Cyclopentadienyl-ruthenium and -osmium chemistry. XXII. Synthesis, X-ray structure and some reactions of RuCl(PPh3,)(η1-dppm)(η-C5H5),containing a monodentate CH2(PPh2)2 ligand

1983 ◽  
Vol 36 (10) ◽  
pp. 2065 ◽  
Author(s):  
MI Bruce ◽  
MG Humphrey ◽  
JM Patrick ◽  
AH White
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Structural Parameters ◽  
The Other ◽  
Chloro Complex ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Halogen Exchange

.Stoichiometric amounts of RuCl(PPh3)2(η-C5H5) and dppm react in refluxing C6H6 to give RuCl- (PPh3)(η1-dppm)(η-C5H5) which has been fully characterized by an X-ray study (triclinic, space group P1, a 22.377(6), b 9.913(2), c 9.826(3)Ǻ, α 70.46(2), β 78.72(2), γ 80.40(2)°, Z 2) in which 3299 data [I > 3σ(I)] were refined to R 0.046, R' 0.052. Structural parameters are similar to those of other RuX(PR3)2(η-C5H5) complexes. The chloro complex was converted into [Ru(PPh3)(η2- dppm)(η-C5H5)]+ salts; the other PPh3 ligand can be replaced by a second dppm ligand to give [Ru(dppm)2(q-C5H3)+ which contains both mono- and bidentate dppm ligands. Alkylation of the uncoordinated phosphorus with MeI is accompanied by halogen exchange to give [RuI(PPh3)- (PPh2CH2PMePh2)(η-C5H5)I], while reactions with a variety of transition metal complexes result in abstraction of PPh3 and formation of RuCl(dppm)(η-C5H5).

Reaktionen N-silylierter Endiamine, I Übergangsmetallkomplexe von 1,3-Diaza-2-sila-4-cyclopentenen / Reactions of N-Silated Endiamines, I Transition Metal Complexes of 1,3-Diaza-2-sila-4-cyclopentenes

1986 ◽  
Vol 41 (10) ◽  
pp. 1230-1238 ◽  
Author(s):  
Michael Zettlitzer ◽  
Heindirk tom Dieck ◽  
Lutz Stamp
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Structure Analysis ◽  
Transition Metal Complexes ◽  
Structural Data ◽  
Spectroscopic Properties ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Poorly Soluble

Abstract1,3-Di̲aza-2-s̱ila-4-c̱yclopentenes 1 (DISC), which are electron-rich and easily oxidizable ole­ fins, form strongly coloured, but poorly soluble 1:1 adducts with cuprous halides, while silver trifluoromethylsulfonate oxidizes 1. Much more soluble and again strongly coloured complexes of stoichiometry LPdX2, (L)1.5PdX2 and L 2PdX2 are formed from 1 and palladium halides. The well-crystallizing adduct (PdCl2 · L)2 3a was chosen for an X-ray structure analysis (monoclinic, space group P2/c; a = 10.215(3), b = 14.681(3), c =23.642(5) Å , β = 101.31(2)°; Z = 8 ; R = 0.054), which revealed an almost planar DISC ligand in an oblique η2(C=C)-coordination relative to the π-plane. Structural data and rather peculiar spectroscopic properties encourage a comparison of 3a with complexes, in which an electron-rich olefin is split to give a bis(carbene) ligand system. The electronic reasons for the splitting of electron-rich olefins at d8 metals are discussed under symmetry considerations.

Synthesis and Structural Systematics of First-Row Transition Metal Complexes with 2-[Bis(benzimidazol-2-ylmethyl)amino]ethanol

1987 ◽  
Vol 42 (10) ◽  
pp. 1307-1314 ◽  
Author(s):  
Kazuhiro Takahashi ◽  
Yuzo Nishida
Keyword(s):  
Transition Metal ◽  
Metal Ions ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Structural Parameters ◽  
Biological Systems ◽  
Tridentate Ligand ◽  
Crystal Data ◽  
Space Group ◽  
Distorted Octahedral

Abstract A nickel(II) complex with (bbimae) (= 2-[bis(benzimidazol-2-ylmethyl)amino]ethanol), [Ni(bbimae)(NCS)2] · H2O (1) and an oxovanadium(IV) complex, [VO(bbimae)(NCS)2] · dma (dma = N.N-dimethylacetamide) (2) have been prepared and their crystal structures determined by X-ray diffraction. Crystal data for 1 at 293 K: a = 13.334(2). b = 17.048(2), c = 10.3829(9) Å, space group P212121, Z = 4, and dcalcd = 1.41 gcm-3. Crystal data for 2 at 293 K: a = 14.099(2). b = 14.998(4), c = 14.051(2) Å, β = 107.634(9)°, space group P21/c, Z = 4, and dcalcd = 1.36 gcm-3. In the nickel(II) complex, (bbimae) functions as a tetradentate ligand, and the geometry around Ni(II) ion is best described as distorted octahedral. The structure is very similar to those of the correspond­ing Co(II) and Mn(II) complexes. In the case of 2, which is also distorted octahedral, (bbimae) is a tridentate ligand without the coordination of the alcohol group. The M-N (benzimidazole) distances are in the range of 1.95-2.18 Å, and also observed for other first-row transition metal complexes with (bbimae). and differ in the order V(IV) < Mn(II) > Co(II) > Ni(II) > Cu(II). consistent with effective ionic radii of the metal ions. Comparison of the structural parameters of these complexes with those of the metal ions in biological systems has supported the usefulness of the tripod-like ligands to synthesis model compounds for biological systems.

Synthesis, characterization, and X-ray structural studies of octahedral transition metal complexes incorporating the novel anionic tridentate ligand, dimethyl(ethanolamino)(1-pyrazolyl)- gallate, [Me2Ga(OCH2CH2NH2)(N2C3H3)]−

1978 ◽  
Vol 56 (9) ◽  
pp. 1212-1221 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Tridentate Ligand ◽  
The Novel ◽  
Structural Studies ◽  
Space Group ◽  
X Ray ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral

Details of the synthesis and physical properties of octahedral transition metal complexes of the tridentate tris chelating ligand [Me2Ga(OCH2CH2NH2)(N2C3H3)]− are given. Crystals of sym-fac-bis[dimethyl(ethanolamino)(1-pyrazolyl)gallato(N(2),O,N]nickel(II) are monoclinic, a = 11.7908(6), b = 7.3158(6), c = 12.5797(8), β = 97.035(7)°, Z = 2, space group P21/n and crystals of the mer isomer are monoclinic, a = 18.6617(7), b = 8.7941(4), c = 13.5670(8), β = 91,766(4)°, Z = 4, space group P21/c. The structures were solved by Patterson and Fourier syntheses and were refined by full-matrix least-squares procedures to final R values of 0.048 and 0.052 for 1881 and 2573 reflections with I ≥ 3σ(I) for the fac and mer isomers respectively. The nickel atoms in both structures were found to have distorted octahedral coordination geometry. Bond lengths (corrected for libration) are: Ni—O, 2.090(3); Ni—N, 2.085(3) and 2.112(3); Ga—O, 1.908(3); Ga—N, 2.010(3); and Ga—C, 1.979(5) and 1.981(6) Å for the fac isomer, and Ni—O, 2.045(4) and 2.049(4); Ni—N, 2.091 (4)-2.156(5); Ga—O, 1.898(4) and 1.899(4); Ga—N, two at 1.991 (5); and Ga—C, 1.948(8)-1.971 (7) Å for the mer isomer.

Preparation, properties and structure of some intermediate nido- and arachno-monocarbaboranes

1981 ◽  
Vol 46 (10) ◽  
pp. 2345-2353 ◽  
Author(s):  
Karel Baše ◽  
Bohumil Štíbr ◽  
Jiří Dolanský ◽  
Josef Duben
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Nmr Spectra ◽  
Liquid Ammonia ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Starting Compound

The 6-N(CH3)3-6-CB9H11 carbaborane reacts with sodium in liquid ammonia with the formation of 6-CB9H12- which was used as a starting compound for preparing the 4-CB8H14, 9-L-6-CB9H13 (L = (CH3)2S, CH3CN and P(C6H5)3), 1-(η5-C5H5)-1,2-FeCB9H10-, and 2,3-(η5-C5H5)2-2,31-Co2CB9H10- carboranes. The 4-CB8H14 compound was dehydrogenated at 623 K to give 4-(7)-CB8H12 carborane. Base degradation of 6-N(CH3)3-6-CB9H11 in methanol resulted in the formation of 3,4-μ-N(CH3)3CH-B5H10. The structure of all compounds was proposed on the basis of their 11B and 1H NMR spectra and X-ray diffraction was used in the case of the transition metal complexes.

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