Spectrum ◽  
Sodium Sulfate ◽  
Triple Bond ◽  
Steric Effects ◽  
X Ray Diffraction ◽  
Silver Azide ◽  
Triclinic Space Group ◽  
X Ray ◽  
Covalently Bonded

The complex AsPh4[MoN(N3)4] is prepared by the reaction of AsPh4[MoNCl4] with silver azide in dichloromethane suspension in the presence of dry sodium sulfate. The IR spectrum indicates an Mo≡N group and four covalently bonded N3 groups for the [MoN(N3)4]⊖ anion. AsPh4[MoN(N3)4] crystallizes in the triclinic space group P1̄ with two formula units in the unit cell. The crystal structure was solved by X-ray diffraction methods (R = 0,038; 4049 independent reflexions). The structure consists of AsPh4⊕ cations and [MoN(N3)4]⊖ anions. The short MoN bond length of the nitrido ligand (163 pm) corresponds to an Mo ≡ N triple bond. The steric effects of the lone pairs of the α-N atoms of the azido groups with tho MoN ligand cause a propellerlike twisted conformation of the four azido groups.

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

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.

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.

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