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°.

Pyridin-Addukte von Cyclothiazeno-Vanadiumdichlorid Die Kristallstruktur von [VCl2(N3S2)(C5H5N)] / Pyridine Adducts of Cyclo-thiazeno Vanadium Dichloride The Crystal Structure of [VCl2(N3S2)(C5H5N)]

1985 ◽  
Vol 40 (12) ◽  
pp. 1631-1637 ◽  
Author(s):  
Ruth Christophersen ◽  
Paul Klingelhöfer ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Chlorine Atom ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Trigonal Bipyramidal ◽  
Independent Molecules

Abstract The pyridine complexes of cyclo-thiazeno vanadium dichloride, [VCl2(N3S2)py] and [VCl2(N3S2)(py)2] were synthesized by reactions of polymeric VCl2(N3S2) with varying amounts of pyridine in CH2Cl2. The compounds were characterized by their IR spectra as well as by their 51V NM R spectra. The crystal structure of [VCl2(N3S2)(C5H5N)] was determined by means of X-ray diffraction (1582 independent observed reflexions, R = 0.031). Crystal data: orthorhombic, space group Pnma, a = 1372, b - 2261, c - 1068 pm, Z = 12. In the lattice there are two monomeric, crystallographically independent molecules [VCl2(N3S2)(C5H5N)], which differ only slightly. The vanadium atoms have a trigonal bipyramidal coordination with the N atom of the pyridine molecule and one chlorine atom in apical positions, and with one chlorine atom and the N atoms of the cyclo-thiazeno ligand in equatorial positions. The VN bond lengths of the planar VN3S2 ring of 174 pm correspond to double bonds

Ein neuer Zugang zu Tetrathiooxalaten. Die Kristallstruktur von (NEt4)2[C2S4] / A Novel Access to Tetrathiooxalates. Crystal Structure of (NEt4)2[C2S4]

1992 ◽  
Vol 47 (5) ◽  
pp. 702-705 ◽  
Author(s):  
Alfred D. Bacher ◽  
Irina Sens ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Dihedral Angle ◽  
Point Symmetry ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Subsequent Addition

(NEt4)2S5 was prepared from NEt4Cl and Na2S4 in ethanol. Its reaction with boiling acetonitrile yielded tetraethylammonium tetrathiooxalate. (NEt4)2[C2S4] was also obtained by heating (NEt4)2S5 with tetraethylammonium dithioacetate in ethanol. Benzyltriethylammonium tetrathiooxalate, (NEt3Bz)2[C2S4]· 2 toluene, crystallized after NEt3BzCl and Na2S4 were heated in acetonitrile on subsequent addition of toluene. The crystal structure of (NEt4)2[C2S4] was determined by X-ray diffraction (454 independent observed reflexions, R = 0.047). Crystal data: tetragonal, a = 871.2(1) pm, c = 1566.0(3) pm, space group P42/nmc, Z = 2. The [C2S4]2- ion has point symmetry 4m2 (D2d), i.e. the dihedral angle between the two CS2 groups is 90°. The ethyl groups of the NEt4+ ions are disordered in two orientations.

Untersuchungen zur möglichen Existenz des S4N4⊕-Radikalkations und die Kristallstruktur von S4N4[FeCl4] / Investigations Concerning the Possible Existence of the S4N4⊕ Radical Cation and the Crystal Structure of S4N4H[FeCl4]

1986 ◽  
Vol 41 (9) ◽  
pp. 1061-1066 ◽  
Author(s):  
Ulf Thewalt ◽  
Konrad Holl ◽  
Udo Demant ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Radical Cation ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

Abstract Brom ination o f S4N 4 Cl[FeCl4], Preparation o f S4N 4 H [FeX 4] (X = Cl, Br), IR Spectra, Crystal Structure of S4N4H[FeCI4] S4N 4 H [FeC l4] as well as S4N 4 D [F eC l4] were prepared in C H 2C12 by reaction o f S4N 4 with FeC l3 and C H 3C O O H and CH 3C O O D , respectively. Bromination o f S4N 4C l[FeCl4] with M e3SiBr in C H 2 C12 yields S4N 4 H[FeBr4]; in this reaction, S4N 4 Br® is presumably formed initially; it then decom p oses by elimination o f bromine and formation of the S4N 4® radical cation; the latter reacts with the solvent, yielding the S4N 4 H® cation. Brom ination of S3N 2C l[FeCl4] with M e3SiBr affords S6N 4 [FeBr4]2. The IR spectra o f the com pounds are discussed. The crystal structure o f S4N 4 H [FeC l4] was determined by X-ray diffraction (1210 observed reflexions, R = 0.035). Crystal data: a = 803.8, b — 1003.9, c = 1507.7 pm, β = 104.52°, Z = 4, space group P 2,/c.

Anionische Komplexe [Mo2(O2CPh)4X2]2⊖ mit X = N3, Cl, Br. Die Kristallstruktur von (PPh4)2[Mo2(O2CPh)4Cl2] · 2CH2Cl2 / Anionic Complexes [Mo2(O2C-Ph)4X2]2⊖ with X = N3, Cl, Br. The Crystal Structure of (PPh4)2[Mo2(O2C-Ph)4Cl2] · 2CH2Cl2

1985 ◽  
Vol 40 (1) ◽  
pp. 13-18 ◽  
Author(s):  
Kay Jansen ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Diffraction Data ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Anionic Complexes

The syntheses and IR spectra of the complexes [Mo2(O2C-Ph)4X2]2⊖ with X = N3, CI, Br and the counter ion PPh4⊕ are reported. The azido and the bromo complexes are obtained from a solution of [Mo2(O2CPh)4] with PPh4N3 in pyridine or by reaction with PPh4Br in CH2Br2, respectively. When (PPh4)2[Mo2(O2CPh)4(N3)2] is dissolved in CH2Cl2, nitrogen is evolved and the complex with X = CI is obtained. The crystal structure of (PPh4)2[Mo2(O2CPh)4Cl2] · 2CH2Cl2 was determined from X-ray diffraction data (5676 observed independent reflexions, R = 0.042). It crystallizes in the monoclinic space group P21/n with four formula units per unit cell; the lattice constants are a = 1549, b = 1400, c = 1648 pm, β = 94.6°. The centrosymmetric [Mo2(O2CPh)4Cl2]2⊖ ion has a rather short Mo-Mo bond of 213 pm, whereas the MoCl bonds are very long (288 pm)

Nitrido-und Oxochlorokomplexe des Vanadiums(V); die Kristallstruktur von AsPh4 [V0C14] Nitrido and Oxochloro Complexes of Vanadium(V); the Crystal Structure of AsPh4[VOCl4]

1980 ◽  
Vol 35 (5) ◽  
pp. 522-525 ◽  
Author(s):  
Gisela Beindorf ◽  
Joachim Strähle ◽  
Wolfgang Liebelt ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Bond Length ◽  
Bond Angle ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Linear Arrangement ◽  
Space Group ◽  
X Ray ◽  
Complex Anions

The complexes AsPh4[Cl4V = N-Cl] and AsPh4[VOCl4] are prepared by the reaction of AsPh4Cl with Cl3VNCl and VOCl3, respectively. The IR spectra indicate C4v symmetry for the complex anions with multiple VN and VO bonds and a linear arrangement for the VNCl-group. AsPh4[VOCl4] crystallizes in the tetragonal space group P4/n with two formula units in the unit cell. The crystal structure was solved by X-ray diffraction methods (R = 0,062, 1096 observed, independent reflexions). The structure consists of AsPh4+ cations and [VOCl4]- anions with symmetry C4v. The extremely short VO bond length corresponds with a VO triple; its steric requirements cause the relatively large bond angle OVCl of 103.4°.

Synthesen und Kristallstrukturen von [PPh3Me]NO2 und [PPh3 Me]HCO2H2O / Syntheses and Crystal Structures of [PPh3Me]NO2 and [PPh3Me]HCO2H2O

1988 ◽  
Vol 43 (10) ◽  
pp. 1279-1284 ◽  
Author(s):  
Mervat El Essawi ◽  
H Gosmann ◽  
D Fenske ◽  
F Schmock ◽  
K Dehnicke
Keyword(s):  
Crystal Structure ◽  
Aqueous Solutions ◽  
Ir Spectra ◽  
Bond Angle ◽  
Water Molecules ◽  
Moist Air ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Structure Determinations

Triphenylmethylphosphonium nitrite and formate have been prepared by the reaction of [PPh3Me]I with silver nitrite, and lead formate, respectively, in aqueous solutions. [PPh3Me]NO2 (1) forms pale yellow crystals, and [PPh3Me]HCO2·H2O (2) forms white crystals. Both compounds are soluble in water, ethanol, and dichloromethane. In moist air 2 is hydrated to yield [PPh3Me]HCO2·2H2O (3). The compounds were characterized by their IR spectra, 1 and 2 also by X-ray crystal structure determinations.[PPh3Me]NO2 (1): space group P21/n, Z = 4, 2088 independent observed reflexions, R = 0.062. Lattice dimensions (20 °C): a = 914.7(3), b = 1887.5(9), c = 1080.0(4) pm, β = 110.29(3)°. The compound consists of PPh3Me+ ions and NO2- anions with bond lengths of 114.2(6) pm and a bond angle of 124.1(7)°. [PPh3Me]HCO2·H2O (2): space group P21/n, Z = 4, 2973 independent observed reflexions, R = 0.069. Lattice dimensions (-20 °C): a = 931(2), b = 1558(3), c = 1281(2) pm, β = 105.9(1)°. The compound consists of PPh3Me+ ions and formate anions which form centrosymmetric dimeric units [HCO2·H2O]22- through hydrogen bridges of the water molecules. Bond lengths CO 122.4(4) and 120.9(4) pm. bond angle OCO 129.9(4)°.

[ 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.

Formamidinhim-Hexachloroferrat(III) Synthese und Kristallstruktur / Formamidinium-Hexachloroferrate(III) Synthesis and Crystal Structure

1985 ◽  
Vol 40 (3) ◽  
pp. 443-446 ◽  
Author(s):  
Udo Demant ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
The Other ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Lattice Constants ◽  
Bond Lengths

[HC(NH2)2]3FeCl6 was obtained together with other products from the reaction of S4N4 with HCl in H2CCl2 in the presence of FeCl3. Its crystal structure was determined from X-ray diffraction data (473 independent observed reflexions, R = 0.047). Lattice constants: a = 961.6, c = 876.4 pm; tetragonal, space group P42/m, Z = 2. Of the two crystallographically independent formamidinium ions HC(NH2)2⊕, one exhibits positional disorder; the other one has C-N bond lengths of 128 pm. The FeCl63⊖ ions have symmetry C2h, but the deviation from Oh is small.

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).

Filling up another Gap: Synthesis and Crystal Structure of Ba2H3I

2011 ◽  
Vol 66 (11) ◽  
pp. 1087-1091 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Title Compound ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

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

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