Crystal structure of chlorodiethyl(2-dimethylaminoethanethiolato) tin(IV), (C2H6NCH2CH2S)SnCl(C2H5)2

C8H2oClNSSn, tetragonal, 1A\cd (No. 110), a = 19.300(2) A, c = 14.020(2) A , V= 5222.3 A ,Z = 16, Rgt(F) = 0.034, wR(F) = 0.036, Γ =293 Κ. Source of material Diethyltin(IV)oxide (2.8 mmol) was added to a solution of 2-dimethylaminoethanethiol hydrochlorid (2.8 mmol) in EtOH and the mixture was stirred for 6 h at 333 K. On cooling, colourless crystals of the complex were obtained. Discussion Two carbon atoms and one sulphur atom form the trigonal base of the bipyramidal coordination arrangement around the metal. Distortions from the idealized geometry are mainly observed in bond angles involving the nitrogen atom ZCl-Sn-N = 164.1(2)°, ZS-Sn-N = 80.4(2)°}vhose position is also determined by structural constraints of the bidentate ligand. Bond distances with the equatorial atoms [</(Sn—S) = 2.414(3) A, d{Sn—C) = 2.13(1) A and 2.15(1) A] agree well with the sum of the respective covalent or atomic radii, while these are considerably longer for the apical atoms [d(Sn—CI) = 2.544(2) A, d(Sn-N) = 2.388(7) A], All other structural data are normal [<i(S—C) = 1.83(1) A, i? mean(N—C) = 1.48 A, rfmean(C—C) = 1.48 A], The high displacement parameter of C(2) indicates some disorder in the position of this terminal atom. Hydrogen atoms were introduced in calculated positions with fixed temperature factors (t/iso = 0.08 A). Table 1. Data collection and handling. Crystal: colourless prism, size 0.2 χ 0.15 χ 0.2 mm Wavelength: Mo Ka radiation (0.71073 Ä) μ: 21.1 cm" Diffractometer, scan mode: Philips PW 1100, Θ/2Θ 29max: 56° N(hkl)measured, N(hkl)an\^. 3209, 1609 Criterion for Fobs, N(hkl)gt: Fobs > 3 a(Fobs), 1306 N(param)re fined: 108 Program: SHELX-78 [1] Table 2. Atomic coordinates and displacement parameters (in Ä). Atom Site χ y ζ V\ so H(l l ) 16 b 0.350 0.114 -0.001 0.08 H(12) 16 b 0.318 0.105 0.116 0.08 H(21) 16 b 0.288 0.218 0.056 0.08 H(22) 16 b 0.212 0.169 0.076 0.08 H(23) 16 b 0.244 0.178 -0.040 0.08 H(31) 16 b 0.181 0.024 -0.170 0.08 H(32) 16 b 0.147 0.086 -0.090 0.08 H(41) 16 b 0.061 0.002 -0.133 0.08 H(42) 16 b 0.082 -0.002 -0.011 0.08 H(43) 16 b 0.116 -0.064 -0.091 0.08 H(51) 16 b 0.264 -0.090 -0.166 0.08 H(52) 16 b 0.353 -0.108 -0.182 0.08 H(61) 16 b 0.291 -0.181 -0.066 0.08 H(62) 16 b 0.368 -0.144 -0.023 0.08 H(71) 16 b 0.406 -0.044 -0.008 0.08 H(72) 16 b 0.414 0.042 -0.050 0.08 H(73) 16 b 0.442 -0.028 -0.121 0.08 H(81) 16 b 0.282 0.024 -0.235 0.08 H(82) 16 b 0.372 0.008 -0.248 0.08 H(83) 16 b 0.343 0.078 -0.178 0.08 * Correspondence author (e-mail: graziani@chim02.chin.unipd.it) 286 Chlorodiethyl(2-dimethylaminoethanethiolato)tin(IV) Table 3. Atomic coordinates and displacement parameters (in A). Atom Site X y ζ υ 11 t/22 C/33 Un Un t/23 Sn 16 b 0.24630(2) 0.01964(2) 0" 0.0448(2) 0.0570(3) 0.0426(3) -0.0004(2) 0.0021(2) 0.0003(5) CI 16 b 0.1690(1) 0.0294(1) 0.1464(2) 0.057(1) 0.092(2) 0.046(1) 0.012(1) 0.015(1) 0.002(1) S 16 b 0.2655(1) -0.0979(1) 0.0525(2) 0.080(1) 0.066(1) 0.066(1) 0.007(1) 0.016(1) 0.018(1) Ν 16 b 0.3330(3) -0.0146(4) -0.1120(6) 0.054(4) 0.066(4) 0.056(4) -0.005(3) 0.006(3) -0.012(3) C(l) 16 b 0.3043(5) 0.1101(6) 0.0419(8) 0.077(6) 0.089(7) 0.079(6) -0.026(5) 0.013(5) -0.027(6) C(2) 16 b 0.2585(8) 0.1720(7) 0.037(2) 0.14(1) 0.09(1) 0.26(3) -0.020(8) 0.03(1) -0.07(1) C(3) 16b 0.1632(5) 0.0339(5) -0.0982(8) 0.056(5) 0.085(6) 0.057(5) 0.004(4) -0.001(4) 0.007(5) C(4) 16 b 0.1028(5) -0.0094(7) -0.0834(9) 0.075(6) 0.104(8) 0.096(8) -0.012(6) -0.026(6) -0.003(7) C(5) 16 b 0.3148(5) -0.0884(4) -0.1326(7) 0.080(6) 0.059(5) 0.063(6) 0.000(4) 0.013(5) -0.010(4) C(6) 16 b 0.3165(5) -0.1330(4) -0.0468(8) 0.081(6) 0.060(5) 0.081(6) 0.009(5) 0.017(5) -0.004(5) C(7) 16 b 0.4035(4) -0.0116(5) -0.0700(8) 0.047(4) 0.081(6) 0.990(8) 0.002(4) 0.002(5) -0.006(6) C(8) 16 b 0.3320(5) 0.0252(4) -0.2004(8) 0.072(5) 0.066(5) 0.071(6) 0.005(4) 0.031(5) 0.015(5) a: arbitrarily fixed for definition of the origin.