U. Bemm et al., SYNTHESIS AND STRUCTURAL INVESTIGATION OF A NEW MANGANESE-ANTIMONY OXOETHOXIDE, (2)(MU(4)-O)(2)(MU(3)-OET)(2)(MU-OET)(16)(HOET)(2), Journal of solid state chemistry, 134(2), 1997, pp. 312-318
A new manganese-antimony oxoethoxide with the formula Mn7Sb4O4(OEt)(18
)(HOEt)(2) has been prepared and characterized by single-crystal X-ray
diffraction and FT-IR techniques, The structure of the compound has t
he noncentrosymmetric tetragonal space group symmetry P4(2) (No. 77) w
ith unit-cell parameters a = 15.164(3), c = 14.729(5) Angstrom, V = 33
87(2) Angstrom(3), Z = 2, and D-x = 1.803(1) g cm(-1) F-w = 1838.8 g m
ol(-1), The crystal structure has been refined against the 2227 most s
ignificant reflections to an R value of 0.059 (R-w = 0.077), The singl
e-crystal X-ray diffraction intensities were collected at 170(1)K usin
g MoK alpha radiation. The structure analysis shows that the structure
consists of roughly spherically shaped molecules of C-2 symmetry and
of composition Mn7Sb4O4(OEt)(18)(HOEt)(2). The antimony atoms are five
-coordinated by oxygen atoms, while four of the manganese atoms are fi
ve-coordinated and three are six-coordinated. The antimony atoms are l
ocated in the outer regions of the molecule and the antimony lone pair
regions are pointing away from the molecule, Four oxooxygens are loca
ted in the core of the molecule, The ethanol molecules coordinating th
e antimony atoms are involved in short intramolecular hydrogen bonds,
A TLS analysis of the rigid-body motion of the central metal-oxygen co
re structure shows that two oxygen atoms involved in the intramolecula
r hydrogen bond do not follow the pattern of the rest of the atoms. Th
e agreement between observed and predicted parameters of the remaining
atoms supports the assumed rigidity in the central metal and oxygen c
ore fragment. Structural relationships are found to other spherically
shaped alkoxides such as Mn8Sb4O4(OEt)(20) and Pb6Nb4O4(OEt)(24). (C)
1997 Academic Press.