Addition/Correction pubs.acs.org/IC
Correction to The Silicon Version of Phosphine Chalcogenides: Synthesis and Bonding Analysis of Stabilized Heavy Silaaldehydes Dennis Lutters, Anastasia Merk, Marc Schmidtmann, and Thomas Müller* Inorganic Chemistry 2016, 55 (17), 9026−9032. DOI: 10.1021/acs.inorgchem.6b01510 S Supporting Information *
In the article in question, we discovered an error in the measurement of the 77Se NMR chemical shifts of compound 15b and in the 125Te NMR chemical shift of compound 15c. The NMR chemical shifts of both heteronuclei were detected indirectly by 1HX HMBC experiments. We overlooked that, in the 1H-detected HMBC experiment, there is the possibility for folding in of resonances outside of the observed spectral range into the spectra. In both cases, this led to an erroneous detection of signals at too far low field. A redetermination using one- and two-dimensional methods gave the following NMR chemical shifts: compound 15b, δ77Se = −534.6; compound 15c, δ125Te = −1236.1. All conclusions drawn in our article are not influenced by this analytical error. The following corrections are required. Page 9027. Table 1 should be replaced.
Figure 1. Selected part of the 1H/77Se HMBC NMR (499.87 MHz, 305.0 K, C6D6) spectrum of 15b.
groups of the coordinating carbene ImMe4 [δ1H = 3.13 (15b), 3.09 (15c)] were detected (Figure 1 provides an example for compound 15b). The 77Se NMR chemical shift for 15b (δ77Se = −534.6) is high-field-shifted compared to those reported for 8b (δ77Se = −374.4) and 9b (δ77Se = −406.7). Similarly, the 125Te NMR signal of 15c (δ125Te = −1236.1) appears at a significantly higher field than that of 8c (δ125Te = −982.5). The Supporting Information has been modified, and new 77 Se NMR and 125Te NMR spectra have been added.
Table 1. NMR and IR Spectroscopic Data for the NHCStabilized Heavy Silaaldehydes 15, Which Are Pertinent for the Discussiona Ch δ1H δ29Si δ15N δ13CNHC δ77Se δ125Te 1 JSi−H 1 JSi−Ch 2 JCh−H IR ν̃̃Si−H calcd IR ν̃̃Si−Ch calcd
15a
15b
15c
13a
S 5.81 −37.3 179.5 152.5 − − 209 Hz − − 2088 cm−1 2222 cm−1 636 cm−1 641 cm−1
Se 5.74 −44.1 179.2 150.7 −534.6 − 210 Hz 247 Hz 11 Hz 2102 cm−1 2231 cm−1 − 540 cm−1
Te 5.86 −77.7 174.4 150.4 − −1236.1 208 Hz 671 Hz 13 Hz 2122 cm−1 2202 cm−1 − 454 cm−1
− 3.88 −80.5 179.2 168.5 − − 105 Hz − − 1970 cm−1 2120 cm−1 − −
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ASSOCIATED CONTENT
S Supporting Information *
The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.inorgchem.7b00929. Experimental procedures and computational details (PDF)
a
Data for the NHC-stabilized hydridosilylene 13a and calculated wavenumbers for the Si−H stretching vibration are given for comparison. Calculations are done at M06-2X/6-311+G(d,p)(H,C,N,Si,S,Se)/def2-TZVP(Te). The scaling factor for the calculated harmonic frequencies is 0.9871.22
Figure 1 should be replaced. Page 9028, left column: 77Se and 125Te NMR chemical shifts of 15b (δ77Se = −534.1) and 15c (δ125Te = −1236.1) were determined indirectly via 1H-detected HMBC spectroscopy and by one-dimensional methods. In both cases, the two-dimensional HMBC spectra showed a correlation between the heavy chalcogen isotopes and the Si−H hydrogen atoms. In addition, the correlations with the hydrogen atoms of the N−CH3 © 2016 American Chemical Society
A
DOI: 10.1021/acs.inorgchem.7b00929 Inorg. Chem. XXXX, XXX, XXX−XXX
