C 4 H 9 Br 2 NO 2 Pb 2 ,triclinic, P 1 (no. 2), a =9.281(2) Å, b =9.311(2) Å, c =13.085(3) Å, a =86.72(9)°, b =69.71(8)°, g =81.48(9)°, V =1048.8
Source of materialLead(II)bromide (0.2 g, Chempur 99 %) and 2,2¢ -iminodiethanol (1 mL,diethanolamine, Chempur, m.p. 300-303 K)were mixed together and filled in aglass ampule (Duran, interior diameter 10 mm, length 80 mm) which wasevacuated and sealed. Following heattreatment wasperformed in anelectric resistanceoven (453 K). After two weeks the ampule wast aken out, rapidly cooled down to room temperature and the solid wass eparated from the liquid phase. The solids contained severalcolorless crystals of the title compound and microcrystalline PbBr 2 .
DiscussionDiethanolamine wasacandidate of our solvent screeningtofind water-like organic solvents for the solvothermals yntheses of ternary inorganic leadc ompounds. Wealready described the successful syntheses of CuPb 3 Br 7 in diethylene glycol [1]. The crystalstructure of the title compound shows deprotonated alcohol groups. This indicatesthatdiethanolamine is aninappropriate solvent for the planned syntheses route. Wealready have observed elsewhere the deprotonation of alcohol groups of diethylene glycol using inorganic oxides asreactants [2]. This behavior wasn ot detected when solely PbBr 2 wasu sed asr eactant with polyethylene glycol assolvent. The atomic arrangement in dilead(II)-(2,2¢ -iminodiethanolate) dibromide canbedescribed asahighly distorted layer structure of leadand bromine. Two crystallographically different diethanolamine-leadgroups are embedded in these layers. The geometry of the oxygen and leadatoms of these partialstructures are congruent to the structure motive of the orthorhombic modification of lead(II)oxide (massicot). Inthe top left corner of the figure asin-Z.Kristallogr