| In this thesis, seven novel Cu'/Au1 supromolecular complexes containing triphenylphosphine or N-donor heterocycles have been synthesized, [Cu(SCN)(2-pds)]n (1), [Cu(Him)(PPh3)2I] (2), [Cu2(PPh3)4(rpp)](BF4)2 (3), [Au(PPh3)(in)] (4), [Au(PPh3)(bta)] (5), [Au(PPh3)(ca)] (6), [Au(PPh3)(spy)] (7). These supramolecular complexes have been characterized by elementary, infrared spectroscopic analysis, ultra-violet and visible spectroscopic analysis, luminescence spectroscopic analysis and X-ray single crystal diffraction.The complex [Cu(SCN)(2-pds)]n (1) crystallizes in the monoclinic space group P21/n, with a = 7.7043(7)A, 6= 11.2291(10)A, c= 14.6727(1 3)A, a =90°, beta = 91.183(2)°, gamma=90°, V= 1269.1(2) A3, Z=4, Dc= 1.790 Mg/m3. The single crystal determination for complex 1 reveals that each Cu1 cation exhibits a N3S coordination sphere using two 2-dps ligands and two SCN" anions in a normal tetrahedral environment. Each 2-pds unit acts as a bidentate ligand and exhibits a typical twisted conformation. Cu atoms are bridged by SCN" ligands to form an infinite square- wave[CuSCN] chain. All atoms in the same chain are nearly coplanar. Adjacent CuSCN chains adopt a reverse direction (SCN-Cu-SCN and NCS-Cu-NCS), and the crest in one chain is opposite to the trough in another adjacent chain. As the edges, two ligands and two SCN" form a 22-membered macrometallacyclic ring made up of four CuI at the corners. The four corner CuI atoms are completely coplanar completing a parallelogram. The complex shows the construction from 2D to 3D supramolecular architecture through intermolecular π-π stacking and edge-to- face CH-π stacking interactions.The complex [Cu(Him)(PPh3)2I] 2 crystallizes in the monoclinic space group P2(1)/n, with a = 13.335(14)A, b= 13.103(9)A, c = 21. 544(1 6)A, ar = 90°, beta = 101.13? gamma=90°, V = 3694(5)A3, Z = 4, Dc= 1.408 Mg/m3. The single crystal determination for complex 2 reveals that each CuI cation exhibits a NI?2 coordination sphere using two triphenylphophine ligands, one I" anion and one imidazole in a distorted-tetrahedral environment with P(l)-Cu(l) 2.300(3) A, P(2)-Cu(l) 2.311(2) A, N(1)-Cu(l) 2.096(7) A and I(1)-Cu(1) 2.702(2) A. Because of the crowd space of PPh3, the bond angle of P- Cu- P is 123.60(8)°, which is larger than those in the analogous complexes. While the bond angle of I - Cu- N, 101.68(18)°, is smaller than the analogous. To be interesting, the C- H-I and N- H-I weak hydrogen bonds in complex 2 lead to the formation of two-dimensional supramolecular structure, with d(NH-I)=2.680 A, d(N- 1)=3.550 A, 6 (N- H- I) =162.8°, d(CH- 1)=3.215 A, d(C-I)=4.062 A, 0(C-H- I)=148.1°.The complex [Cu2(PPh3)4(tpp)](BF4)2 3 crystallizes in the monoclinic space group P2(l)/n, with a=13.1854(9)A, b=11.4871(8)A, c= 27.2975(18)A, a =90°, beta= 100.840(2)°, gamma =90°, V= 100.840(2)A3, Z=2, Dc= 1.422 Mg/m3. Structural analysis reveals that the complex is composed of a cation [Qi2(PPh3)4(tpp)]2+ and two anions BF4 o In [Cu2(PPh3)4(tpp)]2+, each CuI cation exhibits a N2P2 coordination sphere using two triphenylphophine ligands and two N from ligand Tetra-2-pyridinylpyrazine in a distorted-tetrahedral environment with P(1)-Cu(1) 2.2755(10) A , P(2)-Cu(1) 2.2811(10) A, N(1)-Cu(1) 2.115(3) A and N(2)-Cu(1) 2.155(3) A. Only four nitrogen atoms in the ligand tpp coordinate to CuI, two N without coordinating. To be interesting, two phenyl rings from two different triphenylphosphine and pyrazyl ring from ligand tpp are approximately parallel with the face-to-face distance of 3.7821 A and the dihedral angle of 12.4°, indicating π-π stacking interactions.The complex [Au(PPh3)(in)] 4 crystallizes in the triclinic space group P2(1)/n, with a = 6.5683(6)A, b = 11.5851(10)A, c = 15.1189(14)A, a = 103.011(2)°, beta = 97.442(2)°, Y = 96.551(2)°, V= 1099.20(17)A3, Z = 2, Dc= 1.738 Mg/m3. X-ray crystallographic data reveals that complex 4 adopts a three-dimensional supramolecular structure where each AuI cation exhibits a NP coordination sphere using one triphenylphosphin...
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