As reações do ligante 2,6-diacetilpiridina bis(4-feniltiossemicarbazona), H2dappt, com R4-mSnXm (m = 2, 3; R = Me, nBu, Ph e X = Cl) resultaram na formação de quatro novos complexos organoestânicos heptacoordenados, os quais foram caracterizados por análise elementar e pelas espectroscopias no IV e Mössbauer. O derivado n-butila, [nBu2Sn(dappt)]·(Me 2CO)0.5, foi também analisado por um estudo de difração de raios X em um monocristal. O complexo cristalizou-se no sistema monoclínico e grupo espacial C2/c, com a = 36,164(14), b = 9,7050(15), c = 26,194(11) Å, beta = 132,00(2)º, Z = 8. A determinação da estrutura revelou um complexo neutro de Sn(IV), numa geometria bipiramidal pentagonal (BPP), com o plano equatoral definido pelos átomos doadores SNNNS do ligante e dois grupos n-bultila nas posições axiais. Também é discutida uma correlação entre os dados de Mössbauer e de difração de raios X, baseada no modelo da carga-pontual.The reactions of the 2,6-diacetylpyridine bis(4-phenylthiosemicarbazone) ligand, H2dappt, with R4-mSnXm (m = 2, 3; R = Me, nBu, Ph and X = Cl) led to the formation of four new heptacoordinated organotin(IV) complexes, which were characterized by microanalyses and by IR and Mössbauer spectroscopies. The n-butyl derivative [nBu2Sn(dappt)]·(Me 2CO)0.5 was also analyzed by a single crystal X-ray diffraction study. It crystallized in the monoclinic system with a space group C2/c, with a = 36.164(14), b = 9.7050(15), c = 26.194(11) Å, beta = 132.00(2)º, Z = 8. The structure determination revealed a neutral complex of Sn(IV) in a distorted pentagonal bipyramidal (PBP) geometry, with the equatorial plane defined by the SNNNS donor system of the ligand and with the two n-butyl groups in the axial positions. Also, a correlation between Mössbauer and X-ray data based on the point-charge model is discussed.The reactions of the 2,6-diacetylpyridine bis(4-phenylthiosemicarbazone) ligand, H2dappt, with R4-mSnXm (m = 2, 3; R = Me, nBu, Ph and X = Cl) led to the formation of four new heptacoordinated organotin(IV) complexes, which were characterized by microanalyses and by IR and Mössbauer spectroscopies. The n-butyl derivative [nBu2Sn(dappt)]·(Me 2CO)0.5 was also analyzed by a single crystal X-ray diffraction study. It crystallized in the monoclinic system with a space group C2/c, with a = 36.164(14), b = 9.7050(15), c = 26.194(11) Å, beta = 132.00(2)º, Z = 8. The structure determination revealed a neutral complex of Sn(IV) in a distorted pentagonal bipyramidal (PBP) geometry, with the equatorial plane defined by the SNNNS donor system of the ligand and with the two n-butyl groups in the axial positions. Also, a correlation between Mössbauer and X-ray data based on the point-charge model is discussed