Showing papers by "Richard D. Adams published in 1993"
TL;DR: In this paper, the complex Os[sub 3 ] with tetrahydrothiophene (THT) at 25°degree C was decarbonylated and transformed into the new compound Os [sub 3]-CO using a 3-butenethiolate ligand in which the sulfur atom bridges one of the metal-metal bonds.
Abstract: The complex Os[sub 3](CO)[sub 10]([bar S]CH[sub 2]CH[sub 2]CH[sub 2]CH[sub 2])[sub 2] (1) was prepared by the reaction of Os[sub 3](CO)[sub 10](NCMe)[sub 2] with tetrahydrothiophene (THT) at 25[degree]C. When heated to 97[degree]C, 1 was transformed into the complex Os[sub 3](CO)[sub 10][[mu]-[eta][sup 2]-([bar S]CH[sub 2]CH[sub 2]CH[sub 2]CH)]([mu]-H) (2) by loss of one THT ligand and the activation of a C-H bond on one of the methylene groups bonded to the sulfur atom. At 125[degree]C, 2 was decarbonylated and transformed into the new compound Os[sub 3](CO)[sub 9][[mu]-[eta][sup 3]-S(CH[sub 2])[sub 2]CH=CH[sub 2]]([mu]-H) (3) by a ring-opening cleavage of one of the C-S bonds. Compound 3 contains a 3-butenethiolate ligand in which the sulfur atom bridges one of the metal-metal bonds and the double bond is [pi]-coordinated to one of the sulfur-bridged metal atoms. An investigation of the transformation of Os[sub 3](CO)[sub 10][[mu]-([bar S]CH[sub 2]CD[sub 2]CD[sub 2]CH)]-([mu]-H) (2-d[sub 4]) into Os[sub 3](CO)[sub 9][[mu]-[eta][sup 3]-SCH[sub 2]CD[sub 2]CD=CH[sub 2]]([mu]-D) (3-d[sub 4]) at 125[degree]C showed that the hydride ligand was returned to the carbon atom from which it was initially cleaved and deuterium was shifted to the metal atoms. When heated to 205[degree]C, compound 3 released butene. Complexes 1-3 were characterized by single-crystal X-ray diffraction analysis. Crystallographic datamore » are provided. 18 refs., 3 figs., 7 tabs.« less
37 citations
TL;DR: In this article, a new platinum-ruthenium heteronuclear cluster complex Pt2Ru4(CO)18,1 was obtained in 60% yield from the reaction of Ru (CO)5 and Pt(COD)2, COD = 1, 5-cyclooctadiene.
Abstract: From the reaction of Ru(CO)5 and Pt(COD)2, COD = 1, 5-cyclooctadiene, the new platinum-ruthenium heteronuclear cluster complex Pt2Ru4(CO)18,1, was obtained in 60% yield.1 has a folded ladder-like structure with alternating pairs of ruthenium atoms and platinum atoms. The cluster of1 can be split to yield the known compound PtRu2(CO)8(η2-dppe),2, (54% yield) by reaction with 1, 2-bis(diphenylphosphino)ethane, dppe, at 25°C. When1 was treated with excess dppe at 40°C, thebis-diphos compound3, PtRu2(CO)6(μ-η2-dppe)2 was obtained (39% yield). Under the similar reaction conditions,2 was converted to3 in 44% yield. All these complexes were characterized by single crystal X-ray diffraction analyses. Compounds2 and3 both contain a triangular cluster of one platinum and two ruthenium atoms, but in2 the bidentate ligand, dppe, chelates the platinum atom and in3 the two dppe ligands bridge the two Pt-Ru metal-metal bonds. Crystal data for1: space group C2/c,a=12.542(2)A,b=15.350(4)A,c=15.252(3)A, β=105.32(2)°,Z=4, 2192 reflections,R=0.025. For2: space group P21/c,a=14.351(2)A,b=13.486(3)A,c=19.218(3)A, β=108.48(1)°,Z=4, 3029 reflections,R=0.027. For3: space group P21/c,a=18.836(6)A,b=15.559(5)A,c=23.259(7)A, β=111.26(2)°,Z=4, 4204 reflections,R=0.038.
25 citations
25 citations
TL;DR: In this article, it was shown that it is possible to open an azetidine ring in a cluster complex under conditions sufficiently mild that a detailed study of the process might be possible, and two other complexes formed by transformation of the Azetidine ligand have been isolated and characterized.
21 citations
TL;DR: The first example of a metal complex containing the ligand cyclobutyne was reported in this article, where the C[sub 4] ring was opened when the complex was heated to 125 [degree]C.
17 citations
TL;DR: BaCo 2 Si 2 O 7 was obtained by heating the mixture of BaCO 3, CoCO 3 and SiO 2 to 1300°C for 48 hours as discussed by the authors, and was characterized by single-crystal X-ray diffraction and magnetic susceptibility measurements.
16 citations
15 citations
TL;DR: In this paper, the reaction of 4-tert-butyl-4-methyl-1-(phenylthio)-cyclobutene with Os[sub 3](CO)[sub 10]/(NCMe)[sub 2] at 25 degrees C yielded the new compound Os[Sub 3]( CO)[sub 9]-[mu][sub 3]-[eta][sup 2]-C[sub 2]-CH[sub 6]-C(Me)[sup t]Bu]([mu]-H), 3 (54% yield), by displacement of the MeCN ligands
14 citations
TL;DR: In this paper, the presence of crossover in a reaction of a mixture of labeled and unlabeled 1 is consistent with the insertion of the alkyne into the metal-metal bond by an intramolecular mechanism.
13 citations
TL;DR: In this paper, a series of complexes with the general formula Re(CO)[sub 4][trans-[mu]-HC=C(CO[sub 2]Me)] with aryl isothiocyanates have been obtained.
13 citations
TL;DR: In this paper, the alkenyl-N-arylthioamide complexes Re(CO)[sub 4][(E)-HC=C(CO[sub 2]Me)C=N-(C[sub 6]H[sub 4]-p-R)S] were characterized by single crystal X-ray diffraction analyses.
TL;DR: In this paper, a metallacyclic ring formed by the coupling of one molecule of HC[triple bond]COEt to one CO ligand was characterized by a single-crystal X-ray diffraction analysis.
TL;DR: The hexamolybdenum cluster complex [Mo6(μ3-Cl)8(O2CMe)6]2−, 1 was isolated as the Bu4N+ salt in 71% yield from the reaction of (Bu4N)2[Mo 6(μ 3-C)8Cl6] with AgO 2CMe in CH2Cl2 solvent as mentioned in this paper.
Abstract: The hexamolybdenum cluster complex [Mo6(μ3-Cl)8(O2CMe)6]2−, 1 was isolated as the Bu4N+ salt in 71% yield from the reaction of (Bu4N)2[Mo6(μ3-Cl)8Cl6] with AgO2CMe in CH2Cl2 solvent. The compound was characterized by single crystal X-ray diffraction analysis. The cluster contains an octahedral arrangement of six molybdenum atoms with eight chloride ligands bridging the eight trianglar faces and six carboxylate ligands terminally coordinated through one oxygen atom to each of the six molybdenum atoms. Crystal data: space group =P21/n,a=10.713(3)A,b=14.43(1)A,c=21.919(4)A, β=94.37(2)°,Z=2, 1965 reflections,R=0.036.
TL;DR: In this paper, the reactions of thiacyclohexane (TCH) with Os[sub 3](CO)[sub 10](NCMe)[sub 2] at 25°degree]C yielded the disubstituted product O(sub 3]-CO[sub 10]-TCH in 86% yield.
TL;DR: In this article, the Re-C complex with p-tolylisothiocyanate was characterized by IR, {sup 1}H NMR, and single-crystal X-ray diffraction analyses.
TL;DR: The trirhenium complex Re 3 (CO) 10 [μ- SCH 2 CH 2 CH2 ](μ-H) 3 ( 1 ) was found to produce an oligomerization of thietane at 25° C over 18 hours to yield the new complex Re3 (CO), in 47% yield as discussed by the authors.
TL;DR: In this article, the reactive acetonitrile complex (OC)[sub 4]Re[trans]-mu]-HC=C(CO[sub 2]Me)]Re(CO)[sub 5]
TL;DR: In this article, the electron-rich alkynes, MeC{triple_bond}CX, X = NMe{sub 2} or OEt, were added to the dimanganese complex to yield the vinylidene complexes.
TL;DR: The reaction of PtRu5(CO)16(μ6-C),1 with 3-hexyne in the presence of UV irradiation produced two new electron-rich platinum-ruthenium cluster complexes.
Abstract: The reaction of PtRu5(CO)16(μ6-C),1 with 3-hexyne in the presence of UV irradiation produced two new electron-rich platinum-ruthenium cluster complexes PtRu5(CO)13(μ-EtC2Et)(μ3-EtC2Et)(μ5-C),2 (20% yield) and Pt2Ru6(CO)17(μ-η5-Et4C5)(μ3-EtC2Et) (μ6-C),3 (7% yield). Both compounds were characterized by single-crystal X-ray diffraction analyses. Compound2 contains of a platinum capped square pyramidal cluster of five ruthenium atoms with the carbido ligand located in the center of the square pyramid. A EtC2Et ligand bridges one of the PtRu2 triangles and the Ru-Pt bond between the apical ruthenium atom and the platinum cap. The structure of compound3 consists of an octahedral PtRu5 cluster with an interstitial carbido ligand and a platinum atom capping one of the PtRu2 triangles. There is an additional Ru(CO)2 group extending from the platinum atom in the PtRu5 cluster that contains a metallated tetraethylcyclopentadienyl ligand that bridges to the platinum capping group. There is also a EtC2Et ligand bridging one of the PtRu2 triangular faces to the capping platinum atom. Compounds2 and3 both contain two valence electrons more than the number predicted by conventional electron counting theories, and both also possess unusually long metal-metal bonds that may be related to these anomalous electron configurations. Crystal data for2, space group Pna21,a=19.951(3) A,b=9.905(2) A,c=17.180(2) A,Z=2, 1844 reflections,R=0.036; for3, space group Pna21,α=13.339(1) A,b=14.671(2) A,c=11.748(2) A, α=100.18(1)°, β=95.79(1)°, γ=83.671(9)°,Z=2, 3127 reflections,R=0.026.
TL;DR: In this paper, the triosmium complex with diphenylacetylene at 97°degree C resulted in the formation of three products: the known compound Os[sub 2](CO)[sub 6]-[mu]-[eta][sup 2]-C=CHCH[sub 1]CH [sub 2]
TL;DR: In this article, two new mixed metal cluster complexes were obtained from the reaction of Ru3(CO)9(μ3-S)2,1 with Pt(PPh3)2(C2H4) at 0°C.
Abstract: Two new mixed metal cluster complexes PtRu3(CO)10(PPh3)(μ3-S)2,3 14% yield and PtRu3(CO)9(PPh3)2(μ3-S)2,4 23% yield were obtained from the reaction of Ru3(CO)9(μ3-S)2,1 with Pt(PPh3)2(C2H4) at 0°C. The cluster of4 consists of a spiked triangle of four metal atoms with two triply bridging sulfido ligands. The reaction of Ru4(CO)11(μ4-S)2,2 with Pt(PPh3)2(C2H4) yielded the expanded mixed-metal cluster complex PtRu4(CO)12(PPh3)(μ4-S)2,5 in 12% yield. The structure of the cluster5 can be described as a pentagonal bipyramid of five metal atoms and two sulfido ligands with one metal-metal bond missing. Compounds4 and5 were characterized by a single-crystal X-ray diffraction analyses.
TL;DR: In this article, the results of a single-crystal X-ray diffraction analysis were obtained from the reaction of Mn[sub 2](CO)[sub 9]-MeCN, 1, with HC[triple bond]CCO(sub 2]Me in hexane solvent at 25 degrees C.
TL;DR: The hexanuclear tungsten cluster complex [W6(μ3-Cl)8Cl6]2−,1 was isolated as a salt of the cation (MeO2CCH2)2N(H)CH2CH2N (CH2CO2Me)2+, EDTEH+, by crystallization from methanol solvent of the product obtained from the reaction of (H3O)2[W6μ3Cl) 8Cl3] with the disodium salt of ethylenediaminetetraacetic acid as discussed by the authors
Abstract: The hexanuclear tungsten cluster complex [W6(μ3-Cl)8Cl6]2−,1 was isolated as a salt of the cation (MeO2CCH2)2N(H)CH2CH2N(CH2CO2Me)2+, EDTEH+, by crystallization from methanol solvent of the product obtained from the reaction of (H3O)2[W6(μ3-Cl)8Cl3] with the disodium salt of ethylenediaminetetraacetic acid. The compound was charcterized by single-crystal X-ray diffraction analysis. The cluster anion contains an octahedral arrangement of six tungsten atoms with chloride ligands bridging the eight triangular faces of the cluster and one chloride ligand terminally coordinated to each of the six tungsten atoms. The cation (EDTEH)+ achieves its positive charge by protonation of one of the nitrogen atoms. Crystal data: space group = P21/a,a=10.689(2) A,b=22.931(6) A,c=12.093(3) A, β=98.41(2)°,Z=2, 2476 reflections,R=0.028.
TL;DR: BaCo 2 Si 2 O 7 was obtained by heating the mixture of BaCO 3, CoCO 3 and SiO 2 to 1300°C for 48 hours as mentioned in this paper, and was characterized by single-crystal X-ray diffraction and magnetic susceptibility measurements.
Abstract: The new compound BaCo 2 Si 2 O 7 was obtained by heating the mixture BaCO 3 , CoCO 3 and SiO 2 to 1300°C for 48 h. The material was characterized by single-crystal X-ray diffraction and magnetic susceptibility measurements. Each cobalt ion is surrounded by four oxygen atoms arranged in a distorted tetrahedral shape. These tetrahedral are linked into chains through the sharing of one of the oxygen atoms. The CoO 4 chains are cross-linked by bridging Si 2 O 7 groups. The barium ions occupy channels that run parallel to the crystallographic c -axis. The effective magnetic moment, μ eff = 4.70 B.M., at 25°C is consistent with Co 2+ in a tetrahedral environment having three unpaired electrons. Anti-ferromagnetic coupling of the electrons occurs between the nearest neighbour cobalt ions, as indicated by the sign of the Weiss constant, θ p = −46 K, and by the presence of a broad maximum in the susceptibility curve. At 26 K it undergoes a three-dimensional magnetic transition into a field-induced weak ferromagnet that is characteristic of a one-dimensional metamagnet.