The crystal structure of guanidinium hexamolybdobis(phenylarsonate) tetrahydrate, (CN3H6)4[C6H5As)2Mo6O25H2] 4H2O.
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Two heteropoly anions, [C<SUB>6</SUB>H<SUB>5</SUB>AsMo<SUB>6</SUB>O<SUB>21</SUB>(H<SUB>2</SUB>O)<SUB>6</SUB>]<SUP>2－</SUP> and [(C<SUB>6</SUB>H<SUB>5</SUB>As)<SUB>2</SUB>Mo<SUB>6</SUB>O<SUB>25</SUB>H<SUB>2</SUB>]<SUP>4－</SUP>, have been synthesized by the reaction of phenylarsonic acid with molybden um trioxide in an aqueous solution of pH <I>ca.</I> 2. The latter anion has been subjected to crystal-structure analysis as a guanidinium salt, (CN<SUB>3</SUB>H<SUB>6</SUB>)<SUB>4</SUB>[(C<SUB>6</SUB>H<SUB>5</SUB>As)<SUB>2</SUB>Mo<SUB>6</SUB>O<SUB>25</SUB>H<SUB>2</SUB>]·4H<SUB>2</SUB>O, and a heteropoly anion with a new type of structure has been established. The crystal is monoclinic with the space group of P2<SUB>1</SUB> and cell dimensions of <I>a</I>=13.754(5), <I>b</I>=15.752(7), <I>c</I>=11.900(5) Å, β=115.59(2)°, <I>V</I>=2325.3 Å<SUP>3</SUP>, <I>D</I><SUB>m</SUB>=2.25, <I>D</I><SUB>x=</SUB>2.28 g cm<SUP>－3</SUP>, and <I>Z</I>=2. The formula of the anion has been proved to be [(C<SUB>6</SUB>H<SUB>5</SUB>As)<SUB>2</SUB>Mo<SUB>6</SUB>O<SUB>25</SUB>H<SUB>2</SUB>]<SUP>4－</SUP>, which is different from the expected formula, [(C<SUB>6</SUB>H<SUB>5</SUB>As)<SUB>2</SUB>Mo<SUB>6</SUB>O<SUB>24</SUB>]<SUP>4－</SUP>, though the latter had previously been proposed on the basis of a <SUP>17</SUP>O NMR study and an independent X-ray investigation of the methyl derivative had confirmed the existence of the [(CH<SUB>3</SUB>As)<SUB>2</SUB>Mo<SUB>6</SUB>O<SUB>24</SUB>]<SUP>4－</SUP> anion. The present anion, [(C<SUB>6</SUB>H<SUB>5</SUB>As)<SUB>2</SUB>Mo<SUB>6</SUB>O<SUB>25</SUB>H<SUB>2</SUB>]<SUP>4－</SUP>, consists of six MoO<SUB>6</SUB> octahedra, which form a ring with one face-, two corner- and three edge-sharings, the two C<SUB>6</SUB>H<SUB>5</SUB>AsO<SUB>3</SUB> tetrahedra are attached to the ring from above and below, with their three oxygens shared with molybdenums. The two phenyl groups are oriented upwards and downwards from the ring respectively.
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