Ab initio structure determination of [Eu₅(C₂H₄O₂)₆(CH₃CO₂)₃]_n by X-ray powder diffraction

The compound [Eu₅(C₂H₄O₂)₆(CH₃CO₂)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 ų 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 ų, which is of potential interest for gas storage.

Computing details

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.

(I)

Crystal data

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) Å^3	white
Z = 32	cylinder, × 0.5 mm
F(000) = 19200

Data collection

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

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 (Ų)

	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)

Eu1—O4^i	2.487 (12)	Eu3—O14^vii	2.394 (11)
Eu1—O5^ii	2.381 (11)	Eu3—O14^viii	2.394 (9)
Eu1—O8	2.355 (12)	Eu3—O14^ix	2.394 (11)
Eu1—O14^iii	2.648 (12)	Eu3—O14^x	2.394 (11)
Eu1—O14^iv	2.708 (14)	Eu3—O14^xi	2.394 (9)
Eu1—O15	2.610 (11)	Eu3—O14^xii	2.394 (11)
Eu1—O15^iv	2.320 (12)	C2—C3	1.502 (15)
Eu2—O4^v	2.229 (12)	C2—O5	1.409 (13)
Eu2—O4^ii	2.230 (12)	C3—O4	1.439 (18)
Eu2—O5^v	2.380 (9)	C6—C7	1.545 (17)
Eu2—O5^ii	2.380 (9)	C7—O8	1.33 (2)
Eu2—O9	2.287 (14)	C7—O9	1.38 (2)
Eu2—O9^vi	2.287 (13)	C12—C13	1.493 (17)
Eu2—O15	2.697 (11)	C12—O15	1.479 (16)
Eu2—O15^vi	2.697 (11)	C13—O14	1.488 (16)
O5···O15^xiii	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.