Abstract: | Hydrothermal reactions of NaN3, 1, 10‐phenanthroline or 2, 2′‐bipyridine and transition metal cations including ZnII or CoII in basified aqueous solutions yielded the three complexes, [Zn2(bipy)2(N3)4]n ( 1 ), [Zn(phen)(N3)2]n ( 2 ), and [Co(phen)2(N3)2] ( 3 ), which were characterized by X‐ray crystallography. All three complexes crystallize in the triclinic system, space group P1¯, with a = 6.5506(2), b = 10.8441(6), c = 16.893(2)Å, α = 96.333(5), β = 95.361(7), γ = 90.548(6)° for 1 ; a = 7.0302(10), b = 10.0590(14), c = 10.4550(15)Å, α = 109.372(2), β = 103.980(2), γ = 106.137(2)° for 2 ; and a = 8.1722(2), b = 11.0332(3), c = 12.5066(2)Å, α = 82.681(8), β = 82.457(9), γ = 72.991(7)° for 3 , respectively. The photoluminescence spectra for compounds 1 and 2 have also been studied. |