Structural studies of steric effects in phosphine complexes. Part XI. Synthesis, characterization, crystal and molecular structure of the dinitrato(trimesitylarsine)mercury(II) dimer

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Abstract
The synthesis and crystal and molecular structure of the dinitrato(trimesitylarsine)mercury(II) dimer are reported. The compound [HgAs(mesityl)3(NO3)2]2 belongs to the monoclinic space group P21/c[Formula: see text] with a = 20.001(2), b = 17.591(5), c = 16.553(2), β = 99.991(6), and Z = 4; the asymmetric unit contains two independent half dimers. The structure was refined to a final R of 0.0458 for 2631 observed reflections measured by diffractometer with 2 < θ < 20°. The crystal structure consists of discrete centrosymmetric dimeric molecules of [HgAs(mesityl)3(NO3)2]2 separated by normal van der Waals distances. The mercury coordination in both dimers I and II is characterized by three strong, nearly coplanar bonds (in I Hg—As 2.476(3), Hg—O 2.41(2) and 2.20(2), and in II Hg—As 2.482(3), Hg—O 2.28(2) and 2.39(2), and three weaker Hg—O bonds in the range 2.55–2.90 Å. Both independent trimesitylarsine ligands have the same regular propeller conformation (Hg—As—C—C torsion angles of 45 to 50°) and the largest C—As—C angles (mean value 112.5(8)°) yet determined. The As(mesityl)3 cone angle is 202°. The two independent dimers differ primarily in the orientation of the non-bridging nitrato groups. Nitrato vibrational and arsine 1H nmr data are also presented for [HgAs(mesityl)3(NO3)2]2, which becomes monomeric in dichloroethane solution.

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