Bis(butane-1,4-diammonium) di-µ-oxido-bis[trifluoridooxidomolybdate(V)] monohydrate.

The title compound, (C4H14N2)2[Mo2O4F6]·H2O, was obtained by solvothermal reaction at 443 K for 72 h from a mixture of MoO3, HF, 1,4-diamino-butane (dab), water and ethyl-ene glycol. The structure consists of [Mo2O4F6](4-) anionic dimers containing strongly distorted MoO3F3 octa-hedra (with twofold symmetry), diprotonated dab cations and water mol-ecules (twofold symmetry) in the ratio 1:2:1. The cohesion of the three-dimensional structure is ensured through N-H⋯O, N-H⋯F and O-H⋯F inter-actions.

A new organic-inorganic hybrid oxyfluorotitanate [Hgua]2·(Ti5O5F12) as a transparent UV filter.

A new generation UV absorber is obtained by microwave-heating-assisted hydrothermal synthesis: [Hgua](2)·(Ti(5)O(5)F(12)). The structure of this hybrid titanium(IV) oxyfluoride is ab initio determined from powder X-ray data by combining a direct space method, Rietveld refinement [orthorhombic, Cmm2, a = 22.410(1) Å, b = 11.191(1) Å, c = 3.802(1) Å], and density functional theory geometry optimization. The three-dimensional network is built up from infinite inorganic layers (∞)(Ti(5)O(5)F(12)) separated by guanidinium cations. The theoretical optical gap (3.2 eV) estimated from density of state calculations is in good agreement with the experimental gap (3.3 eV) obtained by UV-vis diffuse reflectivity. The optical absorption is mainly due to O(2p) → Ti(3d) and F(2p) → Ti(3d) transitions at higher energies. The refraction index is low in the visible range (n ≈ 1.9) compared to that of TiO(2) and, consequently, [Hgua](2)·(Ti(5)O(5)F(12)) shows a good transparency adapted to UV shielding. Under UV irradiation at 254 nm for 40 h, the white microcrystalline powder turns to light purple-gray. This color change is caused by the reduction of Ti(IV) to Ti(III), confirmed by magnetic measurements.

New pillared layered gallium phosphonates in the gallium/1,2-ethylenediphosphonic acid system.

1,2-Ethylenediphosphonic acid reacts with gallium nitrate in water to give new pillared layered gallium phosphonates, the structure of which depends on the experimental conditions used for their preparation. Thus, Ga(4)(O(3)PC(2)H(4)PO(3))(3) (1) and Ga(2)(OH)(2)(O(3)PC(2)H(4)PO(3)) (2) were isolated and the structure of 1 was solved by single-crystal X-ray diffraction, while 2 was shown to have the same metal/PO(3) arrangement as the previously described Ga(OH)(O(3)PCH(3)). Ga(4)(O(3)PC(2)H(4)PO(3))(3) (1) is triclinic, with space group P1 with Z = 2, a = 5.1480(4), b = 8.0354(7), and c = 12.383(1) A; alpha = 91.34(1), beta = 101.40(1), and gamma = 90.86(1) degrees; V = 501.9(1) A(3). The structure of 1 is unusual with (i) mixed GaO(4) and GaO(5) sites while a 6-fold coordination is observed for gallium in (2) and (ii) the presence of the organic moiety within both the layers and the interlayer space. The two compounds were fully characterized using (31)P and (71)Ga solid-state NMR.