scholarly journals Transition metal complexes with thiosemicarbazide-based ligand: Part 45 - Synthesis, crystal and molecular structure of [2, 6-diacetylpyridine bis(S-methylisothiosemicarbazonato)]diazide-iron(III)

2003 ◽  
Vol 68 (4-5) ◽  
pp. 425-433 ◽  
Author(s):  
Vukadin Leovac ◽  
Vladimir Divjakovic ◽  
Valerija Cesljevic ◽  
Refik Fazlic
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Transition Metal Complexes ◽  
Equatorial Plane ◽  
Crystal And Molecular Structure ◽  
Crystal Data ◽  
X Ray ◽  
High Spin Complex ◽  
Spin Complex ◽  
Template Reaction

The template reaction of a warm methanolic solution of FeCl3.6H2O S-methylisothiosemicarbazidehydroiodide and 2,6-diacetylpyridine in the presence of LiOAc and NaN3 yielded the high-spin complex [Fe(HL)(N3)2], were HL is the monoanion of the ligand 2,6-diacetylpyridine bis(S-methylisothiosemicarbazone). X-Ray analysis of the complex showed its pentagonal-bipyramidal configuration, with pentadenate (N5) HL in the equatorial plane and two monodentate azide groups in the axial positions. Crystal data are: monoclinic, P21/c,a=1.0263(2), b = 1.2525(2), c = 1.6660(3) nm, ?= 98.94?, V = 2.1154 nm3, Z = 4, ?x = 1.499 g cm-3, ?0 = 1.48 g cm-3, F(000) = 984, ?= 9.40 cm-1.

Gehinderte Ligandbewegungen in Übergangsmetallkomplexen, XXXVII [1]: Photoreaktion von Dekacarbonyldirhenium mit Phenylallen / Hindered Ligand Motions in Transition Metal Complexes, XXXVII [1]: Photoreaction of Decacarbonyldirhenium with Phenylallene

1990 ◽  
Vol 45 (6) ◽  
pp. 793-802 ◽  
Author(s):  
Cornelius G. Kreiter ◽  
Wolfgang Michels ◽  
Reiner Exner
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Transition Metal ◽  
Transition Metal Complexes ◽  
Crystal And Molecular Structure ◽  
Dinuclear Complexes ◽  
Rotation Barrier ◽  
Single Bond ◽  
Hindered Rotation ◽  
X Ray

Decacarbonyldirhenium (1) and phenylallene (2) form upon UV irradiation four dinuclear complexes: Decacarbonyl-μ-η1:1-(3,4-diphenyl-1,5-hexadien-2,5-diyl)-dirhenium (3), enneacarbonyl-μ-ηl:3-(3-phenyl-2-propen-1,2-diyl)-dirhenium (4), octacarbonyl-μ-hydrido-μ-η1:2-(3-phenyl-1,2-propadien-l-yl)-dirhenium (5) and octacarbonyl-μ-η2:2-(phenyl-1,2-propadiene)-dirhenium (6). The thermolabile complex 4 looses CO and forms the phenylallene bridged compound 6. Similarly 5 is rearranged to 6 by transfer of the hydrido ligand to the 3-phenyl-1,2-propadien-1-yl bridge. The formation of 3 and 4 can be rationalized via pentacarbonyl-phenylpropenediyl-rhenium radicals which dimerize to give 3 or add pentacarbonylrhenium radicals, loose CO and form 4. The crystal and molecular structure of 3 was determined by X-ray structure analysis. In the solid state the molecule is present in the ± ap conformation. In solution at 233 K the ±ap, +sc, and –sc conformations are equally populated. By a hindered rotation around a CC single bond, the three conformers are interconverted with a rotation barrier of ΔG*258 = 52.3 ± 1 kJ · mol-1.

scholarly journals Transition metal complexes with thiosemicarbazide-based ligands. Part 51. Square-planer nickel(II)complex with acetylacetone bis(S-n-propylisothiosemicarbazone)(L).Crystal and molecular structure of [

2006 ◽  
Vol 71 (6) ◽  
pp. 593-604 ◽  
Author(s):  
Vukadin Leovac ◽  
Vladimir Divjakovic ◽  
Valerija Cesljevic ◽  
Milena Rakocevic
Keyword(s):  
Molecular Structure ◽  
Structural Analysis ◽  
Transition Metal ◽  
Metal Complexes ◽  
Crystal Structures ◽  
Transition Metal Complexes ◽  
Crystal And Molecular Structure ◽  
Square Planar ◽  
Significant Difference ◽  
Template Reaction

The template reaction of a warm methanolic solution of Ni(OAc)2?4H2O S-n-propylisothiosemicarbazide hydroiodide and acetylacetone yielded the needle- like, brown, diamagnetic complex [Ni(L-H)]I?MeOH, and in the presence of an excess of NH 4NCS, brown, prismatic crystals of the complex [Ni(L-H)]NCS (1), both compounds involving the monoanionic form of the ligand, acetylacetone bis(S-n-propylisothiosemicarbazone), L. Slow recrystallization fromMeOH, EtOH, iPrOH and Me2CO gave the corresponding monosolvent complexes [Ni(L-H)]I?solvent, of which only those involving EtOH and iPrOH were suitable for structural analysis. The crystallographic parameters of [Ni(L-H)]I?EtOH (2) and [Ni(L-H)]I?iPrOH (3) are very similar to each other, showing their structures are isomorphic. The crystal structures of the title compounds consist of the independent ions: NCS-, or I-, and the chemically identical cation [Ni(L-H)]+, where L-H is the monoanion resulting from deprotonation of the acetylacetone moiety, a tetradentate N4 ligand forming a square-planar coordination around a Ni(II) ion. It was found that the isothiosemicarbazide fragment of the ligand has an imido form. The complex cations of the compounds [Ni(L-H)]NCS and [Ni(L-H)]I?EtOH exhibit significant difference only in the conformation of their propyl groups.

Gehinderte Ligandbewegungen in Übergangsmetallkomplexen, XLII [1]: Photoreaktionen von Hexacarbonyl-μ-η5:5-fulvalen-dimolybdän und -diwolfram mit konjugierten Dienen / Hindered Ligand Movements in Transition Metal Complexes, XLII [1]: Photoreactions of Hexacarbonyl-μ–η5:5-fulvalene-dimolybdenum and -ditungsten with Conjugated Dienes

1993 ◽  
Vol 48 (11) ◽  
pp. 1635-1650 ◽  
Author(s):  
Cornelius G. Kreiter ◽  
Wolfgang Conrad ◽  
Reiner Exner
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Diffraction Analysis ◽  
Transition Metal Complexes ◽  
Energy Barrier ◽  
Crystal And Molecular Structure ◽  
Conjugated Dienes ◽  
Photochemical Reactions ◽  
X Ray Diffraction ◽  
X Ray

Photochemical reactions of hexacarbonyl-μ-η5:5-fulvalene-dimolybdenum (1) with 1,3-butadiene (a), 2-methyl-1,3-butadiene (b), E-1,3-pentadiene (c), 2,3-dimethyl-1,3-butadiene (d), and E-3-methyl-1,3-pentadiene (e) yield the corresponding tetracarbonyl-η4-s-cisdiene-μ-η5:5-fulvalene-dimolybdenum complexes 3a-3e. In addition to 3a also η4-s-trans1,3-butadiene-tetracarbonyl-μ-η5:5-fulvalene-dimolybdenum (4) is formed. Similarily hexacarbonyl-μ-η5:5-fulvalene-ditungsten (2) forms with a and b tetracarbonyl-η4-s-cis-diene-μ-η5:5-fulvalene-ditungsten (5a, 5b) and bis(η4-s-cis-1,3-butadiene)-dicarbonyl-μ-η5:5-fulvalene-ditungsten (6). The complexes 3b —3e and also 5b are obtained as mixtures of the o- and u-isomers. Only for tetracarbonyl-η4-cis-2,3-dimethyl-1,3-butadiene-μ-η5:5-fulvalene-dimolybdenum (3d) an interconversion of the o- and u-isomers is observed with an energy barrier of ΔG183# = 73.9 kJ/mol. Both isomers of 3d show hindered inversions with energy barriers of ΔG#313 = 66.1 kJ/mol (u-3d) and ΔG183# = 36.4 kJ/mol (o-3d). For o-3d the crystal and molecular structure was determined by an X-ray diffraction analysis. Hexacarbonylµ — η5:5-bis(cyclopentadiendiyl)methane-dimolybdenum (7), hexacarbonyl-μ-η5:5-bis(cyclopentadiendiyl)ethane-dimolybdenum and hexacarbonyl-μ-η5:5-bis(cyclopentadiendiyl)propane-dimolybdenum do not react with conjugated dienes. Upon UV irradiation 7 looses CO and forms by dimerization octacarbonyl-bis(μ-η5:5-(cyclopentadiendiyl-cyclopentadien-triyl)methane)-dihydrido-tetramolybdenum (8).

Heavy transition metal complexes of biologically important molecules. I. The crystal and molecular structure of trans-dichloro(bis(isopropyl)-sulfoxide-S)(1-methylcytosine-N)platinum(II)

1976 ◽  
Vol 54 (1) ◽  
pp. 53-58 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Robert Anthony Speranzini ◽  
John Powell
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Metal Complexes ◽  
Single Crystal ◽  
Least Squares ◽  
Transition Metal Complexes ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray

The crystal and molecular structure of trans-dichloro(bis(isopropyl)sulfoxide-S)(1-methylcytosine-N)platinum(II) has been determined by single crystal X-ray diffraction. The crystals are triclinic with a = 16.205(5), b = 8.078(2), c = 6.776(2) Å, α = 106.53(2), β = 96.35(2), γ = 98.54(2)°. The space group is [Formula: see text] and there are two molecules per unit cell. A total of 2294 independent reflections, of which 2023 were observed, were examined on a Syntex [Formula: see text] diffractometer. The structure was refined by full matrix least squares analysis to an R2 value of 0.0427. The ligands form a rough square around the platinum atom with Pt—Cl(1), 2.304(3), Pt—Cl(2), 2.287(4), Pt—S, 2.232(2), Pt—N, 2.058(7). Distances within the ligands are normal. The plane of the cytosine ring is at 84.4° to the plane formed by the ligands around platinum.

Synthesis and molecular structure of tetraphenylarsonium Tetrakis(benzenethiolato)-oxorhenate(V)-Acetonitrile (1/1)

1983 ◽  
Vol 36 (2) ◽  
pp. 253 ◽  
Author(s):  
AC McDonell ◽  
TW Hambley ◽  
MR Snow ◽  
AG Wedd
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Crystal Data ◽  
Rhenium Atom ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography

The salts Ph4As [ReO(SPh)4].MeCN and Ph4As [ReO(SePh)4] have been synthesized and characterized. The crystal and molecular structure of the thiolate compound has been determined by X-ray crystallography which reveals a square-pyramidal arrangement of ligand atoms around the central rhenium atom of the [ReO(SPh)4]- anion. Crystal data: a 9.756(4), b 18.171(3), c 25.684(4) �, space group P212121, Z 4.

Spaltung von S4N4 zu S2N2 bei Raumtemperatur: Darstellung und Struktur von S2N2 • 2AlBr3 / Cleavage of S4N4 to S2N2 at Room Tem perature: Preparation and Structure of S2N2 • 2AlBr3

1984 ◽  
Vol 39 (2) ◽  
pp. 145-148 ◽  
Author(s):  
Ulf Thewalt ◽  
Konrad Holl
Keyword(s):  
Molecular Structure ◽  
Room Temperature ◽  
Crystal And Molecular Structure ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths

The compound S2N2 • 2AlBr3 has been prepared by reaction of S4N4 with AlBr3 in 1,2-dibromoethane at room temperature. Its crystal and molecular structure have been determined by X-ray diffraction; R = 0.068. Crystal data: monoclinic, P 21/n, a = 9.594(5), b = 9.975(4), c = 7.528(4) Å , β = 111.36(5)°. The S2N2 ring of the centrosymmetrical complex is bonded via its nitrogen atoms to two AlBr3 units thus completing coordination tetrahedra around the Al atoms. Bond distances and angles within the S2N2 ring are d(S-N) = 1.629(13) and 1.651(13) Å, ∢ (S-N-S) = 95.8, and ∢ (N-S-N) - 84.2°. Whereas the S-N bond lengths agree closely with those of free S2N2, the angle at N is enlarged by ca. 5° and the angle at S is decreased by ca. 5°. The sulfur atoms form two close S···Br contacts of length 3.149 (intramolecular) and 3.193 (intermolecular) Å , respectively. The intermolecular attractive nonbonded S···Br interactions tie the complexes together in a way that leads to infinite chains which run parallel to the crystallographic z axis

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