Reaction of square planar [
Platinum(II) terpyridyl complexes with alkynyl ligands have attracted great interest in recent years due to their unique photophysics [
All chemicals employed here were used without further purification unless otherwise stated. All solvents purchased for organic synthesis were anhydrous and used without further purification. A Br2–CHCl3 solution was prepared by addition of 12 drops of Br2 to 10 mL of CHCl3 [
Single crystals of
Crystallographic details for
Empirical formula | C23H16Br3N3Pt |
Fw | 769.20 |
Temperature (K) | 173(2) |
|
0.71075 |
Crystal system | Triclinic |
Space group |
|
|
7.2090(4) |
|
12.9921(6) |
|
13.1231(6) |
|
67.0477(14) |
|
75.8967(15) |
|
78.1381(19) |
|
1089.25(9) |
|
2 |
|
2.345 |
|
11.950 |
Number of reflections | 10839 |
Unique reflections | 4955 |
GOF ( |
1.095 |
|
0.0902 |
|
0.0486 |
|
0.1210 |
Geometrical parameters.
Selected bond lengths and angles (Å, °)
Pt1–Br1 | 2.4498(12) | C1–C2 | 1.059(17) |
Pt1–Br2 | 2.4644(12) | N1–Pt1–N2 | 80.8(4) |
Pt1–N1 | 2.041(10) | N2–Pt1–N3 | 80.2(4) |
Pt1–N2 | 1.976(9) | Pt1–C1–C2 | 175.3(12) |
Pt1–N3 | 2.030(11) | C1–C2–C3 | 174.4(14) |
Pt1–C1 | 2.054(10) | Br1–Pt1–Br2 | 178.46(5) |
Interatomic distances (Å) for intermolecular
C2 |
3.299(15) |
C3 |
3.373(15) |
C3 |
3.302(15) |
C4 |
3.366(17) |
C5 |
3.290(17) |
C5 |
3.362(17) |
C5 |
3.256(16) |
C8 |
3.374(18) |
Symmetry operators: i
Hydrogen-bond geometry (Å, °)
|
|
H |
|
|
---|---|---|---|---|
C4–H1 |
0.95 | 2.84 | 3.688(14) | 149 |
C11–H8 |
0.95 | 2.86 | 3.761(13) | 160 |
C22–H15 |
0.95 | 3.34 | 3.836(14) | 115 |
C23–H16 |
0.95 | 2.80 | 3.576(13) | 140 |
C4–H1 |
0.95 | 3.49 | 4.072(13) | 122 |
C5–H2 |
0.95 | 3.17 | 3.922(14) | 137 |
C16–H11 |
0.95 | 2.87 | 3.702(14) | 147 |
C10–H7 |
0.95 | 2.94 | 3.733(13) | 142 |
C8–H5 |
0.95 | 3.12 | 3.758(13) | 126 |
C9–H6 |
0.95 | 3.14 | 3.738(11) | 122 |
C22–H15 |
0.95 | 3.20 | 3.872(12) | 129 |
C10–H7 |
0.95 | 3.12 | 3.718(13) | 122 |
C12–H9 |
0.95 | 3.19 | 3.945(13) | 138 |
C15–H10 |
0.95 | 2.89 | 3.597(13) | 132 |
C6–H3 |
0.95 | 3.32 | 3.943(13) | 125 |
C17–H12 |
0.95 | 2.89 | 3.819(15) | 166 |
C21–H14 |
0.95 | 3.28 | 3.909(13) | 126 |
Symmetry operators: i
An orange suspension of [Pt(C
The synthetic route for the formation of platinum(IV) terpyridyl complexes is summarized in Scheme
Synthetic route for platinum(IV) complexes in this study.
The identities of the complex
The IR spectrum of
The molecular structure of
The molecular structure of
Packing diagram. The green lines denote intermolecular hydrogen bonds.
In summary, we have prepared an alkynylplatinum(IV) complex by simple oxidation of the corresponding alkynylplatinum(II) one. It is anticipated that the successful route described here provides a useful methodology to obtain a variety of platinum(IV) complexes with a wide range of alkynyl ligands.
Complete lists of positional and isotropic displacement coefficients for hydrogen atoms and anisotropic displacement coefficients for the nonhydrogen atoms, bond lengths and angles, and torsion angles are listed as supplementary material available on line at
The authors declare that there is no conflict of interests regarding the publication of this paper.
H. Watanabe is thanked for experimental assistance at an early stage of the project.