Dihydride formation versus H2-elimination in the protonation of the heterobimetallic FePt complex (CO)3Fe(μ-H)(μ-PCy2)Pt(PEt3)2

1990 ◽  
Vol 68 (6) ◽  
pp. 869-874 ◽  
Author(s):  
Hilary A. Jenkins ◽  
Stephen J. Loeb ◽  
David G. Dick ◽  
Douglas W. Stephan
Keyword(s):  
Crystal Structure ◽  
Infrared Spectroscopy ◽  
Structure Determination ◽  
Reductive Elimination ◽  
Space Group ◽  
X Ray ◽  
Hydride Complex ◽  
H Nmr ◽  
H2 Elimination ◽  
Hydride Ligands

The reaction of Li[Fe(CO)4(PCy2)] with trans-PtCl(H)(PEt3)2 results in the formation of the hydride complex (CO)3Fe((μ-H)((μ-PCy2)Pt(PEt3)2, 1. This heterobimetallic, phosphido-bridged complex reacts with one equivalent of HBF4•Et2O to give the complex [(CO)3Fe(μ-H)2((μ-PCy2)Pt(PEt3)2][BF4], 2, which contains two bridging hydride ligands. This species is isolated and fully characterized by 31P{1H} and 1H NMR and infrared spectroscopy. In contrast, 1 reacts with one equivalent of HCl•DMA (DMA = dimethylacetamide) to give the complex (CO)3ClFe(μ-PCy2)Pt(PEt3)2, 3. This species is the result of oxidative addition of HCl with subsequent reductive elimination of H2(g). This complex is fully characterized by 31P{1H} and 1H NMR, infrared spectroscopy and an X-ray crystal structure determination. 3 crystallizes in the space group [Formula: see text] with a = 10.037(4) Å, b = 10.644(3) Å, c = 17.137(9) Å, α = 102.80(3)°, β = 76.74(3)°, γ = 103.99(3)°, V = 1702(1) Å3, and Z = 2. The structure was refined to R = 2.54% and Rw = 2.73% for 4056 reflections with Fo2 > 3σ(Fo2). Keywords: heterobimetallic, hydride, phosphide, protonation.

scholarly journals Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2 / Molecular and Crystal Structure of l,r-Dimethylsilylene Titanocene Dichloride, (CH3)2Si(C5H4)2TiCl2

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structure Determination ◽  
Titanocene Dichloride ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Structural Dimensions

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2

Crystal structure of 3-chlorobenzo[b]thiophene-2-carbonyl chloride

2009 ◽  
Vol 2009 (7) ◽  
pp. 437-439 ◽  
Author(s):  
Sara Tarighi ◽  
Alireza Abbasi ◽  
Sara Zamanian ◽  
Alireza Badiei ◽  
Mahmood Ghoranneviss
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Cinnamic Acid ◽  
Thionyl Chloride ◽  
Structure Determination ◽  
X Ray ◽  
Packing Structure ◽  
H Nmr ◽  
Carbonyl Chloride ◽  
C Nmr

3-Chlorobenzo[b]thiophene-2-carbonyl chloride was synthesised from cinnamic acid and thionyl chloride. The single crystal X-ray structure determination confirmed the earlier proposed structure and the product was further characterised by 1H NMR, 13C NMR and mass spectrometry. The X-ray structure determination revealed two sets of symmetry related molecules along the b-axis that are loosely connected by relatively weak CH…π ( 3.626, 3.628 Å) interactions, giving rise to two infinite chains. The packing structure is dominated by Van der Waals forces between these chains. No significant π–π interactions are found in the crystal structure.

scholarly journals Über die Reaktion von Wolframhexachlorid mit Se4N2; Kristallstruktur von PPh4[WCl5(NSeCl)] / On the Reaction of Tungsten Hexachloride with Se4N2; Crystal Structure of PPh4[WCl5(NSeCl)]

1991 ◽  
Vol 46 (12) ◽  
pp. 1625-1628 ◽  
Author(s):  
Stefan Vogler ◽  
Werner Massa ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Structure Determination ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Tetraphenylphosphonium Chloride ◽  
Tungsten Hexachloride

The reaction of tungsten hexachloride with Se4N2 leads to [WCl4(NSeCl)]2, which reacts with pyridine to form [WCl4(NSeCl)Py], and with tetraphenylphosphonium chloride to form PPh4[WCl5(NSeCl)], which was characterized by an X-ray structure determination. Space group P21, Z = 2, 1657 observed unique reflections, R = 0.074, wR = 0.061. Lattice dimensions at —80 C: a = 710.7(1), b = 2217.9(4), c = 953.6(2) pm; β = 111.93(3) . The [WCl5(NSeCl)]- ion possesses an almost linear WNSe group with bond lengths WN = 188 pm, corresponding to a double bond, and NSe = 200 pm.

Kristallzucht und Strukturaufklärung von K2[Pt(CN)4Cl2], K2[Pt(CN)4Br2], K2[Pt(CN)4I2] und K2[Pt(CN)4Cl2] · 2H2O/ Crystal Growth and Crystal Structure Determination of K2[Pt(CN)4Cl2], K2[Pt(CN)4Br2], K2[Pt(CN)4I2] and K2[Pt(CN)4]Cl2] · 2H2O

2004 ◽  
Vol 59 (5) ◽  
pp. 567-572 ◽  
Author(s):  
Claus Mühle ◽  
Andrey Karpov ◽  
Jürgen Nuss ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Infrared Spectroscopy ◽  
Crystal Growth ◽  
Single Crystal ◽  
Structure Determination ◽  
Spectroscopy Data ◽  
Crystal Data ◽  
X Ray ◽  
Raman And Infrared Spectroscopy

Abstract Crystals of K2Pt(CN)4Br2, K2Pt(CN)4I2 and K2Pt(CN)4Cl2 ·2H2O were grown, and their crystal structures have been determined from single crystal data. The structure of K2Pt(CN)4Cl2 has been determined and refined from X-ray powder data. All compounds crystallize monoclinicly (P21/c; Z = 2), and K2Pt(CN)4X2 with X = Cl, Br, I are isostructural. K2Pt(CN)4Cl2: a = 708.48(2); b = 903.28(3); c = 853.13(3) pm; β = 106.370(2)°; Rp = 0.064 (N(hkl) = 423). K2Pt(CN)4Br2: a = 716.0(1); b = 899.1(1); c = 867.9(1) pm; β = 106.85(1)°; R(F)N′ = 0.026 (N’(hkl) = 3757). K2Pt(CN)4I2: a = 724.8(1); b = 914.5(1); c = 892.1(1) pm; β = 107.56(1)°; R(F)N′ = 0.025 (N’(hkl) = 2197). K2Pt(CN)4Cl2 ·2H2O: a = 763.76(4); b = 1143.05(6); c = 789.06(4) pm; β = 105.18(1)°; R(F)N′ = 0.021 (N’(hkl) = 2281). Raman and infrared spectroscopy data are reported.

Notizen: Eine neue bicyclische Zinn-Selen-Verbindung. Synthese und Kristallstruktur von [{Cp(CO)2Fe}3ClSn3Se4] / A New Bicyclic Tin Selenium Compound. Synthesis and Crystal Structure of [{Cp(CO)2Fe}3ClSn3Se4]

1993 ◽  
Vol 48 (7) ◽  
pp. 1009-1012 ◽  
Author(s):  
Kurt Merzweiler ◽  
Harald Kraus
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Selenium Compound ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Compound Synthesis

[{Cp(CO)2Fe}SnCl3] reacts with Na2Se in THF to form the compound [{Cp(CO)2Fe}3ClSn3Se4] 1. 1 crystallizes in the monoclinic space group P21/n with 4 formula units per unit cell. The lattice constants are α = 1435.2(7), b = 1124.4(4), c = 1972.7(12) pm, β = 94.59(4)°. According to the X-ray structure determination 1 contains a bicyclic Sn3Se4 framework.

Kristallstruktur von Cs2[B6H5(SCN)]/ Crystal Structure of Cs2[B6H5(SCN)]

1998 ◽  
Vol 53 (8) ◽  
pp. 816-818 ◽  
Author(s):  
W. Preetz ◽  
S. Zander ◽  
C. Bruhn
Keyword(s):  
Crystal Structure ◽  
Ion Exchange ◽  
Structure Determination ◽  
Deae Cellulose ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

Abstract By reaction of [B6H6]2-with (SCN)2 in dichloromethane at -80 C° the thiocyanatohexaborate anion is formed and can be isolated by ion exchange chromatography on diethylaminoethyl (DEAE) cellulose. The X-ray structure determination of Cs2[B6H5(SCN)] (orthorhombic, space group Pbca with a = 9.506(5), b = 10.644(5), c = 21.857(5) Å, Z = 8) reveals that the SCN substituent is bonded via the S atom with the B-S distance of 1.885(9) Å and the B-S-C angle of 99.8(5)°. The SCN group is nearly linear (179.9(9)°).

Synthese und Kristallstruktur von N,N′-Bis(trimethylsilyl)benzamidinato-dichlorogold, Ph— C(NSiMe3)2AuCl2 / Synthesis and Crystal Structure of N,N′-Bis(trimethylsilyl)benzamidinato-dichlorogold, Ph — C(NSiMe3)2AuCl2

1989 ◽  
Vol 44 (9) ◽  
pp. 999-1002 ◽  
Author(s):  
Wolfgang Hiller ◽  
Joachim Strähle ◽  
Alfred Zinn ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Gold Atom ◽  
Chlorine Atoms ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Square Planar

Ph—C(NSiMe3)2AuCl2 has been prepared by the reaction of N,N,N′-tris(trimethylsilyl)-benzamidine with AuCl3 in CH2Cl2 suspension, forming orange-red crystals, which were characterized by an X-ray structure determination.Space group P21/n, Z = 4, 2358 observed independent reflexions, R = 0.028. Lattice dimensions (20°C): a = 695.9(3); b = 1576.1(3); c = 1830.9(3) pm; β = 94.27(3)°. The compound forms monomeric molecules, in which the gold atom is in a square planar arrangement of the two nitrogen atoms of the benzamidinato chelate (Au—N 201.6(7); 203.3(6) pm) and by two chlorine atoms (Au—Cl 227.9(3); 228.5(2) pm).

Die Kristallstruktur von [Na(12-Krone-4)2+]2Se82- · (Se6, Se7) / The Crystal Structure of [Na(12-Crown-4)2+]2Se82- · (Se6, Se7)

1991 ◽  
Vol 46 (10) ◽  
pp. 1287-1292 ◽  
Author(s):  
Rüdiger Staffel ◽  
Ulrich Müller ◽  
Andreas Ahle ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Title Compound ◽  
Crystal Structure Determination ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Disordered Structure

The title compound was prepared from sodium polyselenide and 12-crown-4 in DMF solution in the presence of cerium(III)chloride in the form of black needles. The crystal structure determination by X-ray diffraction shows a partially disordered structure, in which the anionic units Se82- · Se7 and Se82- · Se6 are present in the ratio 0.72/0.28. These units are associated to layers parallel to (100); the layers alternate with pseudohexagonal layers of [Na(12-crown-4)2]+ ions. Space group P1̅, Z = 2, 3903 observed unique reflections, R = 0.114, wR= 0.084. Lattice dimensions at -65°C: a = 1247.9(3), b = 1367.8(8), c = 1660(1) pm, α = 94.65(5), β = 98.94(3), γ = 91.10(3)°.

Synthese und Kristallstruktur von [Rb(18-Krone-6)]2[Zn(Se4)(Se6)] / Synthesis and Crystal Structure of [Rb(18-Crown-6)]2[Zn(Se4)(Se6)]

1991 ◽  
Vol 46 (8) ◽  
pp. 1011-1014 ◽  
Author(s):  
Dieter Fenske ◽  
Sylvia Magull ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Zinc Acetate ◽  
Zinc Atom ◽  
Ionic Structure ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

[Rb(18-crown-6)]2[Zn(Se4)(Se6)] has been prepared by the reaction of a lithium polyselenide solution in DMF with zinc acetate in the presence of rubidium iodide and 18-crown-6. It forms dark red crystals, which were characterized by FIR spectroscopy as well as by an X-ray structure determination. Space group C2/c, Z = 4, 3012 observed unique reflections, R = 0.073. Lattice dimensions at —50 °C: a = 1963.1(14), b = 1125.9(9), c = 2060.3(16) pm, β = 90.05(3)°. The compound has a complex ionic structure, in which the zinc atom of the anion [Zn(Se4)(Se6)]2- is coordinated tetrahedrally by four selenium atoms of a Se42- and a Se62- unit in five and seven membered rings, respectively. The complex cations [Rb(18-crown-6)]+ have Rb · · · Se contacts of 360.7 and 372.0 pm with selenium atoms of the ZnSe4-ring.

Substitutionsreaktionen an der N-Chlornitrenogruppe des [WCl4(NCl)]2. Die Kristallstrukturen von [CH3CN—WCl4(NSMe)] und [WNCl3 · NC—CH3]4 / Substitution Reactions at the N-Chloronitreno Group of [WCl4(NCl)]2. The Crystal Structures of [CH3CN—WCl4(NSMe)] and [WNCl3 · NC—CH3]4

1989 ◽  
Vol 44 (8) ◽  
pp. 903-910 ◽  
Author(s):  
Astrid Görge ◽  
Ute Patt-Siebel ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Trans Position ◽  
Crystal Data ◽  
Substitution Reactions ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations

[WCl4(NCl)]2 reacts in acetonitrile with the trimethylsilyl compounds Me3SiSR (R = Me, Ph), and Me3SiESiMe3 (E = S, Se), with substitution of the chlorine atom of the N-chloronitreno group W=N–Cl and formation of CH3CN–WCl4(NSR) and CH3CN–WCl4(NEN)WCl4–NCCH3, respectively. Excess Me3SiBr reacts with CH3CN–WCl4(NSMe) to afford CH3CN–WBr4(NSMe). [CH3CN–WNCl3]4 was obtained from CH3CN–WCl4(NCl) and N(SiMe3)3. The products were characterized by their IR spectra. Two X-ray crystal structure determinations were also carried out. CH3CN—WCl4(NSMe) forms twinned crystals, and only non-overlapping reflexions of one of the twin individuals were used for the structure determination (846 unique values, R = 0.055). Crystal data: a = 592.4(2), b = 758.8(2), c = 1203.7(8) pm, β = 95.06(4)°, monoclinic, space group P21/m, Z = 2. The compound is a monomer in which the acetonitrile ligand is situated in the trans position to the W≡N–S̱̅–Me group. The bond lengths (W≡N 174(2), N–S 161(2) pm) and bond angles (WNS 176(1), NSC 102.1(9)°) are in agreement with the proposed formula. Crystal data for [CH3CN–WNCl3]4: a = 1009.5(2), b = 1274.5(2), c = 1287.9(2) pm, β = 108.17(1)°, monoclinic, space group P21/c, Z = 2 (2113 unique reflexions, R = 0.057). The compound forms tetrameric units, in which the W atoms form a square and are linked with one another via N atoms at alternating distances (W=N 171(2), W–N 207(2), W–NCMe 238(2) pm).

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