Notizen: Darstellung und Eigenschaften von und Reaktionen mit metallhaltigen Heterocyclen, LXXXI Synthese und Kristallstruktur eines Phospha-arsa-mangana-cyclopropans / Metal-Containing Heterocycles: Preparation, Properties, and Reactions, LXXXI Synthesis and Crystal Structure of a Phospha-arsa-mangana-cyclopropane

1992 ◽  
Vol 47 (12) ◽  
pp. 1798-1800 ◽  
Author(s):  
Ekkehard Lindner ◽  
Paul Fisahn ◽  
Riad Fawzi ◽  
Manfred Steimann

The phospha-arsa-mangana-cyclopropane (OC)4Mn–PPh2–AsAr (4) [Ar = 2,4,6-(t-Bu)3C6H2] is obtained in a one-pot reaction proceeding in the sequence Mn2(CO)10 → HMn(CO)5 (1) → HMn(CO)4PPh2H (2) → Li2[(OC)4Mn—⃛PPh2] (3) → 4. According to an X-ray structural analysis 4 has a short P–As bond (229 pm) and a long Mn–As distance (262 pm).

2014 ◽  
Vol 2014 ◽  
pp. 1-5 ◽  
Author(s):  
Tsugiko Takase ◽  
Dai Oyama

Reaction of square planar [PtII(C≡CPh)(tpy)]+ (tpy = 2,2′:6′,2′′-terpyridine) with bromine at low temperature provides a general route for the synthesis of octahedral alkynyl(terpyridine)platinum(IV) complex. In this first example of alkynyl(terpyridine)platinum(IV) complex, the alkynyl group is situated in trans position relative to the central nitrogen atom of the terpyridine ligand, and the two bromido ligands are situated in trans positions; an X-ray structural analysis has been completed for trans(Br)-[PtIVBr2(C≡CPh)(tpy)]+.


1998 ◽  
Vol 53 (10) ◽  
pp. 1135-1143 ◽  
Author(s):  
Wolfgang Weigand ◽  
Veronika Plener ◽  
Heinrich Nöth ◽  
Ingo Krossing ◽  
Jörg Knizek ◽  
...  

AbstractThe 1,1-ethene dithiolato ligands (dithioylidene barbituric acids) 2a-f react with palladium(II) and platinum(II) compounds L2MCI2 [M = Pd, Pt; L = PEt3, PBu3, PPh3, 1/2 dppe, 1/2 (-)-DIOP, 1/2 2,9-dimethyl phenanthroline] to give the 1,1-ethene dithiolato metal complexes . Compound 4a forms a 1:1 adduct (8) with 2,6-diaminopyridine. The compounds were characterised on the basis of their IR and NMR (1H, 13C, 31P) spectra. Complexes 4a, 4c, and 5a were further studied by X-ray structural analysis. The barbituric unit in 4a undergoes self-assembly through multiple hydrogen-bonding with complementary 2 ,6-diaminopyridine yielding the supramolecular complex 8


2020 ◽  
Vol 17 (8) ◽  
pp. 624-627
Author(s):  
Sujata V. Bhat ◽  
Rohan S. Pawar ◽  
P. Rajakannu

One-pot tandem oxidation and double Diels-Alder reaction of myrcene or ocimene with in situ generated 1,4-benzoquinone or 1,2-benzoquinone at 0°C for 1.5 h yielded polyalkylated 1,4,4a,5,8,8a,9a,10a-octahydro-9,10-anthracenediones and bis(alkylated) 9,10-phenanthrenedione respectively. The structure of novel bis-adduct from ocimene, (1R,4aR,5S,8aS,9aS,10aR)-rel- 1,4,4a,5,8,8a,9a,10a-octahydro-2,6-dimethyl-1,5-bis(3-methyl-2-buten-1-yl)-9,10-anthracenedione, was elucidated through single crystal X-ray analysis.


2019 ◽  
Vol 74 (4) ◽  
pp. 357-363
Author(s):  
Daniela Vitzthum ◽  
Hubert Huppertz

AbstractThe mixed cation triel borate Ga4In4B15O33(OH)3 was synthesized in a Walker-type multianvil apparatus at high-pressure/high-temperature conditions of 12.5 GPa and 1300°C. Although the product could not be reproduced in further experiments, its crystal structure could be reliably determined via single-crystal X-ray diffraction data. Ga4In4B15O33(OH)3 crystallizes in the tetragonal space group I41/a (origin choice 2) with the lattice parameters a = 11.382(2), c = 15.244(2) Å, and V = 1974.9(4) Å3. The structure of the quaternary triel borate consists of a complex network of BO4 tetrahedra, edge-sharing InO6 octahedra in dinuclear units, and very dense edge-sharing GaO6 octahedra in tetranuclear units.


2013 ◽  
Vol 803 ◽  
pp. 80-84
Author(s):  
Yu Qi Liu ◽  
Yong Yang ◽  
Rui Yang ◽  
Xiao Jun Xu

A novel metalorganic coordination polymer, namely [Co3(bpd)5.5(NCS)6(NH3)]n2H2O (1) (bpd=1,4-bis (4-pyridyl)-2,3-diaza-1,3-butadiene), has been synthesized and characterized by elemental analyses, infrared spectroscopy, and single-crystal X-ray diffraction. Compound 1 presents 2D[3,4,-connected 3-nodal net with the point symbol (4268210)(4462)(8210). In addition, four identical 2D single nets is interlocked with each other in parallel, thus directly leading to the formation of a polycatenated layer (2D2D).


2013 ◽  
Vol 28 (1) ◽  
pp. 13-17 ◽  
Author(s):  
F. Laufek ◽  
A. Vymazalová ◽  
D.A. Chareev ◽  
A.V. Kristavchuk ◽  
J. Drahokoupil ◽  
...  

The (Ag,Pd)22Se6 phase was synthesized from individual elements by silica glass tube technique and structurally characterized from powder X-ray diffraction data. The (Ag,Pd)22Se6 phase crystallizes in Fm$\overline3$m symmetry, unit-cell parameters: a = 12.3169(2) Å, V = 1862.55(5) Å3, Z = 4, and Dc = 10.01 g/cm3. The crystal structure of the (Ag,Pd)22Se6 phase represents a stuffed 3a.3a.3a superstructure of the Pd structure (fcc), where only 4 from 108 available octahedral holes are occupied. Its crystal structure is related to the Cr23C6 structure type.


1995 ◽  
Vol 73 (1) ◽  
pp. 95-99 ◽  
Author(s):  
Frank E. Smith ◽  
Rosemary C. Hynes ◽  
John Tierney ◽  
Ying Z. Zhang ◽  
George Eng

The title compound was synthesized as part of an effort to produce a more effective fungicide to combat Dutch Elm Disease (DED), which is caused by the fungus Ceratocystisulmi. A full X-ray structural analysis of the 1:1 adduct has been carried out and the results are reported along with the Mössbauer data for the compound. The crystals are monoclinic, space group P21/a with a = 19.240(3) Å, b = 9.1463(24) Å, c = 19.3512(24) Å, β = 118.874(8)°, V = 2982.0(10) Å3, z = 4, and Dcalc = 1.427 Mg m−3. The final discrepancy factors are RF = 0.056 and Rw = 0.058 for 1915 significant reflections. The QS and IS values in the Mössbauer spectrum of the complex are 3.08 mm s−1 and 1.28 mm s−1, respectively. The 2,3-diphenylthiazolidin-4-one behaves as a monodentate ligand and coordinates to the tin through the oxygen atom. The complex exhibits a trigonal bipyramidal configuration with the three phenyl groups in equatorial positions and the chloride and ligand oxygen occupying the apical sites. Keywords: triorganotin, fungicide, Dutch Elm Disease, thiazolidin-4-one.


2000 ◽  
Vol 53 (3) ◽  
pp. 225 ◽  
Author(s):  
Zdenek Smékal ◽  
Zdenek Trávnícek ◽  
Jaromír Marek ◽  
Milan Nádvornik

Five new complexes of compositions [Cu(1,2-pn)2Fe(CN)5NO]·H2O (1,2-pn = propane-1,2-diamine) and [Cu(L)Fe(CN)5NO]·xH2O (L = tmen (N,N,N′,N′-tetramethylethane-1,2-diamine), x = 0.5; L = trimeen (N,N,N′-trimethylethane-1,2-diamine), x = 1; L = dien (N-(2-aminoethyl)ethane-1,2-diamine), x = 0; L = medpt (N-(3-aminopropyl)-N-methylpropane-1,3-diamine), x = 2) have been isolated from the reaction mixture of Cu(ClO4)2·6H2O (or CuCl2·2H2O), the amine and Na2 [Fe(CN)5NO]·2H2O in water. The complexes have been characterized by infrared and ultraviolet–visible spectroscopies, and magnetic measurements. Single-crystal X-ray structural analysis revealed that the [Cu(1,2-pn)2Fe(CN)5NO]·H2O complex assumes a cyanide-bridged binuclear structure in which iron(II) is six-coordinated by five cyanide ligands and one nitrosyl group (the nitrosyl group lies cis to the bridging cyanide group), while copper(II) is five-coordinated by two propane-1,2-diamine ligands and a bridging cyanide ligand in a distorted tetragonal pyramidal arrangement.


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