Platinum(II) and Palladium(II) Dichalcogenolene Complexes Containing the Ligand Tri(1-cyclohepta-2,4,6-trienyl)phosphane. Molecular Structure, Intramolecular Dynamics in Solution, and the Absolute Signs of Coupling Constants 1J(195Pt, 77Se) and 2J(77Se, Pt, 31P)

2002 ◽  
Vol 57 (1) ◽  
pp. 53-60 ◽  
Author(s):  
Max Herberhold ◽  
Thomas Schmalz ◽  
Wolfgang Milius ◽  
Bernd Wrackmeyer
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Dynamic Process ◽  
Time Scale ◽  
Room Temperature ◽  
Coupling Constants ◽  
Intramolecular Dynamics ◽  
X Ray ◽  
The Absolute

Tri(1-cyclohepta-2,4,6-trienyl)phosphane, P(C7H7)3 (1), serves as a bidentate chelatinglig and [P] in platinum(II) and palladium(II) complexes. Here the synthesis of the four dichalcogenolene complexes [P]M[E2C2(CO2Me)2] (4) (M = Pt) and 5 (M = Pd) with E = S (a) and Se (b) from the reaction of the respective dicyclopentadienyltitanium dichalcogenolenes, Cp2Ti[E2C2(CO2Me)2], and [P]MCl2 with M = Pt (2) and Pd (3) is reported. At room temperature, the complexes 4 and 5 are fluxional with respect to the NMR time scale, and the nature of the dynamic process is discussed. The complexes have been characterised by 1H, 13C, 31P, 77Se and 195Pt NMR spectroscopy. The signs of the coupling constants 1J(195Pt, 77Se) (< 0) and 2J(77Se, 31P) (> 0) were obtained by selective 31P{195Pt} and 31P{77Se} spin tickling experiments. The crystal structure of 4b was determined by X-ray analysis.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

Nuclear magnetic resonance studies on the anions [M(SnCl3)5Cl]4− (M = Ru, Os) and [Ru(SnCl3)5(MeCN)]3−: the X-ray crystal structure of [N(C2H5)4]4[Ru(SnCl3)5Cl]

1982 ◽  
Vol 60 (11) ◽  
pp. 1304-1316 ◽  
Author(s):  
Louis J. Farrugia ◽  
Brian R. James ◽  
Claude R. Lassigne ◽  
Edward J. Wells
Keyword(s):  
Crystal Structure ◽  
Nuclear Magnetic Resonance ◽  
Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Octahedral Geometry ◽  
Coupling Constants ◽  
Order Effects ◽  
Magnetic Resonance Studies ◽  
X Ray ◽  
Crystallographic Study

The octahedral anions [M(SnCl3)5Cl]4− (M = Ru, Os) have been fully characterized by 119Sn FT nmr spectroscopy. For M = Ru, 117Sn and 115Sn nmr spectra were also recorded, and an X-ray crystallographic study was carried out on the tetraethylammonium salt, isolated as a disolvate from acetonitrile. The Ru—Sn bond lengths indicate some degree of dπ–dπ interactions. The slight distortions from octahedral geometry are discussed in connection with the packing of the chlorine atoms. The Sn nmr spectra reveal the first observed coupling to a 99Ru nucleus (I = 5/2, 12.7% natural abundance), very large 2J(119Sn—117Sn) coupling constants, and the first observed second-order effects on a heteronuclear system. The octahedral anion [Ru(SnCl3)5(MeCN)]3− was also synthesized as the tetraethylammonium salt and characterized spectroscopically.

Synthesis and X -Ray Crystal Structure of the Heterobimetallic Complex [FeRh (μ-CO)(CO)3((μ-PBut2)((μ-Ph2PCH2PPh2)]

1997 ◽  
Vol 52 (7) ◽  
pp. 810-814 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Kurt Merzweiler ◽  
Clemens Bruhn
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Room Temperature ◽  
Metal Carbonyl ◽  
Homogeneous Catalyst ◽  
Catalyst Precursor ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Heterobimetallic Complex

Abstract The reaction of the phosphido-bridged metal carbonyl [FeRh(CO)6(μ-PBut2)] (1) with dppm [dppm = bis(diphenylphosphino)methane] leads to the heterobimetallic complex [FeRh(μ-CO)(CO)3(μ-PBut2)(μ-dppm)] (2) in good yields. The molecular structure of 2 was determined at room temperature [triclinic, space group P1̄, a = 9.509(6), b = 13.637(5), c = 14.926(8) Å, α = 81.38(4), β = 82.75(4), γ = 71.25(4)°]. The compound acts as a homogeneous catalyst precursor in the hydroformylation reaction of ethylene, but it decomposes during this process.

A Domino Reaction for the Synthesis of Novel 1,3-Dihydrofuro[3,4-c]pyridines from Pyridoxal and Ketones

Synthesis ◽  
2020 ◽  
Vol 53 (02) ◽  
pp. 365-370
Author(s):  
Lucas Pizzuti ◽  
Izamara Casadia ◽  
Thalita O. Daher ◽  
Sidnei Moura ◽  
Davi F. Back ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
13C Nmr ◽  
Room Temperature ◽  
13C Nmr Spectroscopy ◽  
Domino Reaction ◽  
Alkyl Aryl ◽  
1H And 13C Nmr ◽  
X Ray ◽  
Pyridine Series

A convenient domino route for the synthesis of novel 1,3-dihydrofuro[3,4-c]pyridines from pyridoxal and alkyl, aryl or heteroaryl ketones under basic conditions is reported. A series of nine derivatives is obtained in 53–90% yields after stirring reactants for 48 hours at room temperature. Most products are easily isolated by filtration followed by recrystallization from ethanol. All products were fully characterized by FTIR, HRMS, and 1H and 13C NMR spectroscopy. The X-ray crystal structure of a representative example of the 1,3-dihydrofuro[3,4-c]pyridine series is also presented.

Lanthanide Complexes with Carbacylamidophosphates: The First Registration of Chelate Coordination of the Neutral Ligand Form in the Structure of Di-(N,Nf-tetramethyl-NM -benzoylphosphoryl- triamide)cerium(III) Nitrate

2000 ◽  
Vol 55 (7) ◽  
pp. 576-582 ◽  
Author(s):  
Katerina E. Gubina ◽  
Vladimir A. Ovchynnikov ◽  
Vladimir M. Amirkhanov ◽  
Helmut Fischer ◽  
Rüdiger Stumpf ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Coordination Compounds ◽  
Metal Ion ◽  
Lanthanide Complexes ◽  
Carbonyl Oxygen ◽  
Neutral Ligand ◽  
Crystal Data ◽  
X Ray

Abstract The coordination compounds of the general formula Ln(HL)2(NO3)3, (where Ln = La - Eu (without Pm), HL = C6H5C(O)NHP(O)[N(CH3)2]2, N,Nʹ-tetramethyl-Nʺ-benzovlphosphoryl-triamide) have been synthesized and characterized by means of IR, UV-VIS, 1H, 31P NMR spectroscopy, and X-ray analysis. The complexes are isostructural according to X-ray powder diffraction studies. The crystal structure of the cerium(lll) complex has been determined. Crystal data: monoclinic, P21/c, with a = 10.503(9), b = 15.62(2), c = 21.91(2) Å, β = 99.56(8)°, Z = 4, V = 3546(6) Å3, R1= 0.0550, wR2 = 0.1383 for 6970 unique reflections used. The complex has a molecular structure. Neutral phosphoryltriamide ligands are coordinated to the metal ion in a bidentate manner via phosphoryl and carbonyl oxygen atoms with formation of six membered chelate rings. The coordination polyhedron of the Ce atom is a sphenocorona; C.N. = 10 (4 O[HL] + 6 O [NO3-]).

Synthesis and Crystal and Molecular Structure of trans-Dichloro(ethanedial dioximato(1—)-N,N')(ethanedial dioxime-N,N')rhodium(III)

1989 ◽  
Vol 44 (1) ◽  
pp. 5-8
Author(s):  
Michel Mégnamisi-Bélombé
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Room Temperature ◽  
Crystal And Molecular Structure ◽  
Crystallographic Direction ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cl Atoms

Abstract trans-Dichloro(ethanedial-dioximato)(ethanediaI-dioxime)rhodium (III), RhCl2(GH)(GH2), has been synthesized and its structure determined by single crystal X-ray diffraction at room temperature. C4H7Cl2N4O4Rh, Mr = 348.94. monoclinic space group P21/ɑ; a = 10.543(3), b = 8.363(2), c = 11.512(3)Å ; β = 92.79(2)°; V = 1024Å3; Z = 4; Dc = 2.26 Mg m-3. Final Rw = 0.075 for 2035 reflections and 139 parameters. The coordination geometry around Rh is a dis­torted (4+2) octahedron, with four chelating N atoms lying in the equatorial plane and the two Cl atoms in the apical positions. The H atoms of the oxime groups are involved in relatively weak intramolecular O-H-O bridgings, as well as in very strong intermolecular bridgings which extend throughout the crystal structure and propagate nearly parallel to the [101] crystallographic direction.

Notizen: Synthese und Kristallstruktur von [OsCl4(CH3CN)2] · 1/2 CH3CN / Synthesis and Crystal Structure of [OsCl4(CH3CN)2] · 1/2CH3CN

1990 ◽  
Vol 45 (8) ◽  
pp. 1210-1212 ◽  
Author(s):  
Dieter Fenske ◽  
Gerhard Baum ◽  
Hans-Walter Swidersky ◽  
Kurt Dehnicke
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Room Temperature ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Slow Reaction ◽  
Moisture Sensitive

[OsCl4(CH3CN)2] · 1/2CH3CN has been prepared by the reaction of OsCl5 with acetonitrile in a slow reaction at room temperature, forming red, moisture sensitive crystals. The compound was characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1281 observed unique reflexions, R = 0.031. Lattice dimensions at 20 °C: a = 1032.5(5), b = 1356.0(7), c = 975.9(5) pm. The complex has a molecular structure, in which the osmium atom is octahedrally coordinated by four chlorine atoms and by two N-atoms of the ciscoordinated acetonitrile molecules. The included CH3CN molecules are disordered in two positions.

Synthesis and crystal structure of a homoleptic diruthenium complex containing tetra-2-pyridyl-1,4-pyrazine (tppz)

2017 ◽  
Vol 72 (10) ◽  
pp. 759-762 ◽  
Author(s):  
Marion Graf ◽  
Peter Mayer ◽  
Hans-Christian Böttcher
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Title Complex ◽  
Dinuclear Complex ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diruthenium Complex

AbstractTreatment of hydrated ruthenium(III) chloride with tetra-2-pyridyl-1,4-pyrazine (tppz) in refluxing ethoxyethanol afforded the homoleptic dinuclear complex [(tppz)Ru(μ-tppz)Ru(tppz)]4+ (1) besides small amounts of the species [Ru(tppz)2]2+. The title complex 1 was obtained as purple crystals and characterized as its hexafluoridophosphate salt by NMR spectroscopy, mass spectrometry and microanalyses. The molecular structure of 1(PF6)4 has been established by X-ray crystallography.

scholarly journals Synthesis of Six and Seven-membered Heterocyclic Molecules Containing an Adamantyl Fragment and an X-ray Crystal Structure of (E)-N-(adamantan-1-yl)-1-(3-nitrophenyl)methanimine

2020 ◽  
Vol 17 (1(Suppl.)) ◽  
pp. 0272
Author(s):  
Ahmed Shukkur
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
1H Nmr ◽  
Good Yield ◽  
1H Nmr Spectroscopy ◽  
X Ray ◽  
X Ray Crystallography ◽  
Heterocyclic Molecules ◽  
Citraconic Anhydride

       Our work included a synthesis of three new imine derivatives—1,3-thiazinan-4-one, 1,3-oxazinan-6-one and 1,3-oxazepin-4,7-dione—which contained an adamantyl fragment. These were produced via the condensation of the Schiff`s base (E)-N-(adamantan-1-yl)-1-(3-aryl)methanimine with 3-mercaptopropanoic acid; 3-chloropropanoic acid; and maleic, citraconic anhydride, respectively. These new imines were prepared via the condensation of adamantan-1-ylamine and 3-nitro-, 3-bromobenzaldehyde in n-BuOH. We obtained a good yield of products. FTIR, 1H NMR spectroscopy and C.H.N.S analysis were used to diagnostic the products. The molecular structure of (E)-N-(adamantan-1-yl)-1-(3-nitrophenyl)methanimine was confirmed by X-ray crystallography analysis.  

Di[(hydroxyalkyl)dimethylammonium] tris[benzene-1,2-diolato(2–)]silicates and their germanium analogs: syntheses, crystal structure analyses, and NMR studies

2000 ◽  
Vol 78 (11) ◽  
pp. 1380-1387
Author(s):  
Reinhold Tacke ◽  
Alistair Stewart ◽  
Joachim Becht ◽  
Christian Burschka ◽  
Ingo Richter
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Aqueous Solutions ◽  
Room Temperature ◽  
Model Systems ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
X Ray ◽  
Germanium Silicon ◽  
And Storage

Treatment of Si(OMe)4 with three molar equivalents of 1,2-C6H4(OH)2 (= 1,2-dihydroxybenzene) and two molar equivalents of HO(CH2)nNMe2 (n = 2, 3) in acetonitrile at room temperature yields the λ6Si-silicates (HO(CH2)nNMe2H)2(SiL3) (5: n = 2; 6: n = 3; L2– = 1,2-C6H4(O)22– (= benzene-1,2-diolato(2–))). The analogous λ6Ge-germanates (HO(CH2)nNMe2H)2(GeL3) (7: n = 2; 8: n = 3) were synthesized analogously starting from Ge(OMe)4. Compounds 5·2CH3CN and 6-8 were structurally characterized by single-crystal X-ray diffraction. In addition, aqueous solutions of the Si/Ge analogs 5/7 and 6/8 were studied by NMR spectroscopy. The title compounds may be regarded as model systems for the transport and storage of silicon in biological systems and as tools to investigate biosilification.Key words: hexacoordinate silicon, hexacoordinate germanium, silicon biochemistry

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