The first organoelement oxides containing three different metals; synthesis and structure of (Ph2SiOR2SnOMO) [R = (CH2)3NMe2; M = But2Sn, But2Ge, PhB]† ‡

The First Well-Defined Tellurastannoxanes: the X-ray Structure oftrans-[(Bu3SnO)2{CH2(Ph2SnO)2}2Te]

“…The reaction between Te(OH) 6 and three equivalents of Bu 3 SnOMe quantitatively produced mer-[(Bu 3 SnO) 3 Te-(OH) 3 ] (1) [Equation (1)]: (1) Compound 1 was obtained as a colorless, odorless lowmelting waxy material that slowly crystallized over several weeks. The 119 Sn NMR spectrum (CDCl 3 ) of 1 reveals two signals at δ ϭ 81.…”

“…The reason for selective formation of the mer-isomer under these reaction conditions is still not understood. Reactions of Te(OH) 6 with Bu 3 SnOMe in stoichiometric ratios other than 1:3 provided mixtures of products with a varying degree of substitution, [(Bu 3 SnO) n Te(OH) nϪ6 ] (n Ն 3). [13] The identity of these species was unambiguously proven by 119 Sn and 125 Te NMR spectroscopy, although all attempts to isolate pure compounds from the mixtures failed.…”

“…[13] The identity of these species was unambiguously proven by 119 Sn and 125 Te NMR spectroscopy, although all attempts to isolate pure compounds from the mixtures failed. Moreover, reactions between Te(OH) 6 and other triorganotin methoxides, R 3 SnOMe (R ϭ Me, cHex, Ph), also provided mixtures of products that could not be purified. [14] The reaction of mer-[(Bu 3 SnO) 3 Te(OH) 3 ] (1) with two equivalents of (Ph 2 SnOH) 2 CH 2 [15] gave, with elimination of water and one equivalent of tributyltin hydroxide (Bu 3 SnOH), the spirocyclic tellurastannoxane derivative trans-[(Bu 3 SnO) 2 {CH 2 (Ph 2 SnO) 2 } 2 Te] (2) in good yields [Equation (2)].…”

“…The mean TeϪO bond length amounts to 1.912(3) Å , which is close to the bond length found in [(Me 2 Si-O) 2 ] 3 Te. [4] The central mononuclear TeO 6 (1)ϪO (1)ϪSn (2)Ϫ (3) Te (1)ϪO (2) 1.907 (3) Te (1)ϪO (1) Te (1)ϪO (3) 1.914 (3) Sn (1)ϪO (2) 1.986(3) Sn(1)ϪO(3a) 2.944 (3) Sn (1)ϪC (1) 2.123(5) Sn (1)ϪC (11) 2.137 (6) Sn (1)ϪC (21) 2.128(5) Sn (2)ϪO (1) 1.982 (3) Sn (2)ϪO(3a) 3.003(3) Sn (2)ϪC (1) 2.128 (5) Sn (2)ϪC(31) 2.117(5) Sn (2)ϪC (41) 2.137 (5) Sn (3)ϪO (1) 3.518(3) Sn (3)ϪO (2) 3.398 (3) Sn (3)ϪO (3) 2.015(3) Sn (3)ϪC (51) 2.124 (6) Sn (3)ϪC (61) 2.124(6) Sn (3)ϪC (71) 2.106 (7) O (1)ϪTe (1)ϪO (2) 89.68 (13) O (1)ϪTe ...…”

“…Although the synthesis of the first alkyl ester of orthotelluric acid, Te(OH) 6 , was described early last century there have been only a few subsequent reports utilizing the acidic protons in Te(OH) 6 to build new organometallic complexes. [3] In one case molecular tellurasiloxanes, namely [(Me 2 SiO) 2 ] 3 Te (I), and (Me 3 SiO) 8 Te 2 O 2 (II) [4] were described and in another case a unique mixed-valence Te IV -Te VI species {OTe(C 8 H 8 )[(EtO) 2 PS 2 ]} 6 Te (III) was reported.…”