scholarly journals Notizen: Synthese und Kristallstruktur von PPh3Me[HSO4]/ Synthesis and Crystal Structure of PPh3Me[HSO4]

1988 ◽  
Vol 43 (8) ◽  
pp. 1069-1071 ◽  
Author(s):  
Fritjof Schmock ◽  
Aida Müller ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Hydrogen Bonds ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Crystal Data ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Silver Sulfate ◽  
By Products

AbstractPPh3Me[HSO4] was prepared by the reaction of (PPh3Me)I with silver sulfate in aqueous solution. OPPh2Me and benzene being the by-products. The title compound was characterized by its IR spectrum as well as by an X-ray structure determination (1730 observed independent reflexions, R = 0.043). Crystal data: a = 910.4(3). b = 1587.8(4), c = 1294.2(6) pm, β = 105.52(3)°. space group P21/c, Z = 4. The structure consists of PPh3Me⊕ cations and of HOSO3⊖ ions that are associated via strong hydrogen bonds to dimeric centrosymmetric units.

Synthese und Kristallstruktur des cyclischen Hydrazido-Komplexes {Fe2Cl4[(NSiMe3)(CPh)]2N2} / Synthesis and Crystal Structure of the Cyclic Hydrazido Complex {Fe2Cl4[(NSiMe3)(CPh)]2N2}

1989 ◽  
Vol 44 (4) ◽  
pp. 495-498 ◽  
Author(s):  
Wolfgang Hiller ◽  
Eva Hartmann ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Title Compound ◽  
Crystal Data ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Data Space ◽  
Moisture Sensitive

The title compound has been prepared by the reaction of FeCl3 with N, N, N′-tris(trimethylsilyl) benzamidine in CH2Cl2 solution as dark red, moisture-sensitive crystals. The complex was characterized by its IR spectrum as well as by an X-ray structure determination.Crystal data: space group P21/n, Z = 2 (1178 observed independent reflexions, R = 0.089). Lattice dimensions (20 °C): a = 1240.2(2), b = 645.7(3), c = 1779.7(3) pm, β = 91.31(2)°. The compound forms centrosymmetric molecules, in which the iron atoms are members of two fused planar heterocycles with the NN group as the com m on edge. The NN bond length (142.5(9) pm) is very close to the NN bond length of hydrazine.

Kristallstruktur des Doppelkomplexsalzes trans-(py2CH2)[Pt(OH)2(ox)2]transs-(py2CH2)[Pt(OH)(ox)2(H2O)]2·4H2O / Crystal Structure of the Double Complex Salt trans-(py2CH2)[Pt(OH)2(ox)2](H2O)]2·4H2O

1998 ◽  
Vol 53 (5-6) ◽  
pp. 569-572 ◽  
Author(s):  
J.-G. Uttecht ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Hydrogen Peroxide ◽  
Hydrogen Bonds ◽  
Structure Determination ◽  
Complex Salt ◽  
Double Complex ◽  
Double Complex Salt ◽  
X Ray ◽  
Complex Anions

Abstract By treatment of [Pt(ox)2]2- with hydrogen peroxide the octahedral trans-[Pt(OH)2(ox)2]2- is formed. From the saturated aqueous solution in the presence of dipyridiniomethane dications single crystals of the double complex salt trans-(py2CH2)[Pt(OH)2(ox)2] trans-(py2CH2)[Pt(OH)(ox)2(H2O)]2 · 4H2O were grown and an X-ray structure determination (tricli­nic, space group P1̄, a = 8.649(1), b = 11.189(3), c = 12.731 (2) Å, α = 79.075(12), β = 80.725(8), γ= 73.932(13)°, Z = 1) has been performed. The centrosymmetric trans-[Pt(OH)2(ox)2]2- is connected via hydrogen bonds between its hydroxide groups and the aqua ligands of two protonated complex anions trans-[Pt(OH)(ox)2(H2O)]- .

scholarly journals Synthese und Kristallstruktur von (PPh4)2Te4 / Synthesis and Crystal Structure of (PPh4)2Te4

1991 ◽  
Vol 46 (8) ◽  
pp. 1015-1019 ◽  
Author(s):  
Hans Wolkers ◽  
Bernhard Schreiner ◽  
Rüdiger Staffel ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Crystal Data ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cscl Type ◽  
Type Lattice ◽  
Close Contacts

(PPh4)2Te4 has been prepared by the reaction of Na2Te3 with PPh4Cl in DMF solution in the presence of MnCl2 or FeCl2. The compound forms dark red crystals, which were characterized by IR spectroscopy as well as by an X-ray crystal structure determination (6109 observed independent reflections, R = 0.030). Crystal data: triclinic, space group PĪ, Z = 2, a = 1046.7(2), b = 1130.1(2), c = 1967.8(4) pm, α = 93.63(3), β = 90.43(3), γ = 108.89(3)° at —60 °C. The cations are grouped in pairs (PPh4+)2 around inversion centres, each pair being surrounded by eight Te42- ions, arranged as in the CsCl type lattice. The chain-like Te42- ions have no close contacts with one another.

Synthesis and Crystal Structure of (dmaaH)2(dmaH)2[P12Sn12N12(NH)2] · 4 dmaa, dmaa = N,N-Dimethylacetamide, dma = Dimethylamine, an Anhydrous Example of the P12N14Cage

2001 ◽  
Vol 56 (10) ◽  
pp. 1020-1024
Author(s):  
Stephan Roth ◽  
Wolfgang Schnick
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystals ◽  
Structure Determination ◽  
Title Compound ◽  
Saturated Solution ◽  
Synthesis And Crystal Structure ◽  
X Ray

Abstract The title compound (dmaaH)2(dmaH)2[P12S12N12(NH)2] · 4 dmaa (1) was obtained by crys­tallization from a saturated solution of anhydrous P12S12N8(NH)6 in N,N-dimethylacetamide (dmaa) as large single crystals. According to the X-ray structure determination (P21/n, a = 1421.8(1), b = 1556.5(2), c = 1645.8(1) pm, ß = 112.207(6)°, Z = 2, 6388 observed reflections, R1 = 0.046, wR2 = 0.111) the anionic cage is built up from twelve P3N3 rings in boat confor­ mation. N,N-dimethylammonium ions (dmaH+) are directly connected to the cage, and pairs of N,N-dimethylacetamidonium ions (dmaaH+) and N,N-dimethylacetamide molecules (dmaa) are interconnected by hydrogen-bonds.

Synthesis and Crystal Structure of the Tetra-nickel Substituted [Ni4(H2O)2(AsW9O34)2]10- Polyoxoanion

2004 ◽  
Vol 59 (9) ◽  
pp. 980-984 ◽  
Author(s):  
Daniel Drewes ◽  
Eva Melanie Limanski ◽  
Bernt Krebs
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Hydrogen Bonds ◽  
Monoclinic Crystal System ◽  
Monoclinic Crystal ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Sodium Cations ◽  
Vis Spectroscopy ◽  
Common Plane

The new polyoxotungstate (NH4)6Na4[Ni4(H2O)2(AsW9O34)2] · 20 H2O (1) was synthesized in aqueous solution and characterized by IR and UV/Vis spectroscopy, energy dispersive X-ray fluorescence and single-crystal X-ray analysis. It contains the tetra-nickel substituted [Ni4(H2O)2(AsW9O34)2]10− polyoxoanion, in which the four Ni atoms are in a common plane and form a regular rhombus. 1 crystallizes in the monoclinic crystal system, space group P21/n with a = 11.849(2), b = 16.718(3), c = 21.243(4) Å , β = 100.48(3)◦, and Z = 2. The anions are linked via hydrogen bonds and sodium cations.

Synthese und Kristallstruktur von MoCl4(DME) · 15-Krone-5 und MoCl4(DME) (DME = 1,2-Dimethoxyethan) / Synthesis and Crystal Structure of MoCl4(DME) · 15-Crown-5 and MoCl4(DME) (DME = 1,2-Dimethoxyethane)

1991 ◽  
Vol 46 (3) ◽  
pp. 307-314 ◽  
Author(s):  
Evamarie Hey-Hawkins ◽  
Hans Georg von Schnering
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Structure Determination ◽  
Unit Cell ◽  
Crystal Data ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
Work Up

NaSi reacts with MoCl5 and 15-crown-5 in toluene with reduction of Mo(V) to Mo(IV). Work-up in DME yields MoCl4(DME)· 15-crown-5 (1). MoCl4(DME) (2) is prepared more conveniently from MoCl5/DME. 1 and 2 were characterized spectroscopically and by X-ray structure determination. Crystal data: 1, space group P212121 (No. 19), Z = 4, 2765 observed independent reflexions, R = 0.026, cell dimensions (110 K): a = 16.292(4), b = 12.884(3), c = 10.452(2) Å. 2, space group I4̄2d (No. 122), Z = 8, 558 observed independent reflexions, R = 0.037, cell dimensions (292 K): a = b = 9.562(2), c = 23.777(6)Å. The MoCl4(DME) molecule of 1 and 2 forms a distorted octahedron. There are four non-coordinating 15-crown-5 molecules present in the unit cell of 1. The UV/VIS spectrum and the magnetic properties of 2 are discussed.

Notizen: [K(18-Krone-6)][WF5(NCl)]; Synthese und Kristallstruktur / [K(18-Crown-6)][WF5(NCl)]; Synthesis and Crystal Structure

1992 ◽  
Vol 47 (7) ◽  
pp. 1054-1056 ◽  
Author(s):  
Harald Stenger ◽  
Kurt Dehnicke ◽  
Wolfgang Hiller
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Bond Angle ◽  
Ion Pairs ◽  
Acetonitrile Solution ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ether Molecule

[K(18-crown-6)][WF5(NCl)] has been prepared as yellow crystals by the reaction of KF with WCl4(NCl) in the presence of 18-crown-6 in acetonitrile solution. The compound was characterized by its IR spectrum and by an X-ray structure determination. Space group P21/n, Z = 4, 3697 observed unique reflections, R = 0.034. Lattice dimensions at –65 °C: a = 1313.8(3), b = 851.2(1), c = 1842.7(4) pm, β = 95.304(1)°. The compound forms ion pairs, in which the pottassium ion is coordinated by the six oxygen atoms of the crown ether molecule and by two fluorine ligands of the [WF5(NCl)]- unit with K–F distances of 272.4(5) and 288.6(5) pm. The W=N–Cl group of the anion is nearly linear (bond angle 170.7(5)°) with bond lengths of WN = 172.4(7) and NCI = 162.7(7) pm.

Synthesis and Crystal Structure of the Complex of (R,R)-N,N’-bis(salicylal)-1,2-Cyclohexanediamine with Fe3+

2012 ◽  
Vol 441 ◽  
pp. 382-386
Author(s):  
Yin Zhi Jiang ◽  
Lian Zhu Tian ◽  
Yang Zou ◽  
Lian Qun Zhang
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Elemental Analysis ◽  
Structure Determination ◽  
Nitrate Anion ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Coordinate Bond

The complex 1 (FeC20H24N3O7) was synthesized from (R, R)-N,N-bis (salicylal )1,2-cyclohexanediamine (H2L) and Fe (NO3)3. The complex 1 has been characterized by the elemental analysis and IR spectra. The crystal structure of the complex 1 was determined by single-crystal X-ray diffraction. Crystal data for the complex 1: space group C2/c , with a = 18.967(2)Å, b = 14.526(2)Å, c = 15.3927(18)Å, α=90.00º, β= 95.885(3) º, γ=90.00º, Z=8, V= 4218.5(9) Å3, Dc= 1.494 mg.m-3, µ= 0.763mm-1, F(000)= 1976. The results of crystal structure determination show that there exists rich H-bond. The complex 1 is composed of one [Fe (L2-) (H2O)2]+cation and one nitrate anion. The L2-and two H2O molecular are attached to the Fe3+viacoordinate bond. The nitrate anion is attached to the cation through hydrogen bond with H (3A) and H (4B) atom. The Fe (III) atom is six-coordinated by linking to one quarter-dentate chelating ligand (L2-) and two mono-dentate chelating H2O ligands.

ScOH(CH3SO3)2, a Basic Methanesulfonate of Scandium with Chain Structure

2004 ◽  
Vol 59 (1) ◽  
pp. 33-36 ◽  
Author(s):  
Mathias S. Wickleder ◽  
Ingrid Müller
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Methanesulfonic Acid ◽  
Chain Structure ◽  
Orthorhombic Space Group ◽  
X Ray

Abstract Single crystals of ScOH(CH3SO3)2 were obtained from a solution of Sc2(CO3)3 in methanesulfonic acid at pH 7. According to the X-ray single crystal structure determination, the compound crystallizes with the non-centrosymmetric orthorhombic space group Pmc21 (Z = 8, a = 743.92(8), b = 1497.7(3), c = 1540.1(2) pm, Rall = 0.0925) and contains the Sc3+ ions in octahedral coordination of oxygen atoms which belong to two OH− and four CH3SO3 − ions. The linkage of the Sc3+ ions leads to chains according to the formulation 1∞[Sc(CH3SO3)4/2(OH)2/2] which are oriented along the [100] direction and connected via hydrogen bonds. The IR spectrum of the compound shows the typical bands of the CH3SO3 − ion.

The protonation of the ethylenediphosphinetetraacetate anion and the crystal structure of the bis (hydrogen bromide) of ethylenediphosphinetetraacetic acid

1981 ◽  
Vol 46 (12) ◽  
pp. 3063-3073 ◽  
Author(s):  
Jana Podlahová ◽  
Bohumil Kratochvíl ◽  
Vratislav Langer ◽  
Josef Šilha ◽  
Jaroslav Podlaha
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Structure Determination ◽  
Free Acid ◽  
Hydrogen Bromide ◽  
Carboxyl Groups ◽  
Spectroscopic Methods ◽  
X Ray ◽  
Partial Formation

The equilibria and mechanism of addition of protons to the ethylenediphosphinetetraacetate anion (L4-) were studied in solution by the UV, IR, 1H and 31P NMR spectroscopic methods. A total of six protons can be bonded to the anion. They are added stepwise, first with partial formation of zwitterions containing P-H bonds, which then dissociate with formation of the free acid, H4L, where all four protons are bonded in carboxyl groups. The formation of zwitterions is strongly dependent on the concentration. In the final stage, the acid bonds two additional protons to form the bis-phosphonium cation, H6L2+. A number of isostructural salts containing this cation, H4L.2 HX (X = Cl, Br, I), have been prepared. The X-ray crystal structure determination of the bromide confirmed the expected arrangement. The bromide crystals are monoclinic, a = 578.2, b = 1 425.0, c = 1 046.7 pm, β = 103.07° with a space group of P21/c, Z = 2. The final R factor was 0.059 based on 1 109 observed reflections. The structure consists of H6L2+ cations containing protons bonded to phosphorus atoms (P-H distance 134 pm) and of bromide anions, located in gaps which are also sufficiently large for I- anions in the isostructural iodide. The interbonding of phosphonium cations proceeds through hydrogen bonds, C-OH...O=C, in which the O...O distance is 275.3 pm.

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