Synthese, Struktur und Reaktivität labiler Rhodium(I)-Komplexe mit iPr2PC2H4NMe2 und iPr2PC2H4OMe als Phosphanliganden / Synthesis, Structure and Reactivity of Labile Rhodium(I) Complexes Containing iPr2PC2H4NMe2 and iPr2PC2H4OMe as Phosphine Ligands

1990 ◽  
Vol 45 (11) ◽  
pp. 1548-1558 ◽  
Author(s):  
Helmut Werner ◽  
Andreas Hampp ◽  
Karl Peters ◽  
Eva Maria Peters ◽  
Leonhard Walz ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Chelate Ring ◽  
Parent Compound ◽  
Phosphine Ligand ◽  
Phosphine Ligands ◽  
X Ray ◽  
Vinylidene Complexes ◽  
Square Planar

Square-planar rhodium(I) complexes [RhCl(iPr2PC2H4Y)2] (8, 9) containing one chelating and one P-bonded monodentate phosphine ligand are prepared from [RhCl(C8H14)2]2 (7) and the new functionalized phosphines iPr2PC2H4Y (5,6). Reaction of 9 (Y = NMe2) with CO and of 8 (Y = OMe) with CO, C2H4, C2H2, C2Ph2 and HC2Ph leads to opening of the chelate ring and formation of the complexes trans-[RhCl(L)(η1-P–iPr2PC2H4Y)2] (10-15). Treatment of 8 with H2 gives the dihydridorhodium(III) compound [RhH2Cl(iPr2PC2H4OMe)2] (16). The vinylidene complexes trans-[RhCl(=C=CHR)(η1-P– iPr2PC2H4OMe)2] (17, 18) are obtained by thermal or pyridine promoted rearrangement of 13 (L = C2H2) and 15 (L = HC2Ph). 13 and 15 have also been used as starting materials for the synthesis of the cyclopentadienyl alkyne and vinylidene complexes 19-21. The X-ray crystal structure of the parent compound 8 was determined.

Zur Reaktion von (COD)PtCl2 mit 1,4-Bis-[di(t-butyl)phosphino]butan (dtbpb). Kristallstruktur von [(t-Bu)2P(CH2)4P(t-Bu)2 – (C8H12) – PtCl]+ Cl- / On the Reaction of (COD)PtCl2 with 1,4-Bis-[di(t-butyl)phosphino]butane (dtbpb). Crystal Structure of [(t-Bu)2P(CH2)4P(t-Bu)2–(C8H12)–PtCl]+Cl-

1993 ◽  
Vol 48 (4) ◽  
pp. 425-430 ◽  
Author(s):  
K. Wurst ◽  
J. Strähle
Keyword(s):  
Crystal Structure ◽  
Phosphine Ligand ◽  
Phosphine Ligands ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Square Planar ◽  
Bidentate Phosphine

Whereas (COD)PtCl2 usually reacts with bidentate phosphine ligands under substitution of the COD ligand, the reaction with the newly synthesized 1,4-bis-[di(t-butylphosphino)] butane results in the insertion of COD into one Pt-P bond affording [(t-Bu)2P(CH2)4 P(t-Bu)2-(C8H12)-PtCl]+Cl- (1). 1 crystallizes in the monoclinic space group C2/c with a = 3912.8(8), b = 1765.6(3), c = 3851.3(4) pm, β = 118.36(2)°, Ζ = 24. In the cation of 1 the second C=C bond remains coordinated to the central Pt2+ ion. The square-planar coordination of Pt2+ ion is completed by a Cl ligand and the second P atom of the phosphine ligand. The inserted C-C bond is elongated to 149(5) pm with respect to the coordinating C=C bond of 133(6) pm.

Cyclopalladation of trimesitylarsine. The X-ray crystal structure for

1988 ◽  
Vol 66 (12) ◽  
pp. 3162-3165 ◽  
Author(s):  
Elmer C. Alyea ◽  
George Ferguson ◽  
John Malito ◽  
Barbara L. Ruhl
Keyword(s):  
Crystal Structure ◽  
Cleavage Product ◽  
Phosphine Ligands ◽  
Monoclinic Space Group ◽  
Dimeric Complex ◽  
Tertiary Phosphine ◽  
X Ray ◽  
H Nmr ◽  
Square Planar ◽  
Cleavage Reactions

The bulky trimesitylarsine ligand, As(mes)3, undergoes facile cyclopalladation to yield the dimeric complex, [Formula: see text], characterized by microanalysis, IR and 1H NMR spectroscopy. This complex is very stable but readily undergoes bridge-cleavage reactions with tertiary phosphine ligands having ligand cone angles less than 170°. The crystal structure for the PPh3 bridge-cleavage product is reported. This complex, [Formula: see text] is monoclinic, space group P21/c with a = 20.469(2), b = 12.702(2), c = 15.401(4) Å, β = 98.46(1)°, V = 3961 Å3Z = 4, R = 0.0284 and Rw = 0.0305. The Pd geometry is distorted square-planar with principal dimensions, Pd—Cl 2.395(1), Pd—P 2.318(1), Pd—C 2.056(3), and Pd—As 2.437(1) Å; As—Pd—Cl 96.5(1), Cl—Pd—P 90.9(1), P—Pd—C 93.7(1), As—Pd—C 78.9(1), As—Pd—P 172.6(1), and Cl—Pd—C 171.7(1)°. The average C—P—C angle (104.3(1)°) is smaller than expected and is rationalized on the basis of steric effects operative within the complex.

Boron Chelates and Boron-Metal Chelates, X [1]. 3-(2-Hydroxyphenyl)-2,2-diphenyl-1-oxa-3-azonia-2-borata-naphthalene-methanol (1/1): Synthesis, Spectroscopic Investigations and Crystal Structure

1982 ◽  
Vol 37 (11) ◽  
pp. 1450-1455 ◽  
Author(s):  
Rudolf Allmann ◽  
Eberhard Hohaus ◽  
Stanislaw Olejnik
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Structure Analysis ◽  
Title Compound ◽  
Chelate Ring ◽  
Boron Chelates ◽  
X Ray ◽  
Membered Chelate Ring ◽  
Compound C ◽  
Overall Ratio

The title compound, C25H20BNO2 · CH3OH, was examined by UV, IR, 1H, and 13C NMK spectroscopy as well as by thermogravimetry and X-ray structure analysis (Pbnb, a = 8.815, b = 17.309, c=28.992 Å, R= 5.5%). These investigations show the six-membered chelate ring (chelate A) to exist as formulated in [2] and not as a five-membered chelate ring B. One methanol molecule connects two chelate molecules by hydrogen bonds, resulting in an overall ratio of chelate to methanol of 1 : 1.

Crystal Structure, Spectroscopic and Redox Properties of Copper(II) Bis{2-[(2,6-dimethylphenyl)iminomethyl-3-methoxyphenolate]}

2007 ◽  
Vol 62 (9) ◽  
pp. 1133-1138 ◽  
Author(s):  
Veli T. Kasumov ◽  
Ibrahim Uçar ◽  
Ahmet Bulut ◽  
Fevzi Kösal
Keyword(s):  
Crystal Structure ◽  
Title Complex ◽  
Redox Properties ◽  
Orthorhombic Space Group ◽  
Long Distance ◽  
X Ray ◽  
X Ray Crystallography ◽  
Square Planar ◽  
Planar Molecules ◽  
Exchange Interaction Parameter

The coordination chemistry of N-(2,6-di-methylphenyl)-2-hydroxy-3-methoxybenzaldimine (1) with Cu(II) has been investigated by X-ray crystallography, electronic and EPR spectroscopies, as well as by electro- and magnetochemistry. The title complex 2 crystallizes in the orthorhombic space group P212121 (a = 8.1538, b = 17.7466, c =19.8507 Å). The mononuclear square-planar molecules 2 featuring trans-N2O2 coordination are connected via weak intermolecular C-H· · ·π interactions into infinite chains parallel to the a axis. Although the intermolecular Cu· · ·Cu separations within individual chains and between chains are very long (8.154 and 9.726 Å ), the exchange interaction parameter G = 2.03 < 4, estimated from solid state EPR spectra, suggests the existence of long-distance superexchange pathways between adjacent Cu(II) centers. The electronic and electrochemical features of the compound are also discussed.

The molecular and crystal structure of [Pt(diethylenetriamine)(guanosine)](ClO4)2

1979 ◽  
Vol 57 (1) ◽  
pp. 57-61 ◽  
Author(s):  
R. Melanson ◽  
F. D. Rochon
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Least Squares ◽  
Platinum Atom ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
R Factor ◽  
Square Planar ◽  
Coordination Plane

The crystal structure of [Pt(diethylenetriamine)(guanosine)](ClO4)2 has been determined by X-ray diffraction. The crystals are orthorhombic, space group P212121, with a = 12.486(6), b = 13.444(7), c = 14.678(11) Å, and Z = 4. The structure was refined by block-diagonal least-squares analysis to a conventional R factor of 0.050 and a weighted Rw = 0.045.The coordination around the platinum atom is square planar. Guanosine is bonded to platinum through N(7). The purine planar ring makes an angle of 62.7° with the platinum coordination plane. The structure is stabilized by hydrogen bonding.

scholarly journals Rubidium tetrafluoridobromate(III): redetermination of the crystal structure from single-crystal X-ray diffraction data

IUCrData ◽  
2019 ◽  
Vol 4 (11) ◽  
Author(s):  
Artem V. Malin ◽  
Sergei I. Ivlev ◽  
Roman V. Ostvald ◽  
Florian Kraus
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Diffraction Data ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Square Planar ◽  
Atomic Coordinates

Single crystals of rubidium tetrafluoridobromate(III), RbBrF4, were grown by melting and recrystallizing RbBrF4 from its melt. This is the first determination of the crystal structure of RbBrF4 using single-crystal X-ray diffraction data. We confirmed that the structure contains square-planar [BrF4]− anions and rubidium cations that are coordinated by F atoms in a square-antiprismatic manner. The compound crystallizes in the KBrF4 structure type. Atomic coordinates and bond lengths and angles were determined with higher precision than in a previous report based on powder X-ray diffraction data [Ivlev et al. (2015). Z. Anorg. Allg. Chem. 641, 2593–2598].

Polyfunctional phosphine ligands II. Iridium(I) complexes of the 7-diphenylphosphino-2,4-dimethyl-1,8-naphthyridine (dpnapy) ligand. X-ray crystal structure of [{Ir(cod)Cl}2(μ-dpnapy)]

1994 ◽  
Vol 216 (1-2) ◽  
pp. 209-216 ◽  
Author(s):  
Sandra Lo Schiavo ◽  
Maria Grassi ◽  
Giovanni De Munno ◽  
Francesco Nicolò ◽  
Giuseppe Tresoldi
Keyword(s):  
Crystal Structure ◽  
Phosphine Ligands ◽  
X Ray

Notizen: Bridging of Trigoldsulfonium Clusters by a Silver(I) Ion

1997 ◽  
Vol 52 (2) ◽  
pp. 301-304 ◽  
Author(s):  
Alexander Sladek ◽  
Hubert Schmidbaur
Keyword(s):  
Crystal Structure ◽  
Silver Atom ◽  
Metal Cluster ◽  
Phosphine Ligands ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Site Exchange ◽  
Mixed Metal Cluster ◽  
Short Contacts

Abstract Treatment of tris[(triphenylphosphine)gold(I)]-sulfonium tetrafluoroborate with AgBF4 (molar ratio 2:1) in tetrahydrofuran affords a hepta-nuclear mixed-metal cluster trication {[(Ph3P)6Au6AgS2](thf)}3+ as the tetrafluorobor­ate salt. The crystal structure of the compound has been determined by X-ray diffraction. The sil­ver atom is found in a bridging position between the two Au3S units with short contacts to both sulfur atoms and to three out of six gold atoms. The coordination sphere of the silver atom is complemented by a tetrahydrofuran molecule. In di(tri)chlorom ethane solutions there is rapid site exchange of the silver coordination as shown by virtual equivalence of the phosphine ligands on the NMR time scale at ambient temperature.

Preparation and characterization of some ruthenium(II) porphyrins containing tertiary phosphine axial ligands, including the crystal structure of (octaethylporphinato)bis(triphenylphosphine)ruthenium(II)

1984 ◽  
Vol 62 (4) ◽  
pp. 755-762 ◽  
Author(s):  
Sara Ariel ◽  
David Dolphin ◽  
George Domazetis ◽  
Brian R. James ◽  
Tak W. Leung ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Phosphine Ligands ◽  
Tertiary Phosphine ◽  
X Ray ◽  
Porphyrin Complex ◽  
H Nmr ◽  
Axial Ligands ◽  
Nmr Data ◽  
Phosphine Complex

The ruthenium(II) porphyrin complex Ru(OEP)(PPh3)2 (OEP = the dianion of octaethylporphyrin) has been prepared from Ru(OEP)(CO)EtOH, and the X-ray crystal structure determined; as expected, the six-coordinate ruthenium is situated in the porphyrin plane and has two axial phosphine ligands. Synthesized also from the carbonyl(ethanol) precursors were the corresponding tris(p-methoxyphenyl)phosphine complex, and the Ru(TPP)L2 (TPP = the dianion of tetraphenylporphyrin, L = PPh3, P(p-CH3OC6H4)3, P″Bu3) and Ru(TPP)(CO)PPh3 complexes. Optical and 1H nmr data are presented for the complexes in solution. In some cases dissociation of a phosphine ligand to generate five-coordinate species occurs and this has been studied quantitatively in toluene at 20 °C for the Ru(OEP)L2 and Ru(TPP)L2 systems.

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