Crystal Structures and Raman Spectra of cis‐[SnCl₄(H₂O)₂]·2H₂O, cis‐[SnCl₄(H₂O)₂]·3H₂O, [Sn₂Cl₆(OH)₂(H₂O)₂]·4H₂O, and [HL][SnCl₅(H₂O)]·2.5H₂O (L=3‐acetyl‐5‐benzyl‐1‐phenyl‐4, 5‐dihydro‐1, 2, 4‐triazine‐6‐one oxime, C₁₈H₁₈N₄O₂)

Abstract

The complexes cis-[SnCl 4 (H 2 O) 2 ]·2H 2 O (1), [Sn 2 Cl 6 (OH) 2 (H 2 O) 2 ]·4H 2 O (3), and [HL][SnCl 5 (H 2 O)]·2.5H 2 O (4) were isolated from a CH 2 Cl 2 solution of equimolar amounts of SnCl 4 and the ligand L (Lϭ3-acetyl-5-benzyl-1-phenyl-4,5-dihydro-1,2,4-triazine-6-one oxime,C 18 H 18 N 4 O 2 ) in the presence of moisture. 1 crystallizes in the monoclinic space group Cc with a ϭ 2402.5(1) pm, b ϭ 672.80(4) pm, c ϭ 1162.93(6) pm, β ϭ 93.787(6)°and Z ϭ 8. 4 was found to crystallize monoclinic in the space group P2 1 , with lattice parameters a ϭ 967.38 (5) pm, b ϭ 841 1101.03(6) pm, c ϭ 1258.11(6) pm, β ϭ 98.826(6)°and Z ϭ 2. The cell data for the reinvestigated structures are: [SnCl 4 (H 2 O) 2 ]·3H 2 O (2): a ϭ 1227.0(2) pm, b ϭ 994.8(1) pm, c ϭ 864.0(1) pm, β ϭ 103.86(1)°, with space group C2/c and Z ϭ 4; 3: a ϭ 961.54(16) pm, b ϭ 646.29(7) pm, c ϭ 1248.25(20) pm, β ϭ 92.75(1)°, space group P2 1 /c and Z ϭ 4. Liganden L (Lϭ 3-acetyl-5-benzyl-1-phenyl-4,5,dihydro-1,2,4-triazin-6-on oxim, C 18 H 18 N 4 O 2 ) in CH 2 Cl 2 in Gegenwart von Wasser isoliert. (Kristallstrukturdaten s. Abstract).

Triclinic form of bis{di-μ-hydroxidobis[fac-aquatribromidotin(IV)]} heptahydrate

“…One of the [Br 3 (H 2 O)Sn(µ-OH) 2 SnBr 3 (OH 2 )] molecules occupies a general position, Table 1. The observed trends for the dinuclear species match those found in the monoclinic polymorph (Howie et al, 2005) and other related di-µ-hydroxo-bis[fac-trichloroaquotin(IV)] complexes (Barnes et al, 1980;Cameron et al, 1985;Shihada et al, 2004;Müller et al, 2007).…”

“…For the structure of the monoclinic polymorph, see: Howie et al (2005). For related di--hydroxido-bis[fac-trichloridoaquatin(IV)] complexes, see: Barnes et al (1980); Cameron et al (1985); Shihada et al (2004); Mü ller et al (2007). For analysis of pseudo-symmetry, see: Spek (2003).…”

Crystal structure of tin(IV) chloride octahydrate

“…For the existing hydrates (R = 8, 5, 4, 3 and 2), Meyerhoffer (1891) described the melting points and the existence fields. The crystal structures of the dihydrate (Semenov et al, 2005), trihydrate (Genge et al, 2004;Semenov et al, 2005), tetrahydrate (Genge et al, 2004;Shihada et al, 2004) and pentahydrate (Barnes et al, 1980;Shihada et al, 2004) have been determined previously. For these salt hydrates, vibrational spectra are also available, classifying all hydrate spectra with point group D 4h symmetry (Brune & Zeil, 1962).…”

Diaquatetrabromidotin(IV) trihydrate

“…For background information on hydrates of SnBr 4 , see: Pfeiffer (1914); Pickering (1895); Rayman & Preis (1884). For the isostructural compound [SnCl 4 (H 2 O) 2 ]Á3H 2 O, see: Shihada et al (2004). For structural information on other hydrates of SnCl 4 , see: Semenov et al (2005); Genge et al (2004).…”

“…In contrast to tin(IV) chloride, SnCl 4 , from which the crystal structures of hydrates, SnCl 4 . nH 2 O, with n = 2 (Semenov et al, 2005), n = 3 (Genge et al, 2004;Semenov et al, 2005), n = 4 (Genge et al, 2004;Shihada et al, 2004), and n = 5 (Shihada et al, 2004) are known in detail, no structural data are available concerning the hydrates of tin(IV) bromide, SnBr 4 . nH 2 O, although there are some hints in the older literature that a tetrahydrate, n = 4, (Rayman & Preis, 1884;Pfeiffer, 1914) and octahydrate, n = 8, (Pickering, 1895) exist.…”