Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802020159/cm6023sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802020159/cm6023Isup2.hkl |
CCDC reference: 202281
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.005 Å
- R factor = 0.045
- wR factor = 0.088
- Data-to-parameter ratio = 19.0
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.480 Tmax scaled 0.316 Tmin scaled 0.215
A solution of 2,4-cyclopentadiene-1-ethanol (0.22 g, 2.0 mmol; Ohta et al., 1977) in THF (5 ml) was added to Cp3Y (0.57 g, 2.0 mmol) in THF (10 ml) and the mixture was stirred for 15 min at ambient temperature until Cp3Y was completely dissolved. The solution was concentrated to 3 ml and hexane (10 ml) was added. After the centrifugation of the mixture, the formed white microcrystalline solid of the title compound was separated by decantation, washed with hexane (10 ml) and dried in vacuum (yield 0.51 g, 72%). Suitable crystals were obtained by recrystallization from dme (m.p. 385–388 K). Spectroscopic analysis, IR (Nujol, ν cm−1): 3060 (w), 1360 (m), 1040 (s), 890 (m), 780 (s), 730 (m), 520 (w); elemental analysis, calculated for C32H46O6Y2: Y 25.26%; found: 25.08%.
The H atoms were placed in calculated positions and assigned to an isotropic displacement parameter of 0.08 Å2. The idealized CH3 groups were allowed to rotate about their C—O bond. The geometrical aspects of the structure were analyzed by using PLATON (Spek, 2001).
Data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ZORTEP (Zsolnai, Pritzkow, 1994); software used to prepare material for publication: SHELXL97.
Fig. 1. The molecular structure of the title compound. Displacement ellipsoids are drawn at the 30% probability level. |
[Y2(C5H5)2(C7H8O)2(C4H10O2)2] | Dx = 1.537 Mg m−3 |
Mr = 704.51 | Melting point: 385 K |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 8.6073 (2) Å | Cell parameters from 5194 reflections |
b = 11.2146 (1) Å | θ = 2.2–30.6° |
c = 15.7840 (1) Å | µ = 3.84 mm−1 |
β = 92.751 (1)° | T = 173 K |
V = 1521.83 (4) Å3 | Block, colorless |
Z = 2 | 0.40 × 0.38 × 0.30 mm |
F(000) = 728 |
Siemens SMART CCD diffractometer | 3482 independent reflections |
Radiation source: fine-focus sealed tube | 2489 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.081 |
ω scans | θmax = 27.5°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→11 |
Tmin = 0.448, Tmax = 0.659 | k = −13→14 |
11359 measured reflections | l = −15→20 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.088 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0324P)2] where P = (Fo2 + 2Fc2)/3 |
3482 reflections | (Δ/σ)max < 0.001 |
183 parameters | Δρmax = 0.59 e Å−3 |
0 restraints | Δρmin = −0.47 e Å−3 |
[Y2(C5H5)2(C7H8O)2(C4H10O2)2] | V = 1521.83 (4) Å3 |
Mr = 704.51 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 8.6073 (2) Å | µ = 3.84 mm−1 |
b = 11.2146 (1) Å | T = 173 K |
c = 15.7840 (1) Å | 0.40 × 0.38 × 0.30 mm |
β = 92.751 (1)° |
Siemens SMART CCD diffractometer | 3482 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2489 reflections with I > 2σ(I) |
Tmin = 0.448, Tmax = 0.659 | Rint = 0.081 |
11359 measured reflections |
R[F2 > 2σ(F2)] = 0.045 | 0 restraints |
wR(F2) = 0.088 | H-atom parameters constrained |
S = 1.01 | Δρmax = 0.59 e Å−3 |
3482 reflections | Δρmin = −0.47 e Å−3 |
183 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 | ||
Y | 0.61001 (3) | 0.60490 (3) | 0.57293 (2) | 0.01504 (10) | |
O1 | 0.6236 (2) | 0.43653 (19) | 0.49266 (16) | 0.0176 (5) | |
O2 | 0.4196 (3) | 0.7076 (2) | 0.66086 (16) | 0.0205 (6) | |
O3 | 0.1975 (3) | 0.9047 (2) | 0.65997 (17) | 0.0264 (6) | |
C1 | 0.7646 (4) | 0.4285 (3) | 0.6556 (2) | 0.0191 (8) | |
C2 | 0.6467 (4) | 0.4592 (3) | 0.7104 (3) | 0.0226 (8) | |
H2 | 0.5603 | 0.4129 | 0.7214 | 0.080* | |
C3 | 0.6819 (4) | 0.5724 (3) | 0.7457 (3) | 0.0247 (8) | |
H3 | 0.6242 | 0.6126 | 0.7851 | 0.080* | |
C4 | 0.8188 (4) | 0.6136 (3) | 0.7112 (3) | 0.0271 (8) | |
H4 | 0.8672 | 0.6863 | 0.7229 | 0.080* | |
C5 | 0.8702 (4) | 0.5249 (3) | 0.6555 (3) | 0.0230 (8) | |
H5 | 0.9586 | 0.5293 | 0.6240 | 0.080* | |
C6 | 0.7703 (4) | 0.3210 (3) | 0.5991 (3) | 0.0230 (8) | |
H6A | 0.6871 | 0.2665 | 0.6120 | 0.080* | |
H6B | 0.8685 | 0.2798 | 0.6094 | 0.080* | |
C7 | 0.7530 (4) | 0.3583 (3) | 0.5068 (3) | 0.0220 (8) | |
H7A | 0.8473 | 0.3982 | 0.4908 | 0.080* | |
H7B | 0.7387 | 0.2881 | 0.4714 | 0.080* | |
C8 | 0.8032 (4) | 0.6905 (3) | 0.4585 (3) | 0.0261 (9) | |
H8 | 0.8673 | 0.6344 | 0.4344 | 0.080* | |
C9 | 0.8391 (4) | 0.7565 (3) | 0.5322 (3) | 0.0250 (9) | |
H9 | 0.9312 | 0.7521 | 0.5654 | 0.080* | |
C10 | 0.7114 (4) | 0.8306 (3) | 0.5472 (3) | 0.0257 (9) | |
H10 | 0.7037 | 0.8835 | 0.5922 | 0.080* | |
C11 | 0.5971 (4) | 0.8102 (3) | 0.4818 (3) | 0.0240 (9) | |
H11 | 0.5008 | 0.8477 | 0.4759 | 0.080* | |
C12 | 0.6536 (4) | 0.7235 (3) | 0.4271 (3) | 0.0231 (8) | |
H12 | 0.6016 | 0.6933 | 0.3787 | 0.080* | |
C13 | 0.2977 (4) | 0.6365 (3) | 0.6945 (3) | 0.0288 (9) | |
H13A | 0.3226 | 0.6195 | 0.7532 | 0.080* | |
H13B | 0.2881 | 0.5631 | 0.6634 | 0.080* | |
H13C | 0.2013 | 0.6794 | 0.6893 | 0.080* | |
C14 | 0.4408 (4) | 0.8195 (3) | 0.7056 (3) | 0.0250 (9) | |
H14A | 0.5510 | 0.8366 | 0.7133 | 0.080* | |
H14B | 0.3983 | 0.8131 | 0.7612 | 0.080* | |
C15 | 0.3619 (4) | 0.9197 (3) | 0.6575 (3) | 0.0275 (9) | |
H15A | 0.3923 | 0.9955 | 0.6829 | 0.080* | |
H15B | 0.3926 | 0.9195 | 0.5992 | 0.080* | |
C16 | 0.1182 (4) | 0.9757 (3) | 0.5971 (3) | 0.0306 (10) | |
H16A | 0.1458 | 1.0579 | 0.6056 | 0.080* | |
H16B | 0.0080 | 0.9664 | 0.6014 | 0.080* | |
H16C | 0.1472 | 0.9507 | 0.5419 | 0.080* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Y | 0.01198 (15) | 0.01404 (15) | 0.01890 (18) | −0.00055 (14) | −0.00144 (11) | 0.00072 (17) |
O1 | 0.0129 (11) | 0.0167 (11) | 0.0231 (15) | 0.0003 (9) | −0.0015 (10) | −0.0002 (10) |
O2 | 0.0196 (12) | 0.0203 (12) | 0.0218 (16) | 0.0007 (10) | 0.0023 (11) | −0.0031 (11) |
O3 | 0.0197 (12) | 0.0256 (13) | 0.0340 (17) | 0.0022 (11) | 0.0017 (11) | 0.0055 (13) |
C1 | 0.0187 (17) | 0.0176 (17) | 0.020 (2) | 0.0036 (13) | −0.0071 (15) | 0.0005 (14) |
C2 | 0.0223 (18) | 0.0236 (19) | 0.021 (2) | 0.0016 (15) | −0.0037 (16) | 0.0033 (16) |
C3 | 0.0281 (19) | 0.029 (2) | 0.017 (2) | 0.0052 (15) | −0.0046 (16) | −0.0032 (16) |
C4 | 0.0290 (19) | 0.0221 (18) | 0.029 (2) | −0.0010 (17) | −0.0105 (17) | −0.0001 (18) |
C5 | 0.0162 (17) | 0.0273 (19) | 0.025 (2) | 0.0048 (15) | −0.0025 (16) | 0.0025 (17) |
C6 | 0.0213 (18) | 0.0183 (17) | 0.029 (2) | 0.0027 (14) | −0.0044 (16) | 0.0029 (17) |
C7 | 0.0159 (17) | 0.0219 (17) | 0.028 (2) | 0.0025 (13) | −0.0019 (16) | 0.0000 (16) |
C8 | 0.0213 (18) | 0.0217 (18) | 0.036 (3) | −0.0035 (15) | 0.0107 (17) | 0.0041 (18) |
C9 | 0.0173 (17) | 0.0214 (18) | 0.036 (3) | −0.0072 (14) | 0.0001 (16) | 0.0061 (18) |
C10 | 0.0230 (19) | 0.0185 (18) | 0.036 (3) | −0.0080 (15) | 0.0041 (17) | 0.0000 (17) |
C11 | 0.0201 (18) | 0.0163 (17) | 0.036 (3) | −0.0037 (14) | 0.0037 (17) | 0.0066 (17) |
C12 | 0.0229 (19) | 0.0224 (18) | 0.024 (2) | −0.0097 (15) | 0.0021 (16) | 0.0057 (16) |
C13 | 0.030 (2) | 0.026 (2) | 0.031 (3) | −0.0033 (15) | 0.0070 (18) | 0.0061 (17) |
C14 | 0.0239 (19) | 0.0285 (19) | 0.023 (2) | 0.0009 (16) | −0.0005 (16) | −0.0092 (17) |
C15 | 0.0223 (18) | 0.023 (2) | 0.037 (3) | −0.0028 (15) | 0.0023 (17) | −0.0040 (17) |
C16 | 0.030 (2) | 0.028 (2) | 0.034 (3) | 0.0010 (16) | −0.0020 (19) | 0.0007 (18) |
Y—Cg1 | 2.4537 (19) | C4—C5 | 1.412 (5) |
Y—Cg2 | 2.4260 (17) | C4—H4 | 0.9300 |
Y—O1i | 2.265 (2) | C5—H5 | 0.9300 |
Y—O1 | 2.280 (2) | C6—C7 | 1.516 (5) |
Y—O2 | 2.481 (2) | C6—H6A | 0.9700 |
Y—C1 | 2.687 (3) | C6—H6B | 0.9700 |
Y—C2 | 2.722 (4) | C7—H7A | 0.9700 |
Y—C3 | 2.792 (4) | C7—H7B | 0.9700 |
Y—C4 | 2.761 (4) | C8—C9 | 1.401 (6) |
Y—C5 | 2.690 (3) | C8—C12 | 1.406 (5) |
Y—C8 | 2.690 (4) | C8—H8 | 0.9300 |
Y—C9 | 2.704 (3) | C9—C10 | 1.408 (5) |
Y—C10 | 2.714 (3) | C9—H9 | 0.9300 |
Y—C11 | 2.714 (3) | C10—C11 | 1.410 (6) |
Y—C12 | 2.700 (4) | C10—H10 | 0.9300 |
Y—Yi | 3.7421 (7) | C11—C12 | 1.403 (5) |
O1—C7 | 1.427 (4) | C11—H11 | 0.9300 |
O1—Yi | 2.265 (2) | C12—H12 | 0.9300 |
O2—C13 | 1.440 (4) | C13—H13A | 0.9600 |
O2—C14 | 1.447 (4) | C13—H13B | 0.9600 |
O3—C16 | 1.421 (5) | C13—H13C | 0.9600 |
O3—C15 | 1.427 (4) | C14—C15 | 1.500 (5) |
C1—C2 | 1.407 (5) | C14—H14A | 0.9700 |
C1—C5 | 1.413 (5) | C14—H14B | 0.9700 |
C1—C6 | 1.502 (5) | C15—H15A | 0.9700 |
C2—C3 | 1.414 (5) | C15—H15B | 0.9700 |
C2—H2 | 0.9300 | C16—H16A | 0.9600 |
C3—C4 | 1.400 (5) | C16—H16B | 0.9600 |
C3—H3 | 0.9300 | C16—H16C | 0.9600 |
Cg1—Y—Cg2 | 120.80 (6) | C13—O2—C14 | 112.2 (3) |
Cg1—Y—O1 | 94.49 (7) | C13—O2—Y | 117.5 (2) |
Cg1—Y—O1i | 133.80 (7) | C14—O2—Y | 127.19 (19) |
Cg1—Y—O2 | 93.85 (7) | C16—O3—C15 | 111.0 (3) |
Cg2—Y—O1 | 105.56 (7) | C2—C1—C5 | 107.3 (3) |
Cg2—Y—O1i | 105.33 (7) | C2—C1—C6 | 127.3 (3) |
Cg2—Y—O2 | 104.72 (7) | C5—C1—C6 | 125.0 (3) |
O1i—Y—O1 | 69.17 (9) | C2—C1—Y | 76.3 (2) |
O1i—Y—O2 | 75.83 (8) | C5—C1—Y | 74.89 (19) |
O1—Y—O2 | 138.45 (8) | C6—C1—Y | 109.4 (2) |
O1i—Y—C1 | 118.62 (9) | C1—C2—C3 | 108.3 (3) |
O1—Y—C1 | 67.84 (10) | C1—C2—Y | 73.5 (2) |
O2—Y—C1 | 113.26 (10) | C3—C2—Y | 77.9 (2) |
O1i—Y—C5 | 148.55 (10) | C1—C2—H2 | 125.8 |
O1—Y—C5 | 85.94 (10) | C3—C2—H2 | 125.8 |
O2—Y—C5 | 116.14 (10) | Y—C2—H2 | 114.9 |
C1—Y—C5 | 30.46 (10) | C4—C3—C2 | 108.1 (3) |
O1i—Y—C8 | 109.27 (11) | C4—C3—Y | 74.2 (2) |
O1—Y—C8 | 82.67 (10) | C2—C3—Y | 72.4 (2) |
O2—Y—C8 | 130.98 (9) | C4—C3—H3 | 126.0 |
C1—Y—C8 | 106.34 (11) | C2—C3—H3 | 126.0 |
C5—Y—C8 | 85.25 (12) | Y—C3—H3 | 119.3 |
O1i—Y—C12 | 82.43 (10) | C3—C4—C5 | 107.8 (3) |
O1—Y—C12 | 85.48 (10) | C3—C4—Y | 76.6 (2) |
O2—Y—C12 | 111.75 (10) | C5—C4—Y | 72.2 (2) |
C1—Y—C12 | 133.70 (11) | C3—C4—H4 | 126.1 |
C5—Y—C12 | 115.50 (11) | C5—C4—H4 | 126.1 |
C8—Y—C12 | 30.25 (11) | Y—C4—H4 | 117.1 |
O1i—Y—C9 | 131.44 (11) | C4—C5—C1 | 108.5 (3) |
O1—Y—C9 | 109.33 (10) | C4—C5—Y | 77.8 (2) |
O2—Y—C9 | 110.47 (10) | C1—C5—Y | 74.65 (19) |
C1—Y—C9 | 103.21 (11) | C4—C5—H5 | 125.8 |
C5—Y—C9 | 74.04 (11) | C1—C5—H5 | 125.8 |
C8—Y—C9 | 30.10 (12) | Y—C5—H5 | 114.0 |
C12—Y—C9 | 49.83 (12) | C1—C6—C7 | 110.1 (3) |
O1i—Y—C10 | 114.06 (10) | C1—C6—H6A | 109.6 |
O1—Y—C10 | 131.59 (10) | C7—C6—H6A | 109.6 |
O2—Y—C10 | 82.89 (9) | C1—C6—H6B | 109.6 |
C1—Y—C10 | 127.15 (11) | C7—C6—H6B | 109.6 |
C5—Y—C10 | 96.73 (11) | H6A—C6—H6B | 108.2 |
C8—Y—C10 | 49.71 (11) | O1—C7—C6 | 111.1 (3) |
C12—Y—C10 | 49.79 (12) | O1—C7—H7A | 109.4 |
C9—Y—C10 | 30.11 (10) | C6—C7—H7A | 109.4 |
O1i—Y—C11 | 85.35 (10) | O1—C7—H7B | 109.4 |
O1—Y—C11 | 114.19 (11) | C6—C7—H7B | 109.4 |
O2—Y—C11 | 83.75 (9) | H7A—C7—H7B | 108.0 |
C1—Y—C11 | 152.71 (10) | C9—C8—C12 | 108.4 (3) |
C5—Y—C11 | 123.47 (11) | C9—C8—Y | 75.5 (2) |
C8—Y—C11 | 49.63 (10) | C12—C8—Y | 75.3 (2) |
C12—Y—C11 | 30.03 (11) | C9—C8—H8 | 125.8 |
C9—Y—C11 | 49.66 (11) | C12—C8—H8 | 125.8 |
C10—Y—C11 | 30.12 (12) | Y—C8—H8 | 115.6 |
O1i—Y—C2 | 107.90 (10) | C8—C9—C10 | 108.0 (3) |
O1—Y—C2 | 86.48 (10) | C8—C9—Y | 74.40 (19) |
O2—Y—C2 | 83.54 (9) | C10—C9—Y | 75.33 (19) |
C1—Y—C2 | 30.13 (10) | C8—C9—H9 | 126.0 |
C5—Y—C2 | 49.61 (11) | C10—C9—H9 | 126.0 |
C8—Y—C2 | 134.23 (11) | Y—C9—H9 | 116.4 |
C12—Y—C2 | 163.63 (11) | C9—C10—C11 | 107.7 (3) |
C9—Y—C2 | 120.58 (12) | C9—C10—Y | 74.56 (19) |
C10—Y—C2 | 130.78 (12) | C11—C10—Y | 74.94 (19) |
C11—Y—C2 | 158.72 (12) | C9—C10—H10 | 126.2 |
O1i—Y—C4 | 153.91 (11) | C11—C10—H10 | 126.2 |
O1—Y—C4 | 114.80 (10) | Y—C10—H10 | 116.5 |
O2—Y—C4 | 87.92 (10) | C12—C11—C10 | 108.2 (3) |
C1—Y—C4 | 49.73 (11) | C12—C11—Y | 74.4 (2) |
C5—Y—C4 | 29.99 (11) | C10—C11—Y | 74.9 (2) |
C8—Y—C4 | 96.80 (12) | C12—C11—H11 | 125.9 |
C12—Y—C4 | 123.00 (11) | C10—C11—H11 | 125.9 |
C9—Y—C4 | 73.23 (12) | Y—C11—H11 | 116.8 |
C10—Y—C4 | 83.32 (12) | C11—C12—C8 | 107.7 (3) |
C11—Y—C4 | 113.43 (11) | C11—C12—Y | 75.5 (2) |
C2—Y—C4 | 49.09 (11) | C8—C12—Y | 74.5 (2) |
O1i—Y—C3 | 124.75 (10) | C11—C12—H12 | 126.1 |
O1—Y—C3 | 114.83 (10) | C8—C12—H12 | 126.1 |
O2—Y—C3 | 68.62 (9) | Y—C12—H12 | 116.0 |
C1—Y—C3 | 49.30 (10) | O2—C13—H13A | 109.5 |
C5—Y—C3 | 48.93 (11) | O2—C13—H13B | 109.5 |
C8—Y—C3 | 125.98 (12) | H13A—C13—H13B | 109.5 |
C12—Y—C3 | 149.75 (11) | O2—C13—H13C | 109.5 |
C9—Y—C3 | 100.62 (12) | H13A—C13—H13C | 109.5 |
C10—Y—C3 | 102.12 (12) | H13B—C13—H13C | 109.5 |
C11—Y—C3 | 129.05 (11) | O2—C14—C15 | 111.1 (3) |
C2—Y—C3 | 29.69 (10) | O2—C14—H14A | 109.4 |
C4—Y—C3 | 29.20 (11) | C15—C14—H14A | 109.4 |
O1i—Y—Yi | 34.71 (6) | O2—C14—H14B | 109.4 |
O1—Y—Yi | 34.46 (5) | C15—C14—H14B | 109.4 |
O2—Y—Yi | 107.93 (6) | H14A—C14—H14B | 108.0 |
C1—Y—Yi | 93.45 (7) | O3—C15—C14 | 108.9 (3) |
C5—Y—Yi | 118.25 (8) | O3—C15—H15A | 109.9 |
C8—Y—Yi | 97.01 (9) | C14—C15—H15A | 109.9 |
C12—Y—Yi | 82.66 (8) | O3—C15—H15B | 109.9 |
C9—Y—Yi | 127.03 (9) | C14—C15—H15B | 109.9 |
C10—Y—Yi | 130.63 (9) | H15A—C15—H15B | 108.3 |
C11—Y—Yi | 101.57 (8) | O3—C16—H16A | 109.5 |
C2—Y—Yi | 98.55 (8) | O3—C16—H16B | 109.5 |
C4—Y—Yi | 143.06 (8) | H16A—C16—H16B | 109.5 |
C3—Y—Yi | 126.94 (7) | O3—C16—H16C | 109.5 |
C7—O1—Yi | 127.9 (2) | H16A—C16—H16C | 109.5 |
C7—O1—Y | 118.9 (2) | H16B—C16—H16C | 109.5 |
Yi—O1—Y | 110.83 (9) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Y2(C5H5)2(C7H8O)2(C4H10O2)2] |
Mr | 704.51 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 173 |
a, b, c (Å) | 8.6073 (2), 11.2146 (1), 15.7840 (1) |
β (°) | 92.751 (1) |
V (Å3) | 1521.83 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 3.84 |
Crystal size (mm) | 0.40 × 0.38 × 0.30 |
Data collection | |
Diffractometer | Siemens SMART CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.448, 0.659 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11359, 3482, 2489 |
Rint | 0.081 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.045, 0.088, 1.01 |
No. of reflections | 3482 |
No. of parameters | 183 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.59, −0.47 |
Computer programs: SMART (Siemens, 1995), SAINT (Siemens, 1995), SAINT, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ZORTEP (Zsolnai, Pritzkow, 1994), SHELXL97.
Y—Cg1 | 2.4537 (19) | Y—C4 | 2.761 (4) |
Y—Cg2 | 2.4260 (17) | Y—C5 | 2.690 (3) |
Y—O1i | 2.265 (2) | Y—C8 | 2.690 (4) |
Y—O1 | 2.280 (2) | Y—C9 | 2.704 (3) |
Y—O2 | 2.481 (2) | Y—C10 | 2.714 (3) |
Y—C1 | 2.687 (3) | Y—C11 | 2.714 (3) |
Y—C2 | 2.722 (4) | Y—C12 | 2.700 (4) |
Y—C3 | 2.792 (4) | ||
Cg1—Y—Cg2 | 120.80 (6) | Cg2—Y—O1i | 105.33 (7) |
Cg1—Y—O1 | 94.49 (7) | Cg2—Y—O2 | 104.72 (7) |
Cg1—Y—O1i | 133.80 (7) | O1i—Y—O1 | 69.17 (9) |
Cg1—Y—O2 | 93.85 (7) | O1i—Y—O2 | 75.83 (8) |
Cg2—Y—O1 | 105.56 (7) | O1—Y—O2 | 138.45 (8) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
The title compound, (I), possesses crystallographically imposed inversion symmetry. Both Y atoms of the dimeric complex are bridged by the two O atoms of the 2-(cyclopentadienyl)ethoxy ligands. The metal centers are coordinated to two cyclopentadienyl rings and three O atoms, two cyclopentadienylethoxide O atoms and one O atom of the dme ligand. The coordination geometry around each Y atom corresponds to a distorted trigonal bipyramid. The distances of the metal centers to the bridging O atoms are longer than those reported for the dimeric alkoxides [(Me3SiC5H4)2Y(µ-OMe)]2 [2.217 (3) and 2.233 (3) Å; Evans et al., 1992] and [(MeC5H4)2Y(µ-OiPr)]2 [2.2228 (19) and 2.2432 (19) Å; Li et al., 2000], but comparable with the values found in [(MeC5H4)2Y(µ-OCH═CH2)]2 [2.275 (3) and 2.290 (3) Å; Evans et al., 1986].
Only one O atom of the bidentate 1,2-dimethoxyethane (dme) ligand is coordinated to the metal center. Compared to the Y—O bond lengths of the alkoxide O atoms, the distance between the metal center and the dme O atom is much longer. A similar value was observed for the Y—O distance to THF in Cp3Y(THF) [2.451 (4) Å; Rogers et al., 1981]. A shorter distance was reported for the alkoxide (Cp*2Y)2(µ-OCH2CH2O)(THF)2 [Y—OTHF 2.398 (5) Å; Deelman et al., 1995].
The distances of the Y atom to the cyclopentadienyl-ring centroids are in good agreement with the distances found in Cp3Y(THF) (2.438, 2.453 and 2.454 Å; Rogers et al., 1981).
The O—Y—Oi [symmetry code: (i) 1 − x, 1 − y, 1 − z] bond angle of the central Y2O2 ring is somewhat smaller than in the above described alkoxide complexes [(Me3SiC5H4)2Y(µ-OMe)]2 [73.6 (1)°; Evans et al., 1992, [(MeC5H4)2Y(µ-O-iPr)]2 (74.86 (7)°) (Li et al., 2000) and [(MeC5H4)2Y(µ-OCH═CH2)]2 (73.1 (1)°) (Evans et al., 1986). The Y2O2 ring is perfectly planar.
Due to the trigonal bipyramidal coordination geometry of the metal atom the angle formed by the central yttrium atom and the two ring centroids is smaller than in the related tetrahedral complex [(MeC5H4)2Y(µ-OiPr)]2 (124.0°; Li et al., 2000).