Synthesis and Structure of Tricymantrenyltin Oxide
Abstract
Interaction of tricymantrenyltin chloride with sodium hydroxide in an acetone-water solution leads to formation of tricymantrenyltin oxide {[(CO)3MnС5H4]3Sn}2O (1), yielding 72 %. The structure of the obtained compound has been investigated by IR spectroscopy and X-ray diffraction analysis. The IR spectrum of complex 1 contains the characteristic absorption bands related to stretching vibrations of carbonyl groups at 1921 and 2019 cm–1. According to the X-ray analysis data, obtained on an automatic diffractometer D8 Quest Bruker (MoKa-radiation,
λ = 0.71073 Å, graphite monochromator) at 293 K, compound 1 is crystallized in a monoclinic crystal lattice, the spatial group is P21/c. Cell parameters: a = 12.651(6) Å, b = 35.000(16) Å,
c = 12.297(7) Å, a = g = 90.00, β = 113.44(3) degrees, V = 5251(4) Å3, Z = 4, r(sub.)= 1.861 g/cm3, F(000) = 2856.0, the crystal size is 0.69´0.53´0.33 mm; the 2q range of data collection
is 5.78–54.4 degrees, the ranges of refraction indices are -16 ≤ h ≤ 16, -44 ≤ k ≤ 44, -16 ≤ l ≤ 16; total reflections 50910; independent reflections 11625; refinement variables 676; GOOF 1.122; R1 = 0.0596; wR2 = 0.1321; the residual electron density equals 4.29/-2.57 e/Å3. The tin atoms in 1 have a distorted tetrahedral coordination; the CSnC angles are 102.3(2)°-120.1(2)°,
the Sn–C bond lengths change within the range 2.107(6)-2.119(7) Å, the Sn–O distances are 1.945(4) and 1.959(4) Å. The structural organization of the complex 1 crystal is controlled by intermolecular bonds С–H×××O≡С (2.57-2.71 Å).
