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Mono and dinuclear gold(I) complexes with neutral and deprotonated 1,4-benzodiazepin-2-ones: crystal and molecular structure of (L-H)Au(PPh3)•Et2O, where L = 1,3-dihydro-7-nitro-5-phenyl-2H-1,4-benzodiazepin-2-one, nitrazepam

Cinellu, Maria Agostina and Stoccoro, Sergio and Minghetti, Giovanni and Bandini, Anna Laura and Demartin, Francesco (1990) Mono and dinuclear gold(I) complexes with neutral and deprotonated 1,4-benzodiazepin-2-ones: crystal and molecular structure of (L-H)Au(PPh3)•Et2O, where L = 1,3-dihydro-7-nitro-5-phenyl-2H-1,4-benzodiazepin-2-one, nitrazepam. Inorganica Chimica Acta, Vol. 168 (1), p. 33-41. ISSN 0020-1693. Article.

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DOI: 10.1016/S0020-1693(00)88014-7

Abstract

The preparation of a series of neutral (L)AuCL (1a–3a) and cationic [(L)Au(PPh3)] [BF4] (1b–5b) gold(I) complexes is described (L = DIAZEPAM, 1; PRAZEPAM, 2; NITRAZEPAM, 3; LORAZEPAM, 4; NIMETAZEPAM, 5).
In the presence of alkali, (PPh3)AuCl reacts with 1-unsubstituted 1,4-benzodiazepin-2-ones such as NITRAZEPAM (3) and LORAZEPAM (4) to give neutral gold(I) species (L-H)Au(PPh3) (3c and 4c). The benzodiazepine anion is bonded to Au via the N(1) atom, as shown, in the case of 3c, by X-ray analysis: (L-H)Au(PPh3)•Et2O, C33H25AuN3O3P• C4H10O, monoclinic, space group P21/c, a= 12.717(9), b=19.270(7), c=14.696(3) Å, β= 107.85(3)°, Z= 4. Au---P = 2.238(1), Au---N = 2.071(3) Å. The crystal structure was determined by standard methods and refined to R = 0.028 and Rw = 0.035 on the basis of 4456 unique reflections. p ]The complex 3c reacts with [(Ph3P)Au(S)][BF4], as obtained from (PPh3)AuCl and AgBF4 in methanol, to give the dinuclear cationic species [(Ph3P)Au{μ(L-H)}Au(PPh3)] [BF4] (3d) where the deprotonated NITRAZEPAM bridges two (Ph3P)Au groups through the N(1) and N(4) atoms. All the new derivatives were characterized by elemental analyses and spectroscopic methods (IR; 1H, 31P NMR).

Item Type:Article
ID Code:4903
Status:Published
Refereed:Yes
Uncontrolled Keywords:Gold(I) complexes, benzodiazepines, spectroscopy
Subjects:Area 03 - Scienze chimiche > CHIM/03 Chimica generale e inorganica
Divisions:001 Università di Sassari > 01 Dipartimenti > Chimica
Publisher:Elsevier Science
ISSN:0020-1693
Deposited On:22 Nov 2010 12:15

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