Synthesis and Structural Studies of Tetrahedral [M(Ph2P(CH=CH)PPh2)2]BPh4 and [M(Ph2P(CH2)nPPh2)2]BPh4 (n = 2, 3) Complexes for M = Copper(I), Silver(I), and Gold(I)

2012 ◽  
Vol 65 (7) ◽  
pp. 811 ◽  
Author(s):  
Peter C. Healy ◽  
Bradley T. Loughrey ◽  
Michael L. Williams
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
Single Crystal ◽  
Copper Complex ◽  
Electrospray Mass Spectrometry ◽  
Structural Studies ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

Tetraphenylborate salts of the 1 : 2 tetrahedral bis(bidentate) complexes of copper(i), silver(i), and gold(i) with cis-bis(diphenylphosphino)ethene (dppey), [M(Ph2PCH=CHPPh2)2]BPh4, cis-bis(diphenylphosphino)ethane (dppe), and cis-bis(diphenylphosphino)propane (dppp), [M(Ph2P–R–PPh2)2]BPh4 (R = (CH2)2, (CH2)3), have been prepared and characterized by NMR spectroscopy, electrospray mass spectrometry, and single crystal X-ray structural analysis at 200 K. Structures of the dppey complexes as acetone solvates show the Cu and Ag complexes to be isostructural with the previously reported Au complex, crystallizing in space group P 21/n with a ~ 25.5, b ~ 15.6, and c ~ 34.2 Å, and β ~ 103°. Structures of the dppe complexes show the copper complex to crystallize in the chiral space group P21 with a 11.8954(5), b 20.1904(5), and c 14.8999(5) Å, and β 111.366(5)°. The Ag and Au complexes are isostructural, crystallizing in space group P21/c with a ~ 17.8, b ~ 17.6, and c ~ 20.9 Å, and β ~ 107°. Structures of the dppp complexes show the copper complex to crystallize in space group P21/c with a 17.8399(4), b 19.8803(4), and c 18.7165(3) Å, and β 102.197(2)°. The Ag and Au complexes are isostructural, crystallizing in space group P21/n with a ~ 17.7, b ~ 18.6, and c ~ 19.6 Å, and β ~ 100°. Across the three series of complexes, the M–P bond lengths increase in the order Cu < Au < Ag with Cu–P = 2.281(3)–2.314(1) Å, average 2.30(1) Å; Au–P = 2.363(1)–2.4322(8) Å, average 2.40(2) Å, and Ag–P = 2.445(1)–2.5303(5) Å average 2.49(2) Å.

scholarly journals Synthesis And Single Crystal X-Ray Structure Of 2-(1,3,4-Oxadiazol- 2-yl)Aniline

2007 ◽  
Vol 62 (6) ◽  
pp. 835-840 ◽  
Author(s):  
Ali Souldozi ◽  
Katarzyna Ślepokura ◽  
Tadeusz Lis ◽  
Ali Ramazani
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
Single Crystal ◽  
Structure Determination ◽  
High Yield ◽  
Aminobenzoic Acid ◽  
Aromatic Rings ◽  
X Ray ◽  
C Nmr

Reaction of 2-aminobenzoic acid with (N-isocyanimino)triphenylphosphorane proceeds smoothly at r. t. to afford 2-(1,3,4-oxadiazol-2-yl)aniline in high yield. The structure of this compound was confirmed by IR, 1H, and 13C NMR spectroscopy, mass spectrometry, and single crystal X-ray structure determination. The X-ray structural analysis of the product indicated that its aromatic rings are approximately co-planar

Physical and structural studies of N-substituted-3-hydroxy-2-methyl-4(1H)-pyridinones

1988 ◽  
Vol 66 (1) ◽  
pp. 123-131 ◽  
Author(s):  
William O. Nelson ◽  
Timothy B. Karpishin ◽  
Steven J. Rettig ◽  
Chris Orvig
Keyword(s):  
Mass Spectrometry ◽  
Hydrogen Bonding ◽  
Solid State ◽  
Single Crystal ◽  
Direct Methods ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

A series of 3-hydroxy-2-methyl-4(1H)-pyridinones has been prepared with the substituents H, CH3, n-C6H11, and CH2CH2NH2 at the ring N. The dipyridinone 1,6-bis(3-hydroxy-2-methyl-4(1H)-pyridinon-1-yl)hexane has also been synthesized. The products with H and CH3 substituents have been studied by single crystal X-ray diffraction. Crystals of 3-hydroxy-2-methyl-4-pyridinone are monoclinic, a = 6.8351(4), b = 10.2249(4), c = 8.6525(4) Å, β = 105.215(4)°, Z = 4, space group P21/n and those of 3-hydroxy-1,2-dimethyl-4-pyridinone are orthorhombic, a = 7.3036(4), b = 13.0490(6), c = 13.7681(7) Å, Z = 8, space group Pbca. Both structures were solved by direct methods and were refined by full-matrix least-squares procedures to R = 0.037 and 0.044 for 914 and 857 reflections with I ≥ 3σ(I), respectively. Bond lengths and angles in the two compounds were normal. All the compounds have been studied by mass spectrometry, and by infrared and proton nmr spectroscopies. The importance of hydrogen bonding to both the solution and solid state properties of these compounds has been confirmed by these techniques.

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.

The Crystal and Molecular Structures of Bis(diethyldithiocarbamato)platinum(II) and Bis[di(2-hydroxyethyl)dithiocarbamato]platinum(II)

1992 ◽  
Vol 45 (2) ◽  
pp. 429 ◽  
Author(s):  
AT Baker ◽  
MT Emett
Keyword(s):  
Single Crystal ◽  
Bond Length ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Crystal And Molecular Structures

The structures of [Pt(S2CN(C2H5)2)2] (1) and [Pt(S2CN(C2H4OH)2)2] (2) have been determined by single-crystal X-ray diffractometry. Compound (1) crystallizes in the tetragonal space group P42/n, a 16.4692(10),c 6.2160(6) � (Z = 4); R was 0.029 for 1012 observed reflections. Compound (2) is monoclinic, space group Pc, a 6-0663(11), b 1.1784(15), c 12.5740(21) � ,β92.569(8)� (Z = 2); R was 0.019 for 1573 observed reflections. The presence of electron-withdrawing groups in the ligands of (2) appears to have little effect on the Pt-S distances but causes an increase in the C-N bond length, with the C-N bond lengths being significantly different at the 2 σ level.

Tetrahalogenotellurate(II): Synthese und Kristallstrukturen von Verbindungen mit den Ionen TeX42- (X = Cl, Br, I)/Tetrahalotellurates(II): Syntheses and Crystal Structures of Compounds with TeX42- Ions (X = Cl, Br, I)

1985 ◽  
Vol 40 (2) ◽  
pp. 251-257 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Bernt Krebs
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Square Planar

Abstract The compounds [(C6H5)4As]2 TeCl4 (1), [(C2H5)4 N]2 TeBr4 · CH3CN (2), and [(C2H5)4N]2TeI4 (3) were prepared by the reaction of Te, X2 , and excess (C2H5)4NX (X = Br, I) in acetonitrile solution or by heating of [(C6H5)4 As]2TeCl6 , Te, and (C6H5)4 ASCl for several hours in the same solvent.The structures of 1-3 were determined from single crystal X-ray data.1 crystallizes in the monoclinic space group P21/n with a = 1061.8(2), b = 1614.2(3), c = 1341.7(3) pm, β = 94.21° and Z = 2; 2: tetragonal, P4/mmm, a = 1039.7(2), c = 690.5(1), Z = 1; 3: tetragonal, I4/mmm, a = 1061.7(2), c = 1342.8(4), Z = 2. In 1-3 Te(II) exhibits a square planar coordination. The Te -CI, Te -Br, and Te-I bond lengths were found to be 260.7 (mean), 275.3, and 298.5 pm, respectively.

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.

Metallaborane Reaction Chemistry. Part 3. Reaction of Carbon Monoxide with [6-H-6-(PPh3)-6P,5C-μ-(2-Ph2PC6H4)-nido-6-IrB9H12] and the Isolation and Characterisation of Two arachno-6-Monoiridadecaboranes [6-(CO)-6-H-6,9-(PPh3)2-6P,5C-μ-(2-Ph2PC6H4)-arachno-6-IrB9H11] and sym-[6-(CO)-6-H-6,6-(PMe2Ph)2-9-(PPh3)-arachno-6-IrB9H11]

1997 ◽  
Vol 62 (8) ◽  
pp. 1239-1253 ◽  
Author(s):  
Jonathan Bould ◽  
Paul Brint ◽  
John D. Kennedy ◽  
Mark Thornton-Pett ◽  
Lawrence Barton ◽  
...  
Keyword(s):  
Carbon Monoxide ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Reaction System ◽  
Structural Type ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

[6-(CO)-6-H-6,9-(PPh3)2-6P,5C-μ-(2-Ph2PC6H4)-arachno-6-IrB9H11] (1) results from the reaction of [6-H-6-(PPh3)-6P,5C-μ-(2-Ph2PC6H4)-nido-6-IrB9H12] (2) with carbon monoxide in refluxing benzene. It is characterised by NMR spectroscopy and by single-crystal X-ray diffraction analysis. Crystals were triclinic, space group P1, with a = 10.688(2), b = 13.114(3), c = 22.356(5) Å, α = 78.33(2), β = 89.482(10), γ = 70.884(12)°, and Z = 2. The compound is of the little-examined arachno ten-vertex metallaborane structural type. A second compound of this type, [6-(CO)-6-H-6,6-(PMe2Ph)2-9-(PPh3)-arachno-6-IrB9H11] (3), isolated from a reaction system involving [Ir(CO)Cl(PPh3)2], PMe2Ph and the [nido-B9H12]- anion, has also been characterised crystallographically. Crystals were triclinic, space group P1, with a = 10.389(1), b = 10.511(1), c = 19.699(3) Å, α = 75.03(1), β = 85.53(1), γ = 74.88(1)°, and Z = 2.

Darstellung und Struktur von Ba2AsSe4(OH) · 2H2O / Preparation and Structure of Ba2AsSe4(OH) · 2H2O

1986 ◽  
Vol 41 (4) ◽  
pp. 436-438 ◽  
Author(s):  
Jürgen Kaub
Keyword(s):  
Aqueous Solution ◽  
Structural Analysis ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

Ba2AsSe4(OH)·2H2O 1 has been prepared by the reaction of Ba(OH)2 with As2Se3 in aqueous solution and its structure established by X-ray structural analysis. 1 crystallizes in the m onoclinic system , space group Cm (No. 8 ) with a = 8.992(4), b = 9.967(3). c = 6.340(1) A . ß - 104.51(4). Z = 2. M = 718.5, Dber = 4.34 g-cm-3. In the structure there are isolated AsSe43- tetrahedra with Cs-symmetry and As-Se bond lengths between 2.303 and 2.329 Å. The Ba2+ ions are coordinated by 6 Se and 3 O atoms

Filling up another Gap: Synthesis and Crystal Structure of Ba2H3I

2011 ◽  
Vol 66 (11) ◽  
pp. 1087-1091 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Title Compound ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

Colorless and transparent single crystals of Ba2H3I were obtained by reacting Ba with dried and sublimed NH4I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules at 1100 K for 13 h. The crystal structure of the title compound was determined and refined by means of single-crystal X-ray diffraction. Ba2H3I crystallizes in a stuffed anti-CdI2 structure isotypic to Sr2H3I in the space group P3̄m1 (no. 164) with the lattice parameters a = 451.86(12) and c = 811.84(23) pm. The structural results for Ba2H3I are consistent with bond lengths and coordination geometries of related binary and ternary hydrides

Cis-2-telluro-1.3.2λ5.4λ3-diazadiphosphetidin - Kristallstruktur eines in Lösung fluktuierenden Redoxsystems / Cis-2-telhirium-1.3.2λ5.4λ3-diazadiphosphetidine - Crystal Structure of a Redox System Fluctuating in Solution

1978 ◽  
Vol 33 (6) ◽  
pp. 610-613 ◽  
Author(s):  
Siegfried Pohl
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Bond Length ◽  
Title Compound ◽  
Redox System ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Nitrogen Ring

Abstract The crystal structure of the title compound was determined from single crystal X-ray data. The compound crystallises in the orthorhombic space group Pnma. In contrast to the solution where fluctuating P-Te bonds have been established by NMR analyses the crystals contain isolated molecules with fixed P-Te bonds (bond length: 235.4 pm). The four-membered phosphorus nitrogen ring exhibits significant deviations from planarity. The P-N bond lengths were found to be 168.3 and 175.0 pm, respectively

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