metal-organic compounds
Di-μ-tert-butanolato-bis[bis(η5-cyclopentadienyl)erbium(III)]
aDepartment Chemie und Biochemie, Ludwig-Maximilians-Universität München, Lehrstuhl für Anorganische Festkörperchemie, Butenandtstrasse 5–13 (D), D-81377 München, Germany
*Correspondence e-mail: wolfgang.schnick@uni-muenchen.de
In the centrosymmetric title compound, [Er2(C5H5)4(C4H9O)2], each Er atom is in a distorted tetrahedral coordination environment, coordinated by two cyclopentadienyl rings and two tert-butoxy groups, forming a dimeric complex bridged through the tert-butoxy groups.
Related literature
During our search for highly reactive molecular precursors, we characterized a series of lanthanide amide (Baisch, Pagano, Zeuner, Barros et al., 2006) and carbamate complexes (Baisch, Pagano, Zeuner & Schnick, 2006). The synthesis of [Er2{μ-η1:η2-OC(OBut)NH}Cp4] and its application as a precursor is described by Zeuner et al. (2008). For related literature and a general overview of cyclopentadienyl-containing compounds of the lanthanides, see: Schumann et al. (1995).
Experimental
Crystal data
|
Data collection: COLLECT (Nonius, 2004); cell DENZO/SCALEPACK (Otwinowski & Minor 1997); data reduction: DENZO/SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg 1999); software used to prepare material for publication: SHELXL97.
Supporting information
10.1107/S1600536808004248/su2044sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536808004248/su2044Isup2.hkl
[Er2{µ-η1:η2-OC(OBut)NH}Cp4] was dissolved in dry THF and stirred for 12 h at 297 K. After evaporation of the solvent the orange residue was suspended in dry hexane. The filtrate was stored at 279 K to afford [Cp2ErtBuO]2 as pink crystals.
The H atoms were positioned geometrically and refined using a riding model: C(aromatic)–H = 0.95 Å with Uiso(H) = 1.2Ueq(C), and C(aliphatic)–H = 0.98 Å with Uiso(H) = 1.5Ueq(C).
Data collection: COLLLECT (Nonius, 2004); cell
DENZO/SCALEPACK (Otwinowski & Minor 1997); data reduction: DENZO/SCALEPACK (Otwinowski & Minor 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).[Er2(C5H5)4(C4H9O)2] | F(000) = 716 |
Mr = 741.10 | Dx = 1.928 Mg m−3 |
Monoclinic, P21/n | Melting point: not measured K |
Hall symbol: -P 2yn | Mo Kα radiation, λ = 0.71073 Å |
a = 8.3905 (17) Å | Cell parameters from 14322 reflections |
b = 15.628 (3) Å | θ = 3.1–27.5° |
c = 9.950 (2) Å | µ = 6.55 mm−1 |
β = 101.85 (3)° | T = 200 K |
V = 1276.9 (5) Å3 | Block, pink |
Z = 2 | 0.13 × 0.07 × 0.04 mm |
Nonius KappaCCD diffractometer | 2912 independent reflections |
Radiation source: fine-focus sealed tube | 2578 reflections with I > \2s(I) |
Graphite monochromator | Rint = 0.021 |
Detector resolution: 9 pixels mm-1 | θmax = 27.5°, θmin = 3.2° |
ϕ and ω scans | h = −10→10 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | k = −20→20 |
Tmin = 0.594, Tmax = 0.783 | l = −12→12 |
5666 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.022 | H-atom parameters constrained |
wR(F2) = 0.053 | w = 1/[σ2(Fo2) + (0.025P)2 + 1.7644P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.002 |
2912 reflections | Δρmax = 1.29 e Å−3 |
149 parameters | Δρmin = −1.23 e Å−3 |
0 restraints | Extinction correction: (SHELXL97; Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0022 (2) |
[Er2(C5H5)4(C4H9O)2] | V = 1276.9 (5) Å3 |
Mr = 741.10 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 8.3905 (17) Å | µ = 6.55 mm−1 |
b = 15.628 (3) Å | T = 200 K |
c = 9.950 (2) Å | 0.13 × 0.07 × 0.04 mm |
β = 101.85 (3)° |
Nonius KappaCCD diffractometer | 2912 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | 2578 reflections with I > \2s(I) |
Tmin = 0.594, Tmax = 0.783 | Rint = 0.021 |
5666 measured reflections |
R[F2 > 2σ(F2)] = 0.022 | 0 restraints |
wR(F2) = 0.053 | H-atom parameters constrained |
S = 1.05 | Δρmax = 1.29 e Å−3 |
2912 reflections | Δρmin = −1.23 e Å−3 |
149 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Er1 | 0.080747 (15) | 0.036095 (8) | 0.666673 (13) | 0.01748 (7) | |
C15 | 0.2668 (4) | −0.0762 (3) | 0.8373 (4) | 0.0332 (8) | |
H15 | 0.2131 | −0.1176 | 0.8821 | 0.040* | |
C13 | 0.3898 (5) | 0.0464 (3) | 0.7888 (5) | 0.0385 (9) | |
H13 | 0.4331 | 0.1028 | 0.7953 | 0.046* | |
C23 | −0.0655 (5) | 0.0983 (3) | 0.8573 (4) | 0.0396 (10) | |
H23 | −0.0683 | 0.0605 | 0.9315 | 0.048* | |
C25 | −0.1323 (5) | 0.1661 (2) | 0.6539 (4) | 0.0328 (8) | |
H25 | −0.1887 | 0.1835 | 0.5653 | 0.039* | |
C21 | 0.0166 (5) | 0.1986 (2) | 0.7245 (4) | 0.0349 (8) | |
H21 | 0.0797 | 0.2414 | 0.6919 | 0.042* | |
C11 | 0.3101 (4) | −0.0858 (3) | 0.7084 (4) | 0.0312 (8) | |
H11 | 0.2906 | −0.1350 | 0.6513 | 0.037* | |
C22 | 0.0565 (5) | 0.1574 (3) | 0.8508 (4) | 0.0376 (9) | |
H22 | 0.1505 | 0.1679 | 0.9203 | 0.045* | |
C14 | 0.3175 (5) | 0.0055 (3) | 0.8874 (4) | 0.0391 (9) | |
H14 | 0.3053 | 0.0290 | 0.9728 | 0.047* | |
C12 | 0.3865 (4) | −0.0107 (3) | 0.6790 (4) | 0.0339 (8) | |
H12 | 0.4288 | −0.0001 | 0.5990 | 0.041* | |
C24 | −0.1835 (5) | 0.1041 (3) | 0.7358 (4) | 0.0375 (9) | |
H24 | −0.2809 | 0.0715 | 0.7134 | 0.045* | |
O1 | 0.0788 (3) | 0.06891 (14) | 0.4454 (2) | 0.0195 (4) | |
C1 | 0.1512 (4) | 0.1414 (2) | 0.3870 (3) | 0.0246 (7) | |
C2 | 0.0347 (5) | 0.2174 (2) | 0.3640 (4) | 0.0343 (8) | |
H2A | −0.0665 | 0.2007 | 0.3014 | 0.051* | |
H2B | 0.0853 | 0.2649 | 0.3238 | 0.051* | |
H2C | 0.0106 | 0.2354 | 0.4520 | 0.051* | |
C4 | 0.1903 (5) | 0.1155 (2) | 0.2497 (4) | 0.0328 (8) | |
H4A | 0.2719 | 0.0698 | 0.2642 | 0.049* | |
H4B | 0.2331 | 0.1651 | 0.2082 | 0.049* | |
H4C | 0.0910 | 0.0951 | 0.1883 | 0.049* | |
C3 | 0.3083 (5) | 0.1691 (3) | 0.4829 (4) | 0.0360 (9) | |
H3A | 0.2863 | 0.1820 | 0.5737 | 0.054* | |
H3B | 0.3512 | 0.2203 | 0.4457 | 0.054* | |
H3C | 0.3886 | 0.1228 | 0.4908 | 0.054* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Er1 | 0.01723 (10) | 0.01828 (10) | 0.01704 (10) | 0.00043 (5) | 0.00380 (6) | −0.00140 (5) |
C15 | 0.0310 (19) | 0.038 (2) | 0.0284 (19) | 0.0078 (16) | 0.0010 (14) | 0.0104 (16) |
C13 | 0.0205 (18) | 0.041 (2) | 0.049 (2) | −0.0049 (15) | −0.0040 (16) | 0.0010 (19) |
C23 | 0.058 (3) | 0.035 (2) | 0.033 (2) | 0.0116 (19) | 0.0257 (19) | 0.0020 (17) |
C25 | 0.038 (2) | 0.0274 (19) | 0.033 (2) | 0.0108 (16) | 0.0053 (15) | −0.0065 (15) |
C21 | 0.045 (2) | 0.0218 (18) | 0.042 (2) | −0.0023 (16) | 0.0192 (17) | −0.0102 (16) |
C11 | 0.0268 (18) | 0.036 (2) | 0.0295 (19) | 0.0109 (15) | 0.0022 (14) | 0.0029 (15) |
C22 | 0.042 (2) | 0.038 (2) | 0.031 (2) | 0.0075 (17) | 0.0030 (16) | −0.0179 (17) |
C14 | 0.031 (2) | 0.054 (3) | 0.0276 (19) | 0.0070 (19) | −0.0043 (15) | −0.0051 (19) |
C12 | 0.0188 (17) | 0.049 (2) | 0.035 (2) | 0.0079 (16) | 0.0079 (14) | 0.0053 (18) |
C24 | 0.0297 (19) | 0.030 (2) | 0.058 (3) | 0.0028 (16) | 0.0221 (18) | −0.0096 (19) |
O1 | 0.0228 (11) | 0.0165 (11) | 0.0196 (11) | −0.0040 (9) | 0.0050 (8) | 0.0020 (9) |
C1 | 0.0294 (17) | 0.0178 (16) | 0.0278 (17) | −0.0054 (13) | 0.0088 (13) | 0.0026 (13) |
C2 | 0.045 (2) | 0.0182 (17) | 0.042 (2) | −0.0002 (16) | 0.0144 (17) | 0.0095 (16) |
C4 | 0.042 (2) | 0.0291 (19) | 0.0300 (18) | −0.0063 (16) | 0.0147 (15) | 0.0041 (16) |
C3 | 0.040 (2) | 0.033 (2) | 0.036 (2) | −0.0147 (17) | 0.0101 (16) | −0.0002 (17) |
Er1—O1 | 2.257 (2) | C25—H25 | 0.9500 |
Er1—O1i | 2.262 (2) | C21—C22 | 1.390 (6) |
Er1—C13 | 2.633 (4) | C21—H21 | 0.9500 |
Er1—C12 | 2.646 (3) | C11—C12 | 1.397 (6) |
Er1—C23 | 2.646 (4) | C11—H11 | 0.9500 |
Er1—C24 | 2.673 (3) | C22—H22 | 0.9500 |
Er1—C22 | 2.673 (4) | C14—H14 | 0.9500 |
Er1—C11 | 2.679 (4) | C12—H12 | 0.9500 |
Er1—C21 | 2.682 (4) | C24—H24 | 0.9500 |
Er1—C14 | 2.685 (4) | O1—C1 | 1.461 (4) |
Er1—C25 | 2.692 (4) | O1—Er1i | 2.262 (2) |
Er1—C15 | 2.705 (4) | C1—C3 | 1.523 (5) |
C15—C14 | 1.405 (6) | C1—C4 | 1.524 (5) |
C15—C11 | 1.411 (5) | C1—C2 | 1.525 (5) |
C15—H15 | 0.9500 | C2—H2A | 0.9800 |
C13—C12 | 1.406 (6) | C2—H2B | 0.9800 |
C13—C14 | 1.409 (6) | C2—H2C | 0.9800 |
C13—H13 | 0.9500 | C4—H4A | 0.9800 |
C23—C22 | 1.391 (6) | C4—H4B | 0.9800 |
C23—C24 | 1.399 (6) | C4—H4C | 0.9800 |
C23—H23 | 0.9500 | C3—H3A | 0.9800 |
C25—C24 | 1.391 (6) | C3—H3B | 0.9800 |
C25—C21 | 1.397 (5) | C3—H3C | 0.9800 |
O1—Er1—O1i | 78.39 (8) | Er1—C13—H13 | 114.5 |
O1—Er1—C13 | 104.21 (12) | C22—C23—C24 | 108.3 (4) |
O1i—Er1—C13 | 134.35 (11) | C22—C23—Er1 | 75.9 (2) |
O1—Er1—C12 | 85.46 (10) | C24—C23—Er1 | 75.8 (2) |
O1i—Er1—C12 | 107.00 (11) | C22—C23—H23 | 125.8 |
C13—Er1—C12 | 30.90 (13) | C24—C23—H23 | 125.8 |
O1—Er1—C23 | 134.74 (11) | Er1—C23—H23 | 114.7 |
O1i—Er1—C23 | 107.78 (11) | C24—C25—C21 | 108.1 (4) |
C13—Er1—C23 | 101.80 (14) | C24—C25—Er1 | 74.2 (2) |
C12—Er1—C23 | 131.01 (13) | C21—C25—Er1 | 74.6 (2) |
O1—Er1—C24 | 108.69 (11) | C24—C25—H25 | 126.0 |
O1i—Er1—C24 | 88.69 (11) | C21—C25—H25 | 126.0 |
C13—Er1—C24 | 130.34 (14) | Er1—C25—H25 | 117.3 |
C12—Er1—C24 | 160.99 (13) | C22—C21—C25 | 108.2 (4) |
C23—Er1—C24 | 30.49 (13) | C22—C21—Er1 | 74.6 (2) |
O1—Er1—C22 | 121.39 (11) | C25—C21—Er1 | 75.3 (2) |
O1i—Er1—C22 | 137.07 (11) | C22—C21—H21 | 125.9 |
C13—Er1—C22 | 81.17 (13) | C25—C21—H21 | 125.9 |
C12—Er1—C22 | 111.94 (13) | Er1—C21—H21 | 116.3 |
C23—Er1—C22 | 30.31 (13) | C12—C11—C15 | 108.5 (4) |
C24—Er1—C22 | 50.05 (13) | C12—C11—Er1 | 73.5 (2) |
O1—Er1—C11 | 100.02 (10) | C15—C11—Er1 | 75.8 (2) |
O1i—Er1—C11 | 83.92 (11) | C12—C11—H11 | 125.8 |
C13—Er1—C11 | 50.50 (13) | C15—C11—H11 | 125.8 |
C12—Er1—C11 | 30.41 (12) | Er1—C11—H11 | 116.9 |
C23—Er1—C11 | 125.04 (12) | C21—C22—C23 | 107.8 (4) |
C24—Er1—C11 | 148.22 (12) | C21—C22—Er1 | 75.3 (2) |
C22—Er1—C11 | 123.46 (12) | C23—C22—Er1 | 73.8 (2) |
O1—Er1—C21 | 91.86 (10) | C21—C22—H22 | 126.1 |
O1i—Er1—C21 | 131.93 (10) | C23—C22—H22 | 126.1 |
C13—Er1—C21 | 93.72 (13) | Er1—C22—H22 | 116.9 |
C12—Er1—C21 | 119.13 (13) | C15—C14—C13 | 107.9 (4) |
C23—Er1—C21 | 49.88 (12) | C15—C14—Er1 | 75.7 (2) |
C24—Er1—C21 | 49.84 (12) | C13—C14—Er1 | 72.6 (2) |
C22—Er1—C21 | 30.08 (12) | C15—C14—H14 | 126.0 |
C11—Er1—C21 | 144.01 (12) | C13—C14—H14 | 126.0 |
O1—Er1—C14 | 133.98 (11) | Er1—C14—H14 | 117.7 |
O1i—Er1—C14 | 122.53 (12) | C11—C12—C13 | 107.9 (3) |
C13—Er1—C14 | 30.70 (14) | C11—C12—Er1 | 76.1 (2) |
C12—Er1—C14 | 50.61 (12) | C13—C12—Er1 | 74.0 (2) |
C23—Er1—C14 | 81.56 (13) | C12—C12—H12 | 126.1 |
C24—Er1—C14 | 111.95 (13) | C13—C12—H12 | 126.1 |
C22—Er1—C14 | 73.34 (13) | Er1—C12—H12 | 116.0 |
C11—Er1—C14 | 50.14 (13) | C25—C24—C23 | 107.6 (4) |
C21—Er1—C14 | 98.07 (13) | C25—C24—Er1 | 75.8 (2) |
O1—Er1—C25 | 84.86 (10) | C23—C24—Er1 | 73.7 (2) |
O1i—Er1—C25 | 101.80 (10) | C25—C24—H24 | 126.2 |
C13—Er1—C25 | 123.85 (13) | C23—C24—H24 | 126.2 |
C12—Er1—C25 | 147.00 (13) | Er1—C24—H24 | 116.5 |
C23—Er1—C25 | 49.88 (12) | C1—O1—Er1 | 130.07 (19) |
C24—Er1—C25 | 30.06 (12) | C1—O1—Er1i | 128.22 (18) |
C22—Er1—C25 | 49.74 (12) | Er1—O1—Er1i | 101.61 (8) |
C11—Er1—C25 | 173.19 (12) | O1—C1—C3 | 110.4 (3) |
C21—Er1—C25 | 30.13 (12) | O1—C1—C4 | 109.6 (3) |
C14—Er1—C25 | 123.08 (13) | C3—C1—C4 | 108.6 (3) |
O1—Er1—C15 | 130.36 (10) | O1—C1—C2 | 110.9 (3) |
O1i—Er1—C15 | 92.60 (11) | C3—C1—C2 | 108.6 (3) |
C13—Er1—C15 | 50.45 (13) | C4—C1—C2 | 108.7 (3) |
C12—Er1—C15 | 50.39 (12) | C1—C2—H2A | 109.5 |
C23—Er1—C15 | 94.67 (12) | C1—C2—H2B | 109.5 |
C24—Er1—C15 | 119.92 (13) | H2A—C2—H2B | 109.5 |
C22—Er1—C15 | 98.37 (12) | C1—C2—H2C | 109.5 |
C11—Er1—C15 | 30.38 (11) | H2A—C2—H2C | 109.5 |
C21—Er1—C15 | 126.53 (12) | H2B—C2—H2C | 109.5 |
C14—Er1—C15 | 30.22 (14) | C1—C4—H4A | 109.5 |
C25—Er1—C15 | 144.28 (12) | C1—C4—H4B | 109.5 |
C14—C15—C11 | 107.6 (4) | H4A—C4—H4B | 109.5 |
C14—C15—Er1 | 74.1 (2) | C1—C4—H4C | 109.5 |
C11—C15—Er1 | 73.8 (2) | H4A—C4—H4C | 109.5 |
C14—C15—H15 | 126.2 | H4B—C4—H4C | 109.5 |
C11—C15—H15 | 126.2 | C1—C3—H3A | 109.5 |
Er1—C15—H15 | 117.9 | C1—C3—H3B | 109.5 |
C12—C13—C14 | 108.1 (4) | H3A—C3—H3B | 109.5 |
C12—C13—Er1 | 75.1 (2) | C1—C3—H3C | 109.5 |
C14—C13—Er1 | 76.7 (2) | H3A—C3—H3C | 109.5 |
C12—C13—H13 | 125.9 | H3B—C3—H3C | 109.5 |
C14—C13—H13 | 125.9 |
Symmetry code: (i) −x, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Er2(C5H5)4(C4H9O)2] |
Mr | 741.10 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 200 |
a, b, c (Å) | 8.3905 (17), 15.628 (3), 9.950 (2) |
β (°) | 101.85 (3) |
V (Å3) | 1276.9 (5) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 6.55 |
Crystal size (mm) | 0.13 × 0.07 × 0.04 |
Data collection | |
Diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2001) |
Tmin, Tmax | 0.594, 0.783 |
No. of measured, independent and observed [I > \2s(I)] reflections | 5666, 2912, 2578 |
Rint | 0.021 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.022, 0.053, 1.05 |
No. of reflections | 2912 |
No. of parameters | 149 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.29, −1.23 |
Computer programs: COLLLECT (Nonius, 2004), DENZO/SCALEPACK (Otwinowski & Minor 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg 1999).
Acknowledgements
The authors are indebted to Dr Peter Meyer for performing the single-crystal X-ray diffractometry. Financial support by the Deutsche Forschungsgemeinschaft (DFG) (Schwerpunktprogramm SPP 1166, Lanthanoidspezifische Funktionalitäten in Molekül und Material, project SCHN377/10) and the Fonds der Chemischen Industrie is also gratefully acknowledged.
References
Baisch, U., Pagano, S., Zeuner, M., Barros, N., Maron, L. & Schnick, W. (2006). Chem. Eur. J. 12, 4785–4798. Web of Science CSD CrossRef PubMed CAS Google Scholar
Baisch, U., Pagano, S., Zeuner, M. & Schnick, W. (2006). Eur. J. Inorg. Chem. pp. 3517–3524. Web of Science CSD CrossRef Google Scholar
Brandenburg, K. (1999). DIAMOND. Release 2.1c. Crystal Impact GbR, Bonn, Germany. Google Scholar
Nonius (2004). COLLECT. Nonius BV, Delft, The Netherlands. Google Scholar
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307–326. New York: Academic Press. Google Scholar
Schumann, H., Messe-Marktscheffel, J. A. & Esser, L. (1995). Chem. Rev. 95, 865–986. CrossRef CAS Web of Science Google Scholar
Sheldrick, G. M. (2001). SADABS. Version 2. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zeuner, M., Pagano, S. & Schnick, W. (2008). Chem. Eur. J. 14, 1524–1531. Web of Science CrossRef PubMed CAS Google Scholar
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
By stirring [Er2{µ-η1:η2-OC(OBut)NH}Cp4] in THF the carbamato moiety decomposes to [Cp2ErtBuO]2 and an amorphous solid showing strong C=N vibrations (2190 cm-1) in the IR spectra. It is likely that the tert-butylcarbamato ligand splits up into tert-butanol and cyanate. Attempts to isolate a crystalline cyanato complex were unsuccessful as yet. The structure of [Cp2ErtBuO]2 is in accordance with a series of lanthanide-cyclopentadienyl-alcoholate-complexes synthesized so far (Schumann et al., 1995).