Synthesis and structure of tricymantrenyltin chloride

Interaction of dicymantrenyltin dichloride or tin chloride with cymantenyllithium in tetrahydrofuran at -78°С leads to formation of tricymantrenyltin [(CO)3MnС5H4]3SnCl (1), yielding 92 % and 96 %, respectively. 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 1920 and 2016 cm-1. According to the X-ray analysis data of 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 = 7,087(5) Å, b = 17,841(15) Å, c = 21,180(16) Å, a = g = 90,00, β = 95,91(3) degrees, V = 2664(4) Å3, Z = 4, r(sub.)=1,903 g/cm3, F (000) 1480.0, the crystal size is 0.68´0.55´0.03 mm; q range of data collection 5.78-55.14 degrees, range of refraction indices 9 ≤ h ≤ 9, -23 ≤ k ≤ 23, -27 ≤ l ≤ 27; total reflections 111198; independent reflections 6108; refinement variables 343; GOOF 1.097; R1 = 0,0312; wR2 = 0,0722; residual electron density 0.52/-0.63 e/Å3. The tin atoms in 1 have a distorted tetrahedral coordination; the CSnC angles are 104.68(10)°-106.79(10)°, the Sn-C bond lengths change within the range 2.108(3)-2.116(4) Å, the Sn-Cl distance is 2.3503(16) Å. The structural organization of the complex 1 crystal is controlled by intermolecular bonds H×××O (2.57, 2.59 Å), С×××O (3.157 Å) и Sn(1)×××O(9) (3.193 Å).