Department of Chemistry, University of Copenhagen, Universitetsparken 5, DK-2100 Copenhagen Ø, Denmark.
Inorg Chem. 2010 Oct 4;49(19):8769-78. doi: 10.1021/ic1009797.
The novel S = 1/2 thionitrosyl complexes Cr(NS)(CN)(5)(3-), Cr(NS)(dmso)(5)(2+), and Cr(NS)(nmf)(5)(2+) (dmso = dimethyl sulfoxide, nmf = N-methylformamide) have been prepared, and their optical and electron paramagnetic resonance (EPR) spectra were studied. The values of the isotropic and anisotropic hyperfine and superhyperfine coupling constants A((53)Cr), A((14)N), and A((13)C) and of g were determined from the EPR spectra at room temperature and at 66 K. The values of A(⊥) and A(iso) in the thionitrosyl complexes were slightly higher than in the analogous nitrosyl complexes. A common feature in the optical absorption spectra of the thionitrosyl complexes in solution at 298 K is an absorption band around 600 nm with a vibronic structure whereas such a band is located around 450 nm in the analogous nitrosyl complexes. Density functional theory (DFT) studies of the series of complexes Cr(N)(H(2)O)(5)(2+), Cr(NO)(H(2)O)(5)(2+), Cr(NS)(H(2)O)(5)(2+), and Cr(NSe)(H(2)O)(5)(2+) show that the unpaired electron resides in a metal-based d(xy) orbital and that the electronic structure in the equatorial plane is similar in all four complexes and similar to Cr(3+). The σ donating ability was found in the order N(3-) ≫ NO < NS ≈ NSe and the π accepting ability in the order NO > NS ≈ NSe. Time dependent DFT calculations gave in all four complexes a d(x(2)-y(2)) ← d(xy) transition energy around 17 500 cm(-1).
已制备了新颖的 S = 1/2 硫代亚硝酰配合物 Cr(NS)(CN)(5)(3-), Cr(NS)(dmso)(5)(2+), 和 Cr(NS)(nmf)(5)(2+)(dmso = 二甲亚砜,nmf = N-甲基甲酰胺),并研究了它们的光学和电子顺磁共振(EPR)谱。从室温和 66 K 的 EPR 谱确定了各向同性和各向异性超精细和超超精细耦合常数 A((53)Cr), A((14)N), 和 A((13)C)以及 g 的值。硫代亚硝酰配合物中 A(⊥)和 A(iso)的值略高于类似的亚硝酰配合物。在室温下溶液中硫代亚硝酰配合物的光学吸收光谱的一个共同特征是在大约 600 nm 处存在一个具有振动态结构的吸收带,而在类似的亚硝酰配合物中,该带位于大约 450 nm 处。Cr(N)(H(2)O)(5)(2+), Cr(NO)(H(2)O)(5)(2+), Cr(NS)(H(2)O)(5)(2+), 和 Cr(NSe)(H(2)O)(5)(2+)系列配合物的密度泛函理论(DFT)研究表明,未配对电子位于金属基 d(xy)轨道中,并且在赤道平面中的电子结构在四个配合物中是相似的,类似于 Cr(3+)。发现σ给体能力的顺序为 N(3-)≫NO<NS≈NSe,π接受能力的顺序为 NO>NS≈NSe。在所有四个配合物中,时间相关的 DFT 计算给出了大约 17 500 cm(-1)的 d(x(2)-y(2)) ← d(xy)跃迁能。