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The crystal and molecular structures of R 2 Sn(O 2 CR 1 )Cl: R = Me, t Bu and Ph; − O 2 CR 1 = o -(2-hydroxy-5-methylphenylazo)benzoate

1998; De Gruyter; Volume: 213; Issue: 1 Linguagem: Inglês

10.1524/zkri.1998.213.1.62

2196-7105

Tushar S. Basu Baul, Edward R. T. Tiekink,

Crystal Structures and Properties

Abstract The crystal and molecular structures of three R 2 Sn(O 2 CR 1 )Cl compounds [R = Me, t Bu and Ph; − O 2 CR 1 = o -(2-hydroxy-5-methylphenylazo)benzoate] have been determined at room temperature. Brown crystals of Me 2 Sn(O 2 CR 1 )Cl ( 1 ), C 16 H 17 ClN 2 O 3 Sn, are triclinic, space group P [unk] with unit cell dimensions a = 10.649(4) Å, b = 12.292(3) Å, c = 7.236(2) Å, α = 96.68(3)°, β = 104.03(3)°, γ = 109.12(3)°, Z = 2 and D x = 1.662 Mg m −3 . Red crystals of t Bu 2 Sn(O 2 CR 1 )Cl ( 2 ), C 22 H 29 ClN 2 O 3 Sn, are monoclinic space group P 2 1 / n with unit cell dimensions a = 8.323(5) Å, b = 24.990(5) Å, c = 12.403(5) Å, β = 107.94(3)°, Z = 4 and D x = 1.417 Mg m −3 . Red crystals of Ph 2 Sn(O 2 CR 1 )Cl ( 3 ), C 26 H 21 ClN 2 O 3 Sn, are also monoclinic with space group P 2 1 / c and unit cell dimensions a = 14.416(3) Å, b = 16.373(6) Å, c = 10.489(4) Å, β = 97.10(3)°, Z = 4 and D x = 1.524 Mg m −3 The structures were solved by Patterson ( 1 and 2 ) or direct methods ( 3 ) and each refined by a full-matrix least-squares procedure to final R = 0.039 using 2933 reflections for 1 , R = 0.039 for 2935 reflections for 2 , and R = 0.037 using 2863 reflections for 3 . The structure of 1 is dimeric with the two tin atoms being bridged by two − O 2 CR 1 anions each of which coordinates a tin atom via one of the carboxylate oxygen atom and the second tin atom via the phenoxide oxygen atom; this result indicates that the − O 2 CR 1 anion exists as a Zwitterion. The tin atom geometry is trigonal bipyramidal. trans -O 2 SnC 2 Cl. By contrast to the dimeric structure for 1 , the structures of 2 and 3 are monomeric with the tin atoms in cis -O 2 SnC 2 Cl trigonal bipyramidal geometries. The − O 2 CR 1 anion coordinates the tin atom in each of 2 and 3 via the carboxylate oxygen atoms only.