Synthesis and structural features of gold complexes [Ph3PCH2CH2Br][Au(CN)2Br2], [Ph3PEt]2[Au(CN)2Br2][Au(CN)Br3], [(p-Tol)4Sb][Au(CN)2Br2], Ph3PC(H)(CN)Au(CN)2Cl

Abstract

The interaction of tetraorganylphosphonium,-stibonium halides and triphenylphosphonium cyanomethylide with potassium dihalodicyanoaurates in water or acetonitrile gave gold complexes [Ph3PCH2CH2Br][Au(CN)2Br2] (1), [Ph3PEt]2[Au(CN)2Br2][Au(CN)Br3] (2), [(p-Tol)4Sb][Au(CN)2Br2] (3), Ph3PC(H)(CN)Au(CN)2Cl (4). According to X-ray diffraction data, the pnictogen atoms in the cations of ionic complexes 13 have tetrahedral coordination; in square anions, the bromine atoms and cyano-groups surround the central gold atoms. In complex 4, the phosphorus and gold atoms are tetrahedrally and squarely coordinated; the ylide carbon atom is located at the gold atom in the trans-position relative to the chlorine atom. According to X-ray diffraction data 1 (CCDC 2524652), C22H19AuBr3N2P, M = 779.06; monoclinic syngony, space group P21/n; cell parameters: a = 9,0688(4) Å, b = 16,2023(7) Å, c = 17,0480(8) Å; α = 90,00, β = 99,530(4),  = 90,00, V = 2470,38(19) Å3, Z = 4; выч = 2,095 g/cm3;  = 10,883 mm–1; F(000) = 1456,0; reg. collection by 2q: 4,857; total reflections 10414; independent reflections 6159 (Rint = 0,0337); GOOF = 0,974; R-factor 0,0455; 2 (CCDC 2524655), C43H40Au2Br5N3P2, M = 1454,20; triclinic syngony, space group P–1; cell parameters: a = 10,6211(4) Å, b = 11,5872(6) Å, c = 11,8077(5) Å; α = 115,695(4), β = 91,956(3),  = 115,224(4), V = 1141,09(9) Å3, Z = 1; выч = 2,116 g/cm3;  = 10,902 mm–1; F(000) = 682,0; collection area by 2q: 4,457; total reflections 8285; independent reflections 5615 (Rint = 0,0251); GOOF = 1,023; R-factor 0,0506; 3 (CCDC 2524660), C30H28AuBr2N2Sb, M = 895,08; monoclinic syngony, space group P21/n; cell parameters: a = 13,1198(6) Å, b = 14,8740(5) Å, c = 16,4548(7) Å; α = 90,00, β = 103,964(4),  = 90,00, V = 3116,2(2) Å3, Z = 4; выч = 1,908 g/cm3;  = 8,154 mm–1; F(000) = 1680,0; collection area by 2q: 4,2257; total reflections 12717; independent reflections 7810 (Rint = 0,0453). GOOF = 1,007; R-factor 0,0652; 4 (CCDC 2524646), C22H16AuClN3P, M = 895,08; monoclinic syngony, space group P21/c; cell parameters: a = 8,3955(2) Å, b = 15,0045(3) Å, c = 17,1970(3) Å; α = 90,00, β = 92,778(2),  = 90,00, V = 2163,77(8) Å3, Z = 4; выч = 1,798 g/cm3;  = 7,008 mm–1; F(000) = 1120,0; collection area by 2q: 4,7457; total reflections 9297; independent reflections 5419 (Rint = 0,0239); GOOF = 1,022; R-factor 0,0291.