Synthesis and x-ray structure of a dimeric rhenium(V) compound: Re2O3Cl4(3,5-Me2pzH)4.cntdot.Me2CO (pzH = pyrazole)

Backes-Dahmann, G.; Enemark, John H.

doi:10.1021/ic00270a029

Cited by 37 publications

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“…It is not clear whether oxygen originates from the solvent or air leaking into the argon-filled closed flask. A related [{ReClzOpy2}20] dimer, in which the pyridine ligands are cis to one another, has been prepared by Lock & Turner (1978) (Lock & Turner, 1978;Backes-Dahmann & Enemark, 1987). The Re---N distances determined here are in agreement with these studies.…”

Section: Commentsupporting

confidence: 75%

Structure of μ-oxo-bis[dichlorobis(1-methylimidazole-N3)oxorhenium(V)], [{ReOCl2(C4H6N2)2}2O]

Pearson¹,

Beauchamp²

1994

Acta Crystallogr C

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o(i) 1 0(2) ~c( ) i C(4) Fig. 1. ORTEP drawing of the [{ReOCIdC4H6N2)2}20] molecule. Ellipsoids are drawn at the 50% probability level. H atoms are shown as spheres of arbitrary size. Abstract The crystals contain dinuclear molecules in which all-trans octahedral ReCl2(O)2(1-methylimidazole)2 units share an O-atom apex. The ~Re--O---Re--O backbone is linear by symmetry and the bonds in the ReCI2N2 planes of the two units are staggered. The main bond lengths are: Re---O=l.913(1), Re--O = 1.703 (8), Re---CI = 2.415 (2) and Re--N = 2.132 (6) A. AbstractThe complex [TcCI(NO)(CloHI6As2)2] + lies on a crystallographic inversion centre with disordering of the trans chloro and nitrosyl ligands. The coordination about Tc is close to octahedral with Tc--As distances of 2.479 (1) and 2.502 (2)A. The As--C mean distance is 1.924 (15)A and the angles at As are within 10 ° of tetrahedral.

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Section: Commentsupporting

confidence: 75%

Structure of μ-oxo-bis[dichlorobis(1-methylimidazole-N3)oxorhenium(V)], [{ReOCl2(C4H6N2)2}2O]

Pearson¹,

Beauchamp²

1994

Acta Crystallogr C

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“…[4][5][6][7][8] Complexes with nitroimidazoles and nitropyrazoles have found application as markers for hypoxic tumor cells. 9, 10 These aspects of the chemistry of rhenium complexes with pyridine and imidazole derivatives have been studied in depth. [11][12][13][14][15][16][17][18][19][20] Coordination compounds of rhenium with other heterocyclic ligands, such as pyrazoles and triazoles, have received attention only recently.…”

mentioning

confidence: 99%

“…29 The first structurally characterized rhenium com plex with the pyrazole ligand, [Re 2 O 3 Cl 4 (3,5 Me 2 pzH) 4 ]• •(CH 3 ) 2 CO, was isolated in attempting to synthesize Re V complexes with [HB(3,5 Me 2 pz) 3 ] -. 10 The aim of the present study was to investigate the reactions of Re V , Re IV , and Re III complexes with 3,5 dimethylpyrazole.…”

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confidence: 99%

Rhenium(IV) and rhenium(V) complexes with 3,5-dimethylpyrazole

et al. 2006

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Mono and dinuclear Re IV and Re V complexes with 3,5 dimethylpyrazole (Me 2 pzH) were synthesized. The cis [Re 2 O 3 Cl 4 (3,5 Me 2 pzH) 4 ] complex (cis 1) was prepared by the reaction of NH 4 ReO 4 with K[HB(Me 2 pz) 3 ] in concentrated HCl or by refluxing of [ReCl 3 (MeCN)(PPh 3 ) 2 ] with Me 2 pzH in air. The bromide complex trans [Re 2 O 3 Br 4 (3,5 Me 2 pzH) 4 ] (trans 2) was synthesized by passing dry HBr through a solution of [Re 2 O 3 Br 2 (µ 3,5 Me 2 pz) 2 (3,5 Me 2 pzH) 2 ] (4) in chloroform. The pyrazolate bridged complex [Re 2 O 3 Cl 2 (µ 3,5 Me 2 pz) 2 (3,5 Me 2 pzH) 2 ] (3) was prepared from (Et 4 N) 2 [ReOCl 5 ] or Cs 2 [ReOCl 5 ] and Me 2 pzH. The corresponding bromide and iodide complexes [Re 2 O 3 X 2 (3,5 Me 2 pz) 2 (3,5 Me 2 pzH) 2 ]•C 6 H 6 (X = Br (4) or I (5)) were synthesized by the reactions of (NH 4 ) 2 [ReBr 6 ] or K 2 [ReI 6 ], respectively, with Me 2 pzH. The [ReO(OMe)(3,5 Me 2 pzH) 4 ]Br 2 • •3,5 Me 2 pzH•4H 2 O complex (6) was obtained as a by product in the synthesis of complex 4. The reaction of [ReNCl 2 (PPh 3 ) 2 ] with Me 2 pzH was accompanied by hydrolytic denitration giving rise to the mixed ligand complex [Re 2 O 3 Cl 2 (µ 3,5 Me 2 pz) 2 (3,5 Me 2 pzH)(PPh 3 )] (7). The reaction of (NH 4 ) 2 [ReBr 6 ] with a Me 2 pzH melt gave the trans [ReBr 4 (3,5 Me 2 pzH) 2 ]• •Me 2 CO complex (8). The structures of complexes 2 and 4-8 were established by X ray diffraction. All compounds were characterized by elemental analysis, electronic absorption spectroscopy, 1 H NMR and IR spectroscopy, mass spectrometry, and cyclic voltammetry.

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“…The origin of cis-location of p-acid ligands towards the oxo group seems to be dominated by electronic influence of the multiply bonded ligand, which forces the metal non-bonding d electrons to lie in the in the plane perpendicular to the M-O bond axis. This general rule appears to hold for isonitrile, carbonyl, olefin, acetylene, thioether and often phosphine ligands [14][15][16][17] [26,27]. The bond valences were computed as m ij ¼ exp½ðR ij À d ij Þ=B [28][29][30], where R ij is the bond-valence parameter (in the formal sense R ij is the single-bond length between i and j atoms) [31].…”

Section: Resultsmentioning

confidence: 99%

Synthesis and spectroscopic investigation of the pyrazole complexes. The X-ray structure of [ReOBr 3 (OAsPh 3 )(pzH)]

Machura

Dziegielewski

Kruszyński

et al. 2003

Inorganic Chemistry Communications

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Synthesis and x-ray structure of a dimeric rhenium(V) compound: Re2O3Cl4(3,5-Me2pzH)4.cntdot.Me2CO (pzH = pyrazole)

Cited by 37 publications

References 0 publications

Structure of μ-oxo-bis[dichlorobis(1-methylimidazole-N3)oxorhenium(V)], [{ReOCl2(C4H6N2)2}2O]

Structure of μ-oxo-bis[dichlorobis(1-methylimidazole-N3)oxorhenium(V)], [{ReOCl2(C4H6N2)2}2O]

Rhenium(IV) and rhenium(V) complexes with 3,5-dimethylpyrazole

Synthesis and spectroscopic investigation of the pyrazole complexes. The X-ray structure of [ReOBr 3 (OAsPh 3 )(pzH)]

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