Rhenium Complex with 2-[(2-Pyridylmethyl)amino]ethanethiol

Masahiro MIKURIYA, Tetsuji WATANABE, Aiko SUYAMA, Daisuke YOSHIOKA
2015 X-ray Structure Analysis Online  
There has been considerable interest in the coordination chemistry of metal complexes with organic thiolic ligands because of their various structures involving oligonuclear and polynuclear metal atoms. 1-10 2-[(2-Pyridylmethyl)amino]ethanethiol (Hpmaet) is an interesting thiolic ligand to make such compounds, giving a trinuclear zinc(II) complex, [Zn{Zn(pmaet)2}2](ClO4)2, 5 a trinuclear cadmium(II) complex, [Cd{Cd(pmaet)2}2](ClO4)2, 8 a tetranuclear palladium(II) complex,
more » ... d4(pmaet)4](ClO4)3Cl, 7 and a polynucler manganese(II) complex, [Mn(pmaet)Cl]n. 3 However, there has been no report on a rhenium complex with Hpmaet. In this study, we synthesized a new complex from a reaction of ammonium perrhenate(VII) and Hpmaet, and determined the crystal structure of this compound, which shows an octahedral rhenium(VII) with three donor atoms of pmaet and three oxidooxygen atoms, as shown in Fig. 1 . The Hpmaet ligand was synthesized by a reaction of 2-aminomethylpyridine with ethylene sulfide according to a literature method. 2 To a solution of Hpmaet (75 mg, 0.44 mmol) in 4 cm 3 of methanol was added two drops of triethylamine (24 mg, 0.24 mmol). A solution of ammonium perrhenate (103 mg, 0.38 mmol) in 4 cm 3 of methanol was added with stirring dropwise under argon. The resulting solution was left several days to give colorless crystals. The complexes were collected. X-ray diffraction data for these crystals were collected at 123 K on a Bruker CCD X-ray diffractometer (SMART APEX) using graphite-monochromated Mo-Ka radiation. Crystal data and details concerning data collection are given in Table 1 . The structure was solved by direct methods and refined by full-matrix least-squares methods. The hydrogen atoms were included using the riding atom model. All of the calculations were carried out on a Pentium IV Windows 2000 computer utilizing the SHELXTL software package. Crystallographic data have been deposited with Cambridge Crystallographic Data Centre: Deposit number A rhenium(VII) complex with 2-[(2-pyridylmethyl)amino]ethanethiol (Hpmaet), [Re(pmaet)O3], was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 123 K. It crystallizes in the monoclinic space group P21/n with a = 10.054(5)Å, b = 8.466(4)Å, c = 12.924(7)Å, b = 108.552(9)˚, V = 1043.0(10)Å 3 , Dx = 2.557 g/ cm 3 , and Z = 4. The R1 [I > 2s(I)] and wR2 (all data) values are 0.0195 and 0.0545, respectively, for all 2401 independent reflections. The compound consists of an octahedral molecule of rhenium(VII) with facial pmaet and three oxido oxygens. Table 1 Crystal and experimental data Chemical formula: C8H11N2O3ReS Formula weight = 401.45 T = 123 K Crystal system: monoclinic Space group: P21/n a = 10.054(5)Å b = 8.466(4)Å b = 108.552(9)c = 12.924(7)Å V = 1043.0(10)Å 3 Z = 4 Dx = 2.557 g/cm 3 Radiation: Mo Ka (l = 0.71073 Å) m(Mo Ka) = 11.839 mm -1 F(0 0 0) = 752 Crystal size = 0.22 ¥ 0.17 ¥ 0.17 mm 3 No. of re ections collected = 6196 No. of independent re ections = 2401 q range for data collection: 2.25 to 28.37D ata/Restraints/Parameters = 2401/0/136 Goodness-of-t on F 2 = 1.316 R indices [I > 2s(I)]: R1 = 0.0195, wR2 = 0.0541 R indices (all data): R1 = 0.0203, wR2 = 0.0545 (D/s)max = 0.000 (Dr)max = 1.394 eÅ -3 (Dr)min = -1.417 eÅ -3 Measurement: Bruker Smart APEX CCD diffractometer Program system: SHELXTL Structure determination: Direct methods (SHELXS-97) Re nement: full matrix least-squares (SHELXL-97) CCDC deposition number: 1029775 Fig. 1 Chemical structure of [Re(pmaet)O3].
doi:10.2116/xraystruct.31.3 fatcat:grmyimdaqzcazffgzmjk4vcmhi