Synthesis, crystal structure and reactivity of bis(μ-2methylpyridine N-oxide-κ2O:O)bis[dibromido(2-methylpyridine N-oxide-κO)cobalt(II)] butanol monosolvate

被引:0
|
作者
Naether, Christian [1 ]
Jess, Inke [1 ]
机构
[1] Univ Kiel, Inst Anorgan Chem, Kiel, Germany
关键词
crystal structure; synthesis; thermoanalytical investigations; cobalt thiocyanate; 2-methylpyridine N-oxide; N-OXIDE; THERMAL-PROPERTIES; COORDINATION; COMPLEXES; DERIVATIVES; COPPER(2); CHLORIDE;
D O I
10.1107/S2056989023008228
中图分类号
O7 [晶体学];
学科分类号
0702 ; 070205 ; 0703 ; 080501 ;
摘要
Reaction of CoBr2 with 2-methylpyridine N-oxide in n-butanol leads to the formation of the title compound, [CoBr2](2)(2-methylpyridine N-oxide)(4)center dot n-butanol or [Co2Br4(C6H7NO)(4)]center dot C4H10O. The asymmetric unit of the title compound consists of one CoII cation as well as two bromide anions and two 2-methylpyridine N-oxide coligands in general positions and one n-butanol molecule that is disordered around a center of inversion. The Co-II cations are fivefold coordinated by two bromide anions and one terminal as well as two bridging 2-methylpyridine N-oxide and linked by two symmetry-related mu-1,1(O,O) 2-methylpyridine N-oxide coligands into dinuclear units that are located on centers of inversion. In the crystal structure, the dinuclear units are also connected via pairs of C-H...Br hydrogen bonds into chains that elongate in the b-axis direction. The n-butanol molecules are located between the chains and are linked via O-H center dot center dot center dot Br hydrogen bonds each to one chain. Powder X-ray diffraction (PXRD) measurements reveal that a pure phase has been obtained. Measurements using thermogravimetry and differential thermoanalysis shows one mass loss up to 523 K, in which the n-butanol molecules are removed. PXRD measurements of the residue obtained after n-butanol removal shows that a completely different crystalline phase has been obtained and IR investigations indicate significant structural changes in the Co coordination.
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页码:972 / +
页数:10
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