Abstract
C50H38F18Lu2O16, monoclinic, C2/c (no. 15), a = 15.7024(12) Å, b = 12.6169(10) Å, c = 29.715(2) Å, β = 91.919(10)°, V = 5883.7(8) Å3, Z = 4, Rgt(F) = 0.0273, wRref(F2) = 0.066, T = 273 K.
The crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.
Data collection and handling.
| Crystal: | Block, colorless |
| Size: | 0.32 × 0.32 × 0.30 mm |
| Wavelength: | Mo Kα radiation (0.71073 Å) |
| μ: | 3.46 mm−1 |
| Diffractometer, scan mode: | Bruker APEX2, φ and ω-scans |
| 2θmax, completeness: | 28.3°, 97.1% |
| N(hkl)measured, N(hkl)unique, Rint: | 23077, 7247, 0.016 |
| Criterion for Iobs, N(hkl)gt: | Iobs > 2 σ(Iobs), 6388 |
| N(param)refined: | 445 |
| Programs: | Bruker programs [1], SHELX [2] |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).
| Atom | x | y | z | Uiso*/Ueq |
|---|---|---|---|---|
| Lu1 | 0.08988(2) | 0.22420(2) | 0.37582(2) | 0.03603(5) |
| O1 | 0.23313(15) | 0.20960(19) | 0.38860(8) | 0.0475(6) |
| O2 | 0.14349(14) | 0.16603(18) | 0.31086(7) | 0.0422(5) |
| O3 | 0.13601(17) | 0.37220(19) | 0.41200(8) | 0.0513(6) |
| O4 | 0.06174(15) | 0.35881(16) | 0.32652(7) | 0.0411(5) |
| O5 | 0.11593(15) | 0.05166(19) | 0.39545(9) | 0.0497(6) |
| O6 | −0.01857(14) | 0.12852(17) | 0.34312(8) | 0.0429(5) |
| O7 | 0.0638(2) | 0.2006(2) | 0.45440(9) | 0.0645(7) |
| O8 | −0.04543(16) | 0.3006(2) | 0.39911(10) | 0.0627(7) |
| F1 | 0.42648(19) | 0.0788(4) | 0.38025(12) | 0.1242(14) |
| F2 | 0.40274(19) | 0.2310(3) | 0.40830(13) | 0.1016(11) |
| F3 | 0.3543(2) | 0.0952(3) | 0.43786(11) | 0.1065(11) |
| F4Aa | 0.2372(7) | 0.6149(6) | 0.4150(4) | 0.126(4) |
| F5Aa | 0.1420(5) | 0.5741(8) | 0.4619(3) | 0.166(4) |
| F6Aa | 0.2512(6) | 0.4819(6) | 0.4586(3) | 0.125(3) |
| F5Bb | 0.1850(8) | 0.5127(9) | 0.4741(3) | 0.106(3) |
| F4Bb | 0.2094(8) | 0.6302(7) | 0.4255(4) | 0.083(3) |
| F6Bb | 0.2869(5) | 0.4924(8) | 0.4308(3) | 0.097(3) |
| F7Ac | 0.0901(7) | −0.2211(6) | 0.3951(4) | 0.134(5) |
| F8Ac | 0.2026(4) | −0.1277(7) | 0.4064(4) | 0.122(3) |
| F9Ac | 0.1109(7) | −0.1266(8) | 0.4526(3) | 0.156(3) |
| F7Bd | 0.1719(5) | −0.1777(6) | 0.3695(2) | 0.096(2) |
| F8Bd | 0.1862(6) | −0.1127(6) | 0.4338(3) | 0.089(3) |
| F9Bd | 0.0786(5) | −0.2047(7) | 0.4190(3) | 0.078(3) |
| C1 | 0.3688(2) | 0.1382(4) | 0.39841(14) | 0.0607(10) |
| C2 | 0.2862(2) | 0.1503(3) | 0.37035(12) | 0.0447(7) |
| C3 | 0.2786(2) | 0.0970(3) | 0.33010(12) | 0.0476(8) |
| H3 | 0.3233 | 0.0545 | 0.3211 | 0.057* |
| C4 | 0.2044(2) | 0.1056(2) | 0.30213(11) | 0.0394(6) |
| C5 | 0.19455(19) | 0.0414(3) | 0.26000(11) | 0.0397(7) |
| C6 | 0.2453(2) | −0.0468(3) | 0.25176(13) | 0.0513(8) |
| H6 | 0.2898 | −0.0643 | 0.2719 | 0.062* |
| C7 | 0.2299(2) | −0.1083(3) | 0.21387(14) | 0.0583(10) |
| H7 | 0.2641 | −0.1668 | 0.2085 | 0.070* |
| C8 | 0.1640(2) | −0.0831(3) | 0.18399(13) | 0.0511(8) |
| H8 | 0.1538 | −0.1250 | 0.1586 | 0.061* |
| C9 | 0.11228(19) | 0.0048(3) | 0.19141(11) | 0.0405(7) |
| C10 | 0.12899(19) | 0.0671(3) | 0.22923(11) | 0.0401(7) |
| H10 | 0.0959 | 0.1269 | 0.2341 | 0.048* |
| C11 | 0.2006(3) | 0.5310(3) | 0.43326(17) | 0.0874(18) |
| C12 | 0.1489(2) | 0.4647(3) | 0.39897(12) | 0.0471(8) |
| C13 | 0.1231(2) | 0.5116(3) | 0.35913(13) | 0.0527(9) |
| H13 | 0.1379 | 0.5820 | 0.3542 | 0.063* |
| C14 | 0.0751(2) | 0.4577(2) | 0.32538(10) | 0.0391(6) |
| C15 | 0.0372(2) | 0.5177(3) | 0.28643(11) | 0.0449(7) |
| C16 | 0.0000 | 0.4641(3) | 0.2500 | 0.0394(9) |
| H16 | 0.0000 | 0.3904 | 0.2500 | 0.047* |
| C17 | 0.0371(4) | 0.6280(3) | 0.28584(14) | 0.0843(17) |
| H17 | 0.0622 | 0.6651 | 0.3098 | 0.101* |
| C18 | 0.0000 | 0.6831(6) | 0.2500 | 0.0842(19) |
| H18 | 0.0000 | 0.7568 | 0.2500 | 0.101* |
| C19 | 0.1251(3) | −0.1312(4) | 0.40545(19) | 0.0801(16) |
| C20 | 0.0797(2) | −0.0335(3) | 0.38638(12) | 0.0466(8) |
| C21 | 0.0070(2) | −0.0508(3) | 0.36027(15) | 0.0570(10) |
| H21 | −0.0128 | −0.1198 | 0.3564 | 0.068* |
| C22 | −0.03807(19) | 0.0325(3) | 0.33928(11) | 0.0396(7) |
| C23 | 0.1333(4) | 0.1736(6) | 0.48481(16) | 0.1012(19) |
| H23A | 0.1660 | 0.2360 | 0.4919 | 0.152* |
| H23B | 0.1690 | 0.1222 | 0.4709 | 0.152* |
| H23C | 0.1114 | 0.1445 | 0.5119 | 0.152* |
| C24 | 0.0054(4) | 0.2744(5) | 0.47369(17) | 0.0876(16) |
| H24A | 0.0310 | 0.3443 | 0.4759 | 0.105* |
| H24B | −0.0092 | 0.2516 | 0.5036 | 0.105* |
| C25 | −0.0715(3) | 0.2772(5) | 0.4437(2) | 0.0909(17) |
| H25A | −0.1004 | 0.2093 | 0.4442 | 0.109* |
| H25B | −0.1105 | 0.3312 | 0.4538 | 0.109* |
| C26 | −0.1165(3) | 0.3157(5) | 0.3684(2) | 0.0860(15) |
| H26A | −0.1503 | 0.2523 | 0.3671 | 0.129* |
| H26B | −0.0962 | 0.3312 | 0.3390 | 0.129* |
| H26C | −0.1506 | 0.3736 | 0.3785 | 0.129* |
Occupancies: a = 0.59; b = 0.41; c = 0.55, d = 0.45
Source of material
The title compound is easily synthesized by means of reported procedures [3]. To a methanol solution of 1,3-bis(4,4,4-trifluoro-1,3-dioxobutyl)phenyl (1 g, 2.8 mmol), NaOH (0.2 g, 5.6 mmol) was added, and the mixture was allowed to stir for 5 min. To this methanol solution, LuCl3⋅6H2O (1.86 mmol) was added, and the mixture was allowed to stir for 24 h at ambient temperature. Water was then added to this mixture, and the precipitate thus formed was filtered, washed with water, and dried in air to give the title compound in a yield of 62.1%. Crystals were obtained in about two weeks by recrystallization from DME/hexane.
Experimental details
All H atoms on C atoms were placed in idealized positions [C—H = 0.96 (methyl), 0.97 (methylene) and 0.93 Å (aromatic)] and included in the refinement in the riding-model approximation, with Uiso(H) = 1.5Ueq(methyl C) and 1.2Ueq(methylene and aromatic C). The F4, F5 and F6 atoms are disordered (cf. table 2). The non-hydrogen atoms in the structure of the title complex were refined with anisotropic displacement parameters.
Discussion
Lutetium(III) complexes have wide range applications in catalysis in the past few years [4], [5], [6]. Some directly related structures of the title structure have been reported [3, 7–8]. In the title crystal structure, the bond distances and bond angles are all in normal range [9]. The crystal structure features weak intermolecular C—H⋯F and C—H⋯O hydrogen bonds.
Acknowledgement
We are grateful for financial support by the Education Department of Hei longjiang Province of China (no. 12521413).
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©2017 WeiCan Zhao et al., published by De Gruyter, Berlin/Boston
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