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A series of six new single crystals of  fully stoichiometric  As 3+ -bearing Mo-oxides and partially W-substituted Mo-oxides with formula As  m  O(Mo 1−   x  W  x  O 3 )  p   ( m  = 1, 2;  p  = 5, 7, 9, 10 and 11 and 0 ≤  x  ≤ 0.6) was successfully grown using vapor-phase transport  in vacuo . The crystal structures were determined using single-crystal X-ray diffraction data. All these compounds exhibit acentric orthorhombic symmetry with  Z  = 2, and belong to the so-called ( n )-ITB (intergrowth tungsten bronzes) family, with  n  = 2, 3, 4 and 5. The six ( n )-ITB phases have the following formulae: (2)-AsMo 5 O 16  ( Pm  2 a ), (2)-As 2 Mo 10 O 31  ( Pma  2), (3)-AsMo 7 O 22  ( Pmn  2 1 ), (3)-As(Mo 5.53 W 1.47 )O 22  ( Pmn  2 1 ), (4)-As(Mo 4.33 W 4.67 )O 28  ( Pm  2 a ) and (5)-As(W 6.63 Mo 4.37 )O 34  ( Pmn  2 1 ). Their structures consist of vertex-sharing MO 6  octahedral units (with M either Mo or Mo/W) connected so as to form three-dimensional frameworks. Such frameworks consist of perovskite tungsten bronzes (PTB) type slabs, from 2- to 5-octahedra wide, intergrown with single hexagonal tungsten bronzes (HTB) type slabs, stacked up to form pseudo-hexagonal tunnels along the  a -axis. As 3+  and additional oxygen atoms are located in off-center positions inside the tunnels, forming As–O bonds with peculiar arrangements. In particular, we obtained the first examples of structures where, besides the usual AsO 3 E distorted pyramidal geometry, As 3+  adopts AsO 4 E coordination with a  seesaw  configuration.

Synthesis and crystal structure of a series of stoichiometric ( n )-ITB molybdenum-bronze oxides containing trivalent arsenic