Synthesis and Crystal Structure of (C_6N_3H_(18))_2Ti_4O_4(C_2O_4)_7·4H_2O

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The title compound (C6N3H18)2Ti4O4(C2O4)74H2O 1 (C13H22N3O18Ti2, Mr = 604.14) was synthesized by the reaction of Ti(SO4)2, H2C2O42H2O and N-(2-ammonioethyl)- piperazinium (AEPP) in aqueous solution. The single-crystal X-ray analysis has revealed that 1 crystallizes in the triclinic system, space group Pi with a = 9.1437(6), b = 11.4991(10), c = 11.6975(8) ? a = 96.2915(18), ?= 107.998(3), ? = 104.276(4), V = 1110.35(14) ?, Z = 2, Dc = 1.807 g/cm3, F(000) = 618, ?= 0.815 mm-1, the final R = 0.0463 and wR = 0.1264 for 3718 observed reflections with I > 2s(I). X-ray crystal-structure analysis suggests that compound 1 consists of [Ti4O4(C2O4)7]6- anion and two protonated N-(2-ammonioethyl)piperazinium cations. The anions are linked into an infinite chain through Ti4O4(C2O4)8 by sharing the oxalates as bridging ligands. The title compound (C6N3H18) 2Ti4O4 (C2O4) 74H2O 1 (C13H22N3O18Ti2, Mr = 604.14) was synthesized by the reaction of Ti (SO4) 2, H2C2O42H2O and N- (2- ammonioethyl) - piperazinium (AEPP) single-crystal X-ray analysis has revealed that 1 crystallizes in the triclinic system, space group Pi with a = 9.1437 (6), b = 11.4991 (10), c = 11.6975 (8)? a = 96.2915 (18) = 107.998 (3),? = 104.276 (4), V = 1110.35 (14) ?, Z = 2, Dc = 1.807 g / cm3, F (000) = 618,? = 0.815 mm-1, 0.0463 and wR = 0.1264 for 3718 observed reflections with I> 2s (I). X-ray crystal-structure analysis suggests that compound 1 consists of [Ti4O4 (C2O4) 7] 6-anion and two protonated N- piperazinium cations. The anions are linked into an infinite chain through Ti4O4 (C2O4) 8 by sharing the oxalates as bridging ligands.
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