Thiocarbonyl Complexes of Rhenium. Part I.

1993 ◽  
Vol 48 (6) ◽  
pp. 771-777 ◽  
Author(s):  
Ulrich Abram ◽  
Bernd Lorenz
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Space Group ◽  
X Ray ◽  
Monomeric Complex ◽  
Structure Solution ◽  
R Value

Novel rhenium complexes with terminal thiocarbonyl groups have been synthesized from ReCl3(Me2PhP)3 and sodium diethyldithiocarbamate. mer-(Diethyldithiocarbamato)tris-(dimethylphenylphosphine)(thiocarbonyl)rhenium(I), mer-[Re(CS)(Me2PhP)3(Et2dtc)], and tris(diethyldithiocarbamato)(thiocarbonyl)rhenium(III), [Re(CS)(Et2dtc)3] have been studied by infrared and NMR spectroscopy, mass spectrometry and X-ray diffraction.mer-[Re(CS)(Me2PhP)3(Et2dtc)] crystallizes orthorhombic in the space group Pna21 with a = 1516.1(2), b = 2189.8(2) and c = 1035.6(1) pm. Structure solution and refinement converged at R = 0.042. The coordination geometry is a distorted octahedron. The Re—C bond length is found to be 184(2) pm.[Re(CS)(Et2dtc)3] crystallizes monoclinic in the space group P21/c with a = 962.2(6), b = 1744.0(2), c = 1537.4(6) pm and β = 96.21(1)°. The final R value is 0.028. In the monomeric complex the rhenium atom is seven-coordinate with an approximate pentagonal-bipyramidal coordination sphere and a rhenium-carbon distance of 181(1) pm.

scholarly journals Different Coordination Modes of a Tripod Phosphine in Gold(I) and Silver(I) Complexes

1999 ◽  
Vol 6 (4-5) ◽  
pp. 211-221 ◽  
Author(s):  
P. Sevillano ◽  
M. E. García ◽  
A. Habtemariam ◽  
S. Parsons ◽  
P. J. Sadler
Keyword(s):  
Mass Spectrometry ◽  
Infrared Spectroscopy ◽  
Nmr Spectroscopy ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Fab Mass Spectrometry ◽  
Intramolecular Distance ◽  
Spectroscopy Studies ◽  
Linear Coordination

The following gold(I) and silver(I) complexes of the tritertiary phosphine 1,1,1- tris(diphenylphosphinomethyl)ethane, tripod , have been synthesised: Au3(tripod)X3 [X = Cl(1), Br(2), I(3)]; [Au3  (tripod)2Cl2  ]Cl (4); Au(tripod)X [X = Br(5), I(6)]; Ag3(tripod)(NO3)3 (7), Ag(tripod)NO3 (8). They were characterized by X-ray diffraction (complexes 2, 3 and 4), P31 NMR spectroscopy, electrospray and FAB mass spectrometry and infrared spectroscopy. Complexes 2 and 3 show a linear coordination geometry for Au(I), with relatively short Au-P bond distances. Complex 3 has a Au•••Au intramolecular distance of 3.326 A° , while complex 2 had a short Au•••Au intermolecular interaction of 3.048 A° . Complexes 4-6 were found by P31 NMR spectroscopy studies to contain a mixture of species in solution, one of which crystallised as [Au3(tripod|)2Cl2]Cl which was shown by X-ray diffraction to contain both tetrahedral and linear Au(I), the first example of a Au(I) complex containing such a mixture of geometries. The reaction of [Au3(tripod)Cl3] (1) with tripod led successfully to the formation of [Au3(tripod)Cl3][Au3(tripod|)2Cl2]+ and [Au3(tripod|)3Cl]2+ . The silver(I) complexes, 7 and 8 appear to contain linear and tetrahedral Ag(I), respectively.

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.

Tris(dimethylphenylphosphine)ruthenium(0) Complexes of n4-Coordinated Polycyclic Aromatic Hydrocarbons

2000 ◽  
Vol 53 (6) ◽  
pp. 507 ◽  
Author(s):  
Martin A. Bennett ◽  
Mark Bown ◽  
David C. R. Hockless
Keyword(s):  
Coordination Geometry ◽  
Crystal Data ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Tertiary Phosphine ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Polycyclic Aromatic ◽  
R Value ◽  
Axial Site

From the reaction of [Ru2Cl3(PMe2Ph)6] Cl with the appropriate radical anions, yellow complexes of general formula [Ru(PMe2Ph)3(η4-arene)] [arene = naphthalene (C10H8) (1), anthracene (C14H10) (2), and triphenylene (C18H12) (3)] have been isolated in poor yield and characterized by elemental analysis, n.m.r. (1H, 13C, 31P) spectroscopy and single-crystal X-ray diffraction. Crystal data: (1), monoclinic, C2/c, a 31.096(8), b 12.012(4), c 17.078(8) Å, β 104.41(3)˚, V 6178(4) Å3, ? 8, refined to final R value of 0.032 with use of 3641 reflections [I > 3σ(I)]; (2), monoclinic, C2/c, a 55.909(4), b 14.348(5), c 17.573(5) Å, β 105.41(1)˚, V 13590(6) Å3, Z 16 (two molecules per asymmetric unit), refined to final R value of 0.049 with use of 7770 reflections [I > 3σ(I)]; (3), mono-clinic, Pn, a 9.377(3), b 12.229(3), c 15.975(3) Å, β 103.51(2)˚, V 1781.2 (7) Å3, Z 2, refined to final R value of 0.026 with use of 2830 reflections [I > 3σ(I)]. In each case, coordination of the zerovalent metal fragment Ru(PMe2Ph)3 to the diene section of one of the terminal rings causes the aromatic molecule to be folded by c. 40˚ at the outer carbon atoms of the diene. The coordination geometry about ruthenium is approximately square pyramidal, with the diene and two tertiary phosphines in the equatorial plane and the remaining tertiary phosphine in the axial site.

Silver(I)-Saccharinato Complexes with 2-(Aminomethyl)pyridine and 2-(2-Aminoethyl)pyridine Ligands: [Ag(sac)(ampy)] and [Ag2(sac)2(μ-aepy)2]

2005 ◽  
Vol 60 (9) ◽  
pp. 978-983 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
William T. A. Harrison
Keyword(s):  
Thermal Analysis ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pyridine Ligands

Two new saccharinato-silver(I) (sac) complexes, [Ag(sac)(ampy)] (1), and [Ag2(sac)2(μ-aepy)2] (2), [ampy = 2-(aminomethyl)pyridine, aepy = 2-(2-aminoethyl)pyridine], have been prepared and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group P21/c and triclinic space group P1̄, respectively. The silver(I) ions in both complexes 1 and 2 exhibit a distorted T-shaped AgN3 coordination geometry. 1 consists of individual molecules connected into chains by N-H···O hydrogen bonds. There are two crystallographically distinct dimers in the unit cell of 2 and in each dimer, the aepy ligands act as a bridge between two silver(I) centers, resulting in short argentophilic contacts [Ag1···Ag1 = 3.0199(4) Å and Ag2···Ag2 = 2.9894(4) Å ]. Symmetry equivalent dimers of 2 are connected by N-H···O hydrogen bonds into chains, which are further linked by aromatic π(py)···π(py) stacking interactions into sheets.

Carbacylamidophosphates: Synthethis and Structure of N,N'-Tetramethyl-NM-benzoylphosphoryltriamide and Dimorpholido-N-benzoylphosphorylamide

2000 ◽  
Vol 55 (6) ◽  
pp. 495-498 ◽  
Author(s):  
Katerina E. Gubina ◽  
Vladimir A. Ovchynnikov ◽  
Vladimir M. Amirkhanov ◽  
Viktor V. Skopenkoa ◽  
Oleg V. Shishkinb
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Sodium Salts ◽  
Space Group ◽  
X Ray ◽  
Centrosymmetric Dimers ◽  
Oxygen Atoms

N,N′-Tetramethyl-N"-benzoylphosphoryltriamide (I) and dimorpholido-N-benzoylphosphorylamide (II), and their sodium salts Nal, Nall were synthesized and characterized by means of IR and 1H, 31P NMR spectroscopy. The structures of I, II were determined by X-ray diffraction: I monoclinic, space group P2i/c with a = 10.162(3), b= 11.469(4), c = 12.286(4) Å , β = 94.04°, V = 1428.4(8) A 3, Z = 4, p(calcd) = 1.187 g/cm3; II monoclinic, space group C2/c with a = 15.503(4), b = 10.991(3), c = 22.000(6) Å, β = 106.39°, V = 3596.3(17) Å3, Z = 8, p(calcd.) = 1.253 g/cm3. The refinement of the structures converged at R = 0.0425 for I, and R = 0.068 for II. In both structures the molecules are connected into centrosymmetric dimers via hydrogen bonds formed by the phosphorylic oxygen atoms and hydrogen atoms of amide groups.

Synthese und Kristallstruktur von l,13-Bis(8-chinolyl)- 1,4,7,10,13-pentaoxatridecan-diquecksilber(I)-diperchlorat

1991 ◽  
Vol 46 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Klaus Brodersen ◽  
Jörg Zimmerhackl
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
R Value ◽  
Torsional Angles ◽  
L 13 ◽  
Oxygen Atoms

1,13-Bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane-dimercury(I)-diperchlorate is formed by the reaction of 1,13-bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane in ethanol with an aqueous solution of dimercury(I)-diperchlorate.It crystallizes in the triclinic space group P Ī with a = 1020.6(2), b = 1200.6(8), c = 1441.1(6) pm , α = 69.60(5)°, β = 83.04(13)°, y = 66.53(4)° and Z = 2. The crystal structure was determined by X -ray diffraction and refined to an R-value o f 0.079. The Hg22+ -ion is coordinated to both nitrogen atoms and four oxygen atoms of one molecule of the ligand. By changing four C - O torsional angles from trans to gauche, the ligand adopts a helical, chiral configuration around the Hg22+-ion. The CIO4--ions are not coordinated to the Hg22+-ion.

Structure and magnetism in a hydroxy bridged binuclear copper(II) system with a "tunable" binuclear centre

1983 ◽  
Vol 61 (3) ◽  
pp. 579-583 ◽  
Author(s):  
Laurence K. Thompson
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Coordination Geometry ◽  
Antiferromagnetic Exchange ◽  
X Ray Diffraction ◽  
Binuclear Copper ◽  
Space Group ◽  
X Ray ◽  
Oxygen Bridge ◽  
Copper Coordination

The molecular structure of [Cu2(PAP)(OH)(IO3)3]•4H2O (PAP = 1,4-di(2′-pyridyl)aminophthalazine) has been determined by single crystal X-ray diffraction. [Cu2(PAP)(OH)(IO3)3]•4H2O belongs to the space group P21/c with a = 7.266(1), b = 15.269(1), c = 25.870(1) Å, β = 96.40(I)°, V = 2852.2 Å3, Z = 4. The copper coordination geometry lies between a square pyramid and a trigonal bipyramid and the two copper(II) centres are bridged by three groups: N2 (phthalazine), hydroxide, and bidentate iodate, in a structure which is analogous to that reported for [Cu2(PAP)(OH)Cl3]•1.5H2O. Replacing the chlorine bridge by iodate has the effect of forcing the two metal centres further apart, thus creating a larger Cu—O—Cu bridge angle. This increase in oxygen bridge angle (101° to 114°) is also reflected in the enhanced antiferromagnetic exchange (−2J(Cl) = 201 cm−1, −2J(IO3) = 335 cm−1). Other groups of varying size (e.g. Br, NO3, SO4) can act as bridges between the two copper centres in systems of this sort with the resultant variation in copper–copper separation and oxygen bridge angle.

1,3,5-Triphosphorinane. Synthese und Struktur der Isomeren des 1,3,5-Triphenyl-1,3,5-triphosphorinans/ 1,3,5-Triphosphorinanes. Synthesis and Structure of the Isomers of 1,3,5-Triphenyl-1,3,5-triphosphorinane

2006 ◽  
Vol 61 (5) ◽  
pp. 577-582 ◽  
Author(s):  
Manfred Fild ◽  
Peter G. Jones ◽  
Michael Lorms ◽  
Stefan Jäger
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Column Chromatography ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The reaction of lithiated Ph(H)PCH2P(H)Ph with (ClCH2)2PPh yields 1,3,5-Triphenyl-1,3,5- triphosphorinane (1) as a mixture of two isomers. The isomers have been separated by column chromatography and characterized by NMR spectroscopy and single crystal X-ray diffraction as the eq-eq-eq (1a) and eq-eq-ax-isomers (1b). (1a) crystallizes with a = 1326.9(3) pm and c = 933.4(3) pm in the rhombohedral space group R3 and displays 3-fold symmetry, showing an eq-eq-eq conformation. (1b) crystallizes in the monoclinic space group P21/c with a = 984.09(12) pm, b = 1757.5(2) pm, c = 1083.13(12) pm, β = 93.329(2)° and displays an ax-eq-eq conformation.

Synthesis and Characterization of Tetrakis(pentafluoroethyl)germane

Synthesis ◽  
2017 ◽  
Vol 49 (11) ◽  
pp. 2389-2393 ◽  
Author(s):  
Stefanie Pelzer ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Nikolai Ignat’ev ◽  
Reint Eujen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Diffraction Analysis ◽  
Spectroscopic Characterization ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Comprehensive Characterization

This paper describes the synthesis and comprehensive characterization of tetrakis(pentafluoroethyl)germane. In addition to a complete NMR spectroscopic characterization, including the rarely used 73Ge NMR spectroscopy, Ge(C2F5)4 was studied by IR spectroscopy, mass spectrometry as well as X-ray diffraction analysis. A 73Ge NMR investigation as well as an X-ray diffraction study of the related germane Ge(CF3)4 are also included.

In situ structure solution of helical sulphur at 3GPa and 400ºC

2001 ◽  
Vol 216 (8) ◽  
Author(s):  
W. A. Crichton ◽  
G. B. M. Vaughan ◽  
M. Mezouar
Keyword(s):  
Global Optimization ◽  
Simulated Annealing ◽  
Rietveld Refinement ◽  
Diffraction Data ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Structure Solution

AbstractThe structure of a 2-chain helical form of sulphur with 9 atoms per unit-cell has been determined from powder synchrotron x-ray diffraction data obtained at 3 GPa and 400ºC, using a combination of global optimization, simulated annealing and Rietveld refinement techniques. Final refinement of the structure in trigonal space group

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