Journal
ORGANOMETALLICS
Volume 32, Issue 17, Pages 4973-4984Publisher
AMER CHEMICAL SOC
DOI: 10.1021/om400694z
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- TU Dortmund
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The reactions of the in situ prepared organotin(I) compounds RSnSnR with diary! dichalcogenides ArEEAr provided, depending on the ratio of the reactants, the intramolecularly coordinated heteroleptic organotin(II) chalcogenoarylates RSnEAr (1, R = 2,6-(Me2NCH2)(2)C6H3, -E = S, Ar = Ph; 2, R = 2,6-(Me2NCH2)(2)C6H3, E = Se, Ar = Ph; 3, R = 2,6(Me2NCH2)(2)C6H3, E Te, Ar = Ph; 6, R = 4-t-Bu-2,6-{P(O)(O-i-ET)z}(2)C6H2, E = Se, Ar = Ph; 7, R = 4-t-Bu-2,6-{P(O)(O-i-Pr)(2)}(2)C6H2, E = Te, Ar = Ph; 8, R = 4-t-Bu-2,6-{P(O)(O-i-Pr)(2)}(2)C6H2, E = Se, Ar = 2-C5H4N) and the corresponding organotin(IV) compounds RSn(EAr)(3) (4, R = 2,6-(Me2NCH2)(2)C6H3, E = S, Ar = Ph; 5, R = 2,6-(Me2NCH2)(2)C6H3, E = Se, Ar = Ph; 10, R = 4-t-Bu-2,6-{P(O)(O-i-PO2}(2)C6H2, E = S, Ar = 2-C5H4N), respectively. Compound 1O undergoes a thermally initiated cyclization reaction to give the benzoxaphosphastannole derivative {1(P),3(Sn)-Sn(S-Py)2-OP(O)(O-i-Pr)-6-t-Bu-4-P(O)(Oi-Pr)2}C6H2 (11). The compounds were characterized by H-1, C-13, P-31,Sn-119, and Te-125 NMR and IR spectroscopy, electrospray ionization mass spectrometry, and single-crystal X-ray diffraction analysis. The intramolecular Sn-N and Sn-O distances range between 2.501(3) (2) and 2.815(3) angstrom (4) and between 2.407(2) (8 center dot C7H8) and 2.497(2) angstrom, respectively. Compounds 6 and 7 show intermolecular secondary Sn center dot center dot center dot Sn interactions at distances of 3.8876(3) and 3.8379(5) A, respectively.
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