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The compound [Eu
5(C
2H
4O
2)
6(CH
3CO
2)
3]
n was synthesized by dissolving acetate europium salt in ethylene glycol solvent and heating under reflux for a short time. Its structure was solved
ab initio from synchrotron powder diffraction data using optimization methods in direct space. The compound has a very large unit-cell volume of 23679 Å
3 and the highest centred cubic symmetry space group,
(No. 230). The porous metal–organic framework structure is similar to those usually observed in zeolites, with pores volumes of 82 Å
3, which is of potential interest for gas storage.
Supporting information
CCDC reference: 1867704
Program(s) used to solve structure: FOX; program(s) used to refine structure: FULLPROF; molecular graphics: DIAMOND; software used to prepare material for publication: WORD.
Crystal data top
C18H33Eu5O18 | Dx = 2.912 Mg m−3 |
Mr = 1297.29 | Synchrotron radiation, λ = 0.776651 Å |
Cubic, Ia3d | µ = 13.20 mm−1 |
Hall symbol: -I 4bd 2c 3 | T = 293 K |
a = 28.7121 (3) Å | Particle morphology: plate-like |
V = 23669.7 (4) Å3 | white |
Z = 32 | cylinder, × 0.5 mm |
F(000) = 19200 | |
Data collection top
CRISTAL Beamline, SOLEIL diffractometer | Data collection mode: transmission |
Radiation source: CRISTAL Beamline, SOLEIL | Scan method: step |
Specimen mounting: powder in a glass capillary | 2θmin = 2.007°, 2θmax = 60.006°, 2θstep = 0.004° |
Refinement top
Rp = 0.026 | Profile function: pseudo-Voigt |
Rwp = 0.029 | 53 parameters |
Rexp = 0.004 | 16 restraints |
RBragg = 0.076 | H-atom parameters not refined |
16112 data points | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Eu1 | 0.08552 (5) | 0.89895 (5) | 0.99515 (5) | 0.0450 (3)* | |
Eu2 | 0.13950 (5) | 0.88951 (5) | 0.87500 | 0.0494 (6)* | |
Eu3 | 0.00000 | 0.00000 | 0.00000 | 0.0460 (10)* | |
C2 | 0.0685 (7) | 0.0289 (4) | 0.8082 (3) | 0.026 (3)* | |
H2A | 0.03840 | 0.01333 | 0.80632 | 0.02596* | |
H2B | 0.09279 | 0.00621 | 0.80331 | 0.02596* | |
C3 | 0.0713 (6) | 0.0671 (4) | 0.7726 (4) | 0.026 (3)* | |
H3A | 0.08312 | 0.05411 | 0.74357 | 0.02596* | |
H3B | 0.04020 | 0.07885 | 0.76639 | 0.02596* | |
O4 | 0.1005 (4) | 0.1054 (4) | 0.7860 (4) | 0.026 (3)* | |
O5 | 0.0736 (4) | 0.0514 (4) | 0.8515 (3) | 0.026 (3)* | |
C6 | 0.0651 (8) | 0.7565 (4) | 0.9322 (7) | 0.074 (4)* | |
H6A | 0.09267 | 0.74190 | 0.91897 | 0.07530* | |
H6B | 0.03989 | 0.75309 | 0.91059 | 0.07530* | |
H6C | 0.05767 | 0.74135 | 0.96087 | 0.07530* | |
C7 | 0.0751 (6) | 0.8088 (4) | 0.9407 (7) | 0.074 (4)* | |
O8 | 0.0474 (4) | 0.8304 (4) | 0.9710 (4) | 0.074 (4)* | |
O9 | 0.1135 (4) | 0.8306 (5) | 0.9216 (5) | 0.074 (4)* | |
C12 | 0.0198 (4) | 0.9164 (4) | 0.8947 (7) | 0.057 (3)* | |
H12A | 0.00441 | 0.90075 | 0.91693 | 0.05637* | |
H12B | 0.02394 | 0.89679 | 0.86787 | 0.05637* | |
C13 | −0.0060 (6) | 0.9597 (3) | 0.8822 (5) | 0.057 (3)* | |
H13A | 0.00361 | 0.97015 | 0.85122 | 0.05637* | |
H13B | −0.03637 | 0.95472 | 0.88212 | 0.05637* | |
O14 | 0.0072 (5) | 0.9958 (4) | 0.9166 (4) | 0.057 (3)* | |
O15 | 0.0652 (3) | 0.9327 (5) | 0.9129 (4) | 0.057 (3)* | |
Geometric parameters (Å, º) top
Eu1—O4i | 2.487 (12) | Eu3—O14vii | 2.394 (11) |
Eu1—O5ii | 2.381 (11) | Eu3—O14viii | 2.394 (9) |
Eu1—O8 | 2.355 (12) | Eu3—O14ix | 2.394 (11) |
Eu1—O14iii | 2.648 (12) | Eu3—O14x | 2.394 (11) |
Eu1—O14iv | 2.708 (14) | Eu3—O14xi | 2.394 (9) |
Eu1—O15 | 2.610 (11) | Eu3—O14xii | 2.394 (11) |
Eu1—O15iv | 2.320 (12) | C2—C3 | 1.502 (15) |
Eu2—O4v | 2.229 (12) | C2—O5 | 1.409 (13) |
Eu2—O4ii | 2.230 (12) | C3—O4 | 1.439 (18) |
Eu2—O5v | 2.380 (9) | C6—C7 | 1.545 (17) |
Eu2—O5ii | 2.380 (9) | C7—O8 | 1.33 (2) |
Eu2—O9 | 2.287 (14) | C7—O9 | 1.38 (2) |
Eu2—O9vi | 2.287 (13) | C12—C13 | 1.493 (17) |
Eu2—O15 | 2.697 (11) | C12—O15 | 1.479 (16) |
Eu2—O15vi | 2.697 (11) | C13—O14 | 1.488 (16) |
| | | |
O5···O15xiii | 2.608 (15) | | |
| | | |
C3—C2—O5 | 105.5 (12) | O8—C7—O9 | 121.2 (18) |
C2—C3—O4 | 113.9 (15) | C13—C12—O15 | 105.9 (15) |
C6—C7—O8 | 117.1 (17) | C12—C13—O14 | 108.3 (13) |
C6—C7—O9 | 121.4 (18) | | |
Symmetry codes: (i) −y+1/4, x+3/4, z+1/4; (ii) −z+1, −x+1, −y+1; (iii) y−1, z, x+1; (iv) −z+1, −x+1, −y+2; (v) −x+1/4, −z+7/4, y+3/4; (vi) y−3/4, x+3/4, −z+7/4; (vii) x, y−1, z−1; (viii) y−1, z−1, x; (ix) z−1, x, y−1; (x) −x, −y+1, −z+1; (xi) −y+1, −z+1, −x; (xii) −z+1, −x, −y+1; (xiii) −y+1, −z+1, −x+1. |
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