C 33 H 25 Bi 2 Br 6 N 7 O 7 S 6 , P1 (no. 2), a =13.484(1) Å, b =13.631(1) Å, c =15.249(1) Å, a =94.434(1)°, b =114.215(2)°, g =107.841(2)°, V =2365.9 Å 3 , Z =2,R gt(F) =0.066, wRref(F 2 ) =0.194, T =298 K.
Source of materialAs olution of Bi(NO 3 ) 3. · . 5H 2 O( 475 mg, 1m mol) in water (15m L) was dropped slowly into as olution of 5-bromo-1-hydroxy-2(1H)-pyridinethione (5-Br-HPT, 618 mg, 3mmol) in EtOH (25 mL). The mixed solution was stirred for 3hat40°Cand was then cooled to room temperature to give yellow polycrystals, which were collected by filtration, washed successively with H 2 Oand EtOH, and dried in vacuo. Yellow square-shaped crystals suitable for X-ray analysis were obtained by recrystallization of the precipitate from N,N-dimethylformamid (m.p. 247 -249°C).
DiscussionBismuth compounds have been used to treat avariety of medical disorders for over 200 years [1]. Current interest in bismuth thiolates derives in part from their ability as fungicides, antitumor agents, nanoparticle synthesis and mechanism research of bioactivity [2][3][4][5]. Although Bi(III) compounds of the Bi(mpo) 3 and Bi(ph)(mpo)2 (Hmpo =2 -mercaptopyridine-N-oxide) have been prepared previously [6,7], X-ray structural data are available only for not-substituted base on the pyridine ring. The crystal structure of the title compound is adimer with heptacoordination for each bismuth imposed by three sulfur and four oxygen atoms. Except for bridging oxygen atom O2, the coordination polyhedron around Bi1 can be described as ad istorted trigonal prism with O1, S1, S4 and O3, O4, S3 at the triangular bases (dihedral angle between their mean planes 29.3(4)°,which is larger than 9.5(2)°in Bi(mpo) 3 ) [7], different from Fe(mpo) 3 [8]. In Fe(mpo)3,the arrangement of the ligands gives the complex with meridional octahedral geometry.