Synthesis and Crystal Structure of 4,5-Diazafluorene-9-one Azine Hydrochloride Hydrate

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Crystals of the title compound C22H12N62HCl?H2O (DAA稨Cl) were obtained from a HCl aqueous solution of 4, 5-diazafluorene-9-one azine. The crystal belongs to monoclinic, space group P21/c with a = 5.203(3), b = 8.991(3), c = 22.17(1) , b = 92.13(4), V = 1036.2(9) 3, Z = 2, C22H18N6O2Cl2, Mr = 468.1, Dc = 1.503 g/cm3, F(000) = 484, m(MoKa) = 0.344 mm-1, R = 0.052 and wR = 0.056 for 755 observed reflections. The Cl…N(2) distance of 2.999(6) ?and Cl…HN(2) angle of 160.8(8)o imply the existence of a stronger H-bond between Cl and DAA. And both the rather longer ClH distance of 1.814(2) ?and the unexpected shorter N(2)H distance of 1.236(6) ?suggest the protonation of DAA molecule and explain the weak coordination ability of DAA to a metal center in the acidic solution. Crystals of the title compound C22H12N62HCl? H2O (DAA Cl) were obtained from a HCl aqueous solution of 4, 5-diazafluorene-9-one azine. The crystal belongs to monoclinic, space group P21 / c with a = 5.203 , b = 8.991 (3) c = 22.17 (1) b = 92.13 (4) V = 1036.2 (9) 3 Z = 2 C22H18N6O2Cl2 Mr = 468.1 Dc = 1.503 g / cm3 F ) = 484, m (MoKa) = 0.344 mm -1, R = 0.052 and wR = 0.056 for 755 observed reflections. The Cl ... N (2) distance of 2.999 (6)? And Cl ... HN (2) angle of 160.8 (8) o imply the existence of a stronger H-bond between Cl and DAA. And both of them rather longer ClH distance of 1.814 (2)? And the unexpected shorter N (2) H distance of 1.236 (6)? Suggest the protonation of DAA molecule and explain the weak coordination ability of DAA to a metal center in the acidic solution.
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