The complex(2-pyridinecarboxylato) 2 diphenyltin?was synthesized by the reaction of 2-pyridinecarboxylic acids with the diphenyltin?oxide.The crystal structure was determined by X-ray diffraction.The crystal belongs to monoclinic with space group P2 1 /n,a=1.46504(19)nm,b=1.01225(13)nm,c=1.45406(19)nm,β=94.849(2)°,Z =4,R 1 =0.0285,w R 2 =0.0672.In this complex,the tin ato m rendered six-coordinate in a distorted octahedron geometry.Eac h central tin atom is surrounded equatorial by two oxygen atoms coming fro m two carboxyl groups,one nitrogen atom c oming from pyridinyl group and one carbon atom of the penyl group and axially by one carbon atom of the phenyl group and one nitrogen atom coming from pyridinyl group.CCDC:180021.
The chlorodibenzyltin dithiopiperidylcarbamate was synthesized by the reaction of dibenzyltin dichloride with dithiopiperidylcarbamate and was characterized by elemental analysis, IR and 1H NMR. The crystal structure was determined by X ray single crystal diffraction. The crystallographic data are as follows: monoclinic, space group P21, a=0.63464(13)nm, b=1.9110(4)nm, c=0.87367(17)nm, β=97.67(3)°, Z=2, V=1.0501(4)nm3, Dc=1.571g·cm-3, μ=1.546mm-1, F(000)=500, R=0.0209, wR=0.0381 [I ≥2σ(I)]. The str uctures consist of discrete molecules containing five coordinate tin atoms in a seriously distorted trigonal bipyramidal configuration. The molecules are packed in the unit cell in one dimensional chain complex through a weak interaction between the chlorine atom, the sulfur atom and one of the other sulfurs of an adjacent molecule. CCDC: 180034.
Title compounds \[Et 3 N-CH 2 Cl\] + \[COO-Y-COOH\] - (the la tter is pyridine-2,6- dicarboxyl or dithio (bis-2,2′-benzoyloxy) wer e synthesized by reaction of pyridine-2,6-dicarboxylic aicd or dithio(bis-2,2 ′- benzoic aicd) with CH 2 Cl 2 and triethylamine in 1∶1 molar ratio and characterized by elemental analysis, IR and 1 H NMR . Their crystal structures were determined by X-ray single crystal diffractometry, the crystal(Ⅰ) belongs to orthorhombic with a=0 699 43(14) nm, b=1 348 9(3 ) nm, c=1 668 9(3) nm, V= 1 574 5(6) nm 3 , Z=4, D c =1 336 Mg/m 3 , μ=0 259 mm -1 , R 1 =0 033 4, wR 2 =0 080 6, F(000)=672. The crystal(Ⅱ) belongs to triclinic with a=0 788(12) nm, b=1 239(19) nm, c=2 18(3) nm, α= 89 2°, β =89 6°, γ=76 9°, V=2 078(55) nm 3 , Z=4, D c=1 457 Mg/m 3 , μ=0 414 mm -1 , R 1 =0 062 0, wR 2 =0 151 6, F(000)=960.
Three tin ? complexes with N,N- dialkyl dithiocarbamates Ph3SnS2CN(CH3)C6 H5 (1),Ph3SnS2CN(C4H8NH) (2) and Sn(Cl)2(S2CNEt2)2 (3) have been synthesized. Th e crystal structures have been determined by X- ray sin- gle crystal diffraction. A crystal of the complex 1 is triclinic with space group , a=0.9485(3)nm, b=1.0491(3)nm, c=1.3631(4)nm, α =70.996(4)° , β =72.294(4)° , γ =79.609(4)° , Z=2, V=1.2168(6)nm3, Dc=1.453g· cm- 3, μ =1.234mm- 1, R =0.0442, wR=0.0858. A crystal of the complex 2 is monoclinic with space group P2 (1)/c, a=1.2214(2)nm, b=1.1651(2)nm, c=1.5769(3)nm,β =99.039(2)° , Z=2, V=2.21 62(7)nm3, Dc=1.532g· cm- 3, μ =1.352mm- 1, R=0.0267, wR=0.0591. A crystal of the complex 3 is triclinic with space group , a=0.7179(2)nm, b=0.9256(3)nm, c=1 .5327(5)nm,α =93.857(4)° ,β =98.992(4)° , γ =109.481(4)° , Z=2, V=0.9405(5 )nm3, Dc=1.717g· cm- 3, μ =2.076mm- 1, R=0.0263, wR=0.0662. In the complexes 1 and 2 the tin atoms rendered five- coordination in a distorted tigonal bipyr amidal structure and in the complex 3 the tin atom rendered six- coordination i n a distorted octahedron structure. CCDC: 1, 179918; 2, 180024; 3, 180004.
The novel bismuth?complex with dithiotetrahydropyrrolocarbamate, [Bi(S2CNC4H8 )3]2 has been synthesized. The crystal structure has been determined by X-ray s ingle crystal diffraction. The crystal belongs to monoclinic with space group C2 /c, a=1.6356(9) nm, b=1.1875(6) nm, c=2.3954(13) nm, β=100.741(8)°, Z=4, V=4.5 71(4) nm3, Dx=1.882g·cm-3,μ=8.267mm-1, F(000)=2512, R=0.0404, wR=0.0622. In this binuclear complex, each Bi?is seven coordinate with a distorted pentagonal bipyramidal geometry. CCDC: 179924.
gle crystal diffraction. A crystal of the complex 1 is triclinic with space group , a=0.9485(3)nm, b=1.0491(3)nm, c=1.3631(4)nm, α =70.996(4)° , β =72.294(4)° , γ =79.609(4)° , Z=2, V=1.2168(6)nm3, 