σ-Ferrocenyl-Komplexe der frühen Übergangsmetalle – Synthese und Struktur / σ-Ferrocenyl Complexes of the Early Transition Metals – Synthesis and Structure

1988 ◽  
Vol 43 (11) ◽  
pp. 1461-1467 ◽  
Author(s):  
Michael Wedler ◽  
Herbert W. Roesky ◽  
Frank T. Edelmann ◽  
Ulrich Behrens
Keyword(s):  
Transition Metals ◽  
Structure Analysis ◽  
Monoclinic Space Group ◽  
Substitution Product ◽  
Carbon Bond ◽  
Space Group ◽  
X Ray ◽  
Sterically Demanding ◽  
Cp Ti ◽  
Early Transition

Abstract Ferrocenyllithium, FcLi (1), reacts with (C5H4CH3)2TiCl2, CpTiCl, and Cp*TiCl 3 to give the new σ-ferrocenyl complexes (C5H4CH3)2TiFc2 (2), CpTiFc3 (3) and Cp*Ti(Fc)2Cl (4), respectively. Treatment of Cp*2ZrCl2 with FcLi yields the mono-substitution product Cp*2Zr(Fc)Cl (5), which has been characterized by an X-ray structure analysis. Compound 5 crystallizes in the monoclinic space group P21/c (a = 1622.3(6), b = 995.0(2), c = 1664.3(6) pm; β = 94.78(3)°; Z = 4). Due to the sterically demanding pentamethylcyclopentadienyl ligands 5 contains a long zirconium-carbon bond (231.4(8) pm) and the Cp rings of the ferrocenyl substituent are tilted by 10.2°. The syntheses of CpZrFc3 (6), Cp*HfFc3 (7) and Cp2VFc2 (8) are also described.

Zur Darstellung und Struktur des 1.3-Dichloro-5-N.N-dimethylamino-1.3-dithia-2.4.6-triazins / Synthesis and Structure of 1,3-Dichloro-5-N,N-dimethylamino-1,3-dithia-2,4,6-triazine

1983 ◽  
Vol 38 (3) ◽  
pp. 347-349 ◽  
Author(s):  
Herbert W. Roesky ◽  
Pierre Schäfer ◽  
Mathias Noltemeyer ◽  
George M. Sheldrick
Keyword(s):  
Structure Analysis ◽  
Nmr Spectra ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cl Atoms ◽  
C Nmr

Abstract The six membered ring of composition (CH3)2NCN3S2Cl2 3 a was prepared from N,N-dimethylguanidinhydrochloride and trithiadiazindichloride. 3 a was characterized on the basis of mass, 1H, 13C NMR spectra and X-ray structure analysis. Crystals of 3 a are monoclinic, space group P21/c, with a = 660.3(6), b = 834.5(7), c = 1774.7(15) pm, β = 112.83(6)° and Z = 4. The C2N unit lies approximately in the plane of the [-CNSNSN-] ring, with both Cl atoms on the same side of the ring.

scholarly journals Preparation and Crystal Structure of Zinc Bis[orotate(1–)] Octahydrate

1993 ◽  
Vol 48 (7) ◽  
pp. 961-964 ◽  
Author(s):  
Otto Kumberger ◽  
Jürgen Riede ◽  
Hubert Schmidbaur
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Medical Treatment ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Structure Analysis ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

A discrete zinc bis[orotate(1—)] complex of the composition Zn(OrH)2·8 H2O has been isolated and characterized by a single-crystal X-ray structure analysis. The crystals are monoclinic, space group P21/c (No. 14), Z = 2, a = 10.884(2), b = 12.896(1), c = 6.954(1) Å, β = 98.27(1)°. The crystal lattice features hexaquo complexes of zinc, the Zn(H2O)62+ cations being associated with two hydrated OrH- ions only through hydrogen bonds. The results are relevant for applications of zinc orotates in medical treatment.

Preparation and Crystal Structure Determination of [(C2Η5)4N]2Hg3Cl8

1995 ◽  
Vol 50 (1) ◽  
pp. 66-70 ◽  
Author(s):  
Inge Pabst ◽  
Peter Sondergeld ◽  
Mirjam Czjzek ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Analysis ◽  
Structure Determination ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Coordination Type ◽  
X Ray

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.

scholarly journals Darstellung und Charakterisierung der μ3-Oxo-Cluster [Cp3Mo3(CO)4µ-Cl)(µ3-O)] und [Cp3Mo3(µ-CO)3(CO)3(µ3-O)]+ / Synthesis and Characterization of the µ3-Oxo Clusters [Cp3Mo3(CO)4μ-Cl)(μ3-O)] and [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+

1990 ◽  
Vol 45 (4) ◽  
pp. 508-514 ◽  
Author(s):  
B. Nuber ◽  
W. Schatz ◽  
M. L. Ziegler
Keyword(s):  
Structure Analysis ◽  
Elemental Analysis ◽  
Spectroscopic Data ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

[CpMo(CO)3]2 (1) (Cp = cyclopentadienyl) reacts with InCl3 in diglyme to yield the oxo-cluster [Cp3Mo3(CO)4(μ-Cl)(μ3-O)] (2) and the cationic oxo-cluster [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+ as the salt [Cp3Mo3(μ-CO)3(CO)3(μ3-O)][CpMo(CO)3InCl3] (3). The compounds were characterized by elemental analysis, spectroscopic data and X-ray structure analysis. Compound 2 crystallizes in the orthorhombic space group P212121 with a = 1006.0(3), b = 1244.6(4) and c = 1600.8(5) pm, V = 2004.3 x 106 pm3, Z = 4. Compound 3 crystallizes in the monoclinic space group P 21/m with a = 874.4(8), b = 1407(1) and c = 1500(1) pm, β = 92.95(6) , V = 1843 × 106 pm3, Z = 2.

Oxidative S-S-Kopplung von 1,2-Dithiooxalat durch intramolekulare Redoxreaktion der Selen(II)- und Tellur(II)-Komplexe/Oxidative S-S Coupling of 1,2-Dithiooxalate by Intramolecular Redox Reaction of the Selenium (II) and Tellurium(II) Complexes

1999 ◽  
Vol 54 (1) ◽  
pp. 73-76 ◽  
Author(s):  
U. Drutkowski ◽  
P. Strauch
Keyword(s):  
Structure Analysis ◽  
Redox Reaction ◽  
Main Product ◽  
Methanol Solution ◽  
Redox Process ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Coordination Center ◽  
Reaction In Solution

The reaction of sodium monochalcogenopentathionates, Na2[Y(S2O3)2] (Y = Se, Te) with potassiumdithiooxalate in a water/methanol solution in presence of large cations (e. g. Ph4P+, Ph4As+ or BzlPh3P+) yields complexes of the type [Y(dto)2]2- (Y = Se, Te). These complexes are of limited stability and undergo a redox reaction in solution. As the main product of this redox process the 3,4-dithiahexane-2,5-dione-1,6-di(thiocarboxylate) was isolated and characterized by X-ray structure analysis as the benzyltriphenylphosphonium salt (monoclinic space group P2J/c, Z = 2, a = 8.899(5) Å, b = 16.458(2) Å, c = 16.034(6) Å and β = 98.02(2)°). With Te2+ (Y = Te) as the coordination center we have been able to isolate the intermediate complex (Ph4P)2[Te(dto)2].

Reaktionen N-silylierter Endiamine, I Übergangsmetallkomplexe von 1,3-Diaza-2-sila-4-cyclopentenen / Reactions of N-Silated Endiamines, I Transition Metal Complexes of 1,3-Diaza-2-sila-4-cyclopentenes

1986 ◽  
Vol 41 (10) ◽  
pp. 1230-1238 ◽  
Author(s):  
Michael Zettlitzer ◽  
Heindirk tom Dieck ◽  
Lutz Stamp
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Structure Analysis ◽  
Transition Metal Complexes ◽  
Structural Data ◽  
Spectroscopic Properties ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Poorly Soluble

Abstract1,3-Di̲aza-2-s̱ila-4-c̱yclopentenes 1 (DISC), which are electron-rich and easily oxidizable ole­ fins, form strongly coloured, but poorly soluble 1:1 adducts with cuprous halides, while silver trifluoromethylsulfonate oxidizes 1. Much more soluble and again strongly coloured complexes of stoichiometry LPdX2, (L)1.5PdX2 and L 2PdX2 are formed from 1 and palladium halides. The well-crystallizing adduct (PdCl2 · L)2 3a was chosen for an X-ray structure analysis (monoclinic, space group P2/c; a = 10.215(3), b = 14.681(3), c =23.642(5) Å , β = 101.31(2)°; Z = 8 ; R = 0.054), which revealed an almost planar DISC ligand in an oblique η2(C=C)-coordination relative to the π-plane. Structural data and rather peculiar spectroscopic properties encourage a comparison of 3a with complexes, in which an electron-rich olefin is split to give a bis(carbene) ligand system. The electronic reasons for the splitting of electron-rich olefins at d8 metals are discussed under symmetry considerations.

Synthesis and crystal structures of β-[Be(DMF)4]I2, [Be(Pyr)4]I2, [Be(NMP)4]I2 and [BeI2(Lut)2]

2020 ◽  
Vol 75 (5) ◽  
pp. 509-516 ◽  
Author(s):  
Timotheus Hohl ◽  
Torben Sinn ◽  
Constantin Hoch
Keyword(s):  
Crystal Structures ◽  
Dimethyl Formamide ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Neutral Complex ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Sterically Demanding ◽  
Methyl Pyrrolidone

AbstractFour solvent complexes of beryllium iodide were prepared by dissolving BeI2 in N,N-dimethyl formamide (DMF), pyridine (Pyr), N-methyl pyrrolidone (NMP) and 2,6-dimethyl pyridine (2,6-lutidine, Lut). Their crystal structures were established from single crystal X-ray diffraction. For [Be(DMF)4]I2 a new modification is reported (monoclinic, space group P21/c, a = 12.491(2), b = 11.593(2), c = 15.310(3) Å, β = 94.7073(6)°). In [Be(Pyr)4]I2 (monoclinic, space group C2/c, a = 17.8799(13), b = 7.6174(5), c = 18.2611(14) Å, β = 113.508(4)°) and [Be(NMP)4]I2 (orthorhombic, space group Pbca, a = 13.941(5), b = 15.754(3), c = 24.634(7) Å) homoleptic tetrahedral complex cations are formed, while the sterically demanding solvent ligand Lut yields a neutral complex with covalently bound iodine ligands [BeI2(Lut)2] (monoclinic, space group P21/c, a = 7.8492(9), b = 24.265(3), c = 27.037(3) Å, β = 97.076(3)°). Their electrochemical stability with respect to their application as beryllium electrolytes for deposition of beryllium from solution is discussed.

Tris(benzoyl-thiobenzoyl-methanato-O,S)indium, a Conformer of a Facial Isomer

1989 ◽  
Vol 44 (2) ◽  
pp. 149-152 ◽  
Author(s):  
Vishnu D. Gupta ◽  
Anil K. Mishra ◽  
Heinrich Nöth ◽  
Kurt Polborn
Keyword(s):  
Structure Analysis ◽  
Indium Atom ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Oxygen Atoms

Abstract A second modification o f the title com pound has been isolated and characterized by an X-ray structure analysis. It crystallizes in the monoclinic space group P21/c. The indium atom is hexacoordinated and surrounded by three sulfur and three oxygen atoms in a facial arrangement as has been found for a previously known isomer. However, the phenyl groups adopt a different orientation, hence it is a rotamer.

Ein neuer Wasserstoffbrücken-Typ: Intramolekulare S—H···S-Brücken in Dithiotropolon / A Novel Type of Hydrogen Bond: Intramolecular S—H···S-B ridges in Dithiotropolone

1984 ◽  
Vol 39 (1) ◽  
pp. 43-49 ◽  
Author(s):  
Bernt Krebs ◽  
Gerald Henkel ◽  
Wolfgang Stücker
Keyword(s):  
Hydrogen Bond ◽  
Single Crystal ◽  
Structure Analysis ◽  
Monoclinic Space Group ◽  
Bridge Bond ◽  
Space Group ◽  
X Ray ◽  
Sh Group ◽  
Group A

In dithiotropolone (2-mercaptocycloheptatrienethione) a novel type of S - H···S hydrogen bond is observed from spectroscopic results and from a single crystal X-ray structure analysis. Intramolecular S-H···S bonds with a very short S ··· S separation of 3.13 Å and with d(S···H) = 2.10 Å, ∢ (S-H···S) = 136° are formed, the S-H stretching frequency of 2450 cm-1 being lowered by about 120 cm-1 from the value for the free SH group. A different relationship between S···S bridge bond distances and S-H stretching frequencies applies as compared to the intermolecular bridges of thiophosphinic and thiocarbonic acids. Crystalline dithiotropolone is monoclinic, space group P21/c, Z = 8, with a = 8.352(2), b = 13.806(4), c = 12.371(2) Å, β= 103.46(2)°.

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

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