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Acta Crystallographica Section E: Crystallographic Communications logoLink to Acta Crystallographica Section E: Crystallographic Communications
. 2016 Mar 4;72(Pt 4):448–451. doi: 10.1107/S2056989016003546

Crystal structure of octa­kis­(N,N-di­methyl­formamide-κO)europium(III) tetra­cosa-μ2-oxido-dodeca­oxido-μ12-phosphato-dodeca­molybdate(VI)

Yassine Ghandour a,*, Imen Hammami a, Shabir Najmudin b, Cecilia Bonifácio c, Mohamed Salah Belkhiria a
PMCID: PMC4910337  PMID: 27375861

The asymmetric unit of the title compound consists of one [Eu(C3H7NO)8]3+ complex cation and one α-Keggin-type [PMo12O40] polyanion. Cations and anions are linked through C—H⋯O hydrogen bonds.

Keywords: crystal structure, α-Keggin-type [PMo12O40]3− polyanion, europium, IR spectroscopy

Abstract

In the title salt, [Eu(C3H7NO)8][PMo12O40], the asymmetric unit comprises one α-Keggin-type [PMo12O40]3− polyoxidometalate anion and one distorted dodeca­hedral [Eu(C3H7NO)8]3+ complex cation. In the crystal, the isolated polyoxidometalate anions are packed into hexa­gonally arranged rows extending parallel to [001]. The complex cations are situated between the rows and are linked to the neighbouring anions through weak C—H⋯O hydrogen-bonding inter­actions, leading to the formation of a three-dimensional network structure.

Chemical context  

Polyoxidometalates (POMs) are versatile metal–oxygen complexes which have attracted inter­est due to their topolog­ical properties and their potential applications in catalysis, photoluminescence, electrochromism and magnetism (Long et al., 2010; Pope & Müller, 2010; Coronado & Gómez-García, 1998). Up to date, a variety of strategies have been developed and used to assemble POM-based hybrid materials by controlling reaction factors such as metal ions, organic ligands, POM species, pH, molar ratio of raw materials or reaction environments (Wang et al., 2013; Liu et al., 2013). Even with these approaches, the design and synthesis of new stable polyoxidomolybdate complexes are still challenging.graphic file with name e-72-00448-scheme1.jpg

Herein, we report on the synthesis, UV–vis and IR spectra along with the crystal structure of the hybrid europium(III) POM title compound, [Eu(C3H7NO)8][PMo12O40], (I).

Structural commentary  

The structures of the mol­ecular components of compound (I) are illustrated in Fig. 1. The [PMo12O40]3− polyoxidoanion of (I) exhibits a classical α-Keggin-type structure. The central P atom is tetra­hedrally surrounded with all four oxygen atoms (Oa) linked to four Mo3O13 moieties. The latter species are fused together by sharing corner atoms (Ob) and consist of three MoO6 octa­hedra condensed in a triangular arrangement by sharing edges (Oc). There is also a terminal oxygen atom (Od) in every MoO6 octa­hedron. The P—O bond lengths range from 1.521 (5) Å to 1.536 (4) Å and the Mo—O bond lengths from 1.690 (5) Å to 2.438 (4) Å. The O—P—O angles [109.1 (2)–109.8 (3)°] indicate only a slight distortion of the central PO4 tetra­hedron. The EuIII cation is coordinated by eight di­methyl­formamide ligands through their oxygen atoms with Eu—O distances from 2.369 (5) to 2.416 (6) Å. These values are comparable to those of related oxido-europium(III) species, e.g for the [Eu(thd)3(DMF)2] complex (thd is the ion of 2,2,6,6-tetra­methyl-3,5-hepta­nedione) with Eu—O = 2.494 (5)–2.442 (5) Å (Cunningham & Siever, 1980). Calculations with the SHAPE software (Alvarez et al., 2005) indicate that the coordination polyhedron of EuIII is a slightly distorted dodeca­hedron approaching mol­ecular D 2d symmetry (Casanova et al., 2005).

Figure 1.

Figure 1

The mol­ecular structures of the cation and anion in compound (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 40% probability level. H atoms have been omitted for clarity.

Supra­molecular features  

The unit cell content of the title compound is illustrated in Fig. 2. In the crystal structure of (I), each [Eu(DMF)8]3+ cation is linked to four neighbouring α-Keggin-type [PMo12O40]3− anions through C—H⋯O hydrogen-bonding inter­actions between the methyl groups of the DMF ligands and the terminal-oxygen (Od) and the bridging-oxygen atoms (Ob,c) of the [PMo12O40]3− anions (Fig. 3, Table 1). The C(donor)⋯Od(acceptor) distances are between 3.174 (10) and 3.541 (11) Å while the C⋯O(b,c) distances are between 3.289 (11) and 3.473 (12) Å. In the crystal packing, the POM anions are packed into hexa­gonally arranged rows extending parallel to [001] with the [Eu(DMF)8]3+ cations located between the rows (Fig. 4).

Figure 2.

Figure 2

The contents of the unit cell of complex (I). H atoms have been omitted for clarity.

Figure 3.

Figure 3

C—H⋯O hydrogen bonds (dashed lines) link one [Eu(dmf)8]3+ cation to four neighbouring α-Keggin-type [PMo12O40]3− anions. Symmetry codes refer to Table 1.

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A D—H H⋯A DA D—H⋯A
C3—H4⋯O31i 0.96 2.72 3.289 (11) 118
C4—H7⋯O36ii 0.96 2.61 3.476 (12) 150
C7—H13⋯O7 0.96 2.65 3.473 (12) 145
C8—H15⋯O28ii 0.96 2.51 3.316 (13) 141
C8—H16⋯O5 0.96 2.58 3.424 (11) 147
C10—H18⋯O28ii 0.93 2.62 3.516 (10) 162
C15—H29⋯O16i 0.96 2.55 3.299 (12) 135
C15—H27⋯O32iii 0.96 2.52 3.440 (10) 160
C15—H28⋯O52iv 0.96 2.29 3.174 (10) 153
C16—H31⋯O6iii 0.96 2.63 3.541 (11) 159
C22—H41⋯O55 0.96 2.53 3.280 (12) 135
C22—H42⋯O11iv 0.96 2.45 3.305 (11) 149
C22—H43⋯O45 0.96 2.61 3.567 (13) 172
C23—H44⋯O17v 0.96 2.52 3.443 (11) 161
C25—H55⋯O24 0.93 2.53 3.337 (11) 145
C25—H55⋯O44 0.93 2.58 3.091 (10) 115
C28—H56⋯O36v 0.93 2.62 3.476 (11) 153
C30—H60⋯O36v 0.96 2.58 3.458 (14) 152

Symmetry codes: (i) Inline graphic; (ii) Inline graphic; (iii) Inline graphic; (iv) Inline graphic; (v) Inline graphic.

Figure 4.

Figure 4

The crystal packing of (I) with the [PMo12O40]3− anions in polyhedral representation.

Synthesis and crystallization  

The starting material [(C4H9)4N)4H3][PMo11O39] was prepared using a literature method (Combs-Walker & Hill, 1998). EuCl3·6H2O (361.41 mg, 1 mmol) and isonicotinic acid (C6H5NO2) (123.11 mg, 1 mmol) were dissolved in 10 ml of di­methyl­formamide. This solution was added dropwise to a yellow di­methyl­formamide solution of [(C4H9)4N)4H3][PMo11O39] (0.33 mmol in 10 ml). The mixture was heated under stirring for 1 h at 333 K. Single crystals of the title compounds were obtained by slow diffusion of 2-propanol through the di­methyl­formamide solution. UV–vis spectrum in di­methyl­formamide: λmax (nm) 315 and 205.

FT–IR spectroscopy  

The FT–IR spectrum was recorded in the range 4000–400 cm−1 on a Nicolet 470 FT–IR spectrophotometer with pressed KBr pellets.

The FT–IR spectrum of (I) (Fig. 5) exhibits characteristic bands attributed to the stretching and deformation modes of the Mo—O bond vibration of the [PMo12O40]3− anion in the region 1100–400 cm−1 . Thus, the asymmetric vibration νas(P—Oa), νas(Mo=Od), νas(Mo—Ob—Mo) and νas(Mo—Oc—Mo) appear at 1065, 951, 885 and 974 cm−1, respectively (Masteri-Farahani & Shahbazi, 2012). The absorption bands at 1265 and 1657 cm−1 are characteristic of the asymmetric vibration of the C—N and the C=O bonds, respectively. The vibration bands at 1115, 1440, 1385 and 2964 cm−1 are attributed to the vibration ρ(CH3) (rocking vibration), δa(CH3), δs(CH3) and ν(C-H) of the di­methyl­formamide ligand (Durgaprasad et al., 1971).

Figure 5.

Figure 5

The FT–IR spectrum of (I).

Refinement  

Crystal data, data collection and structure refinement details are summarized in Table 2. Hydrogen atoms were placed in calculated positions and refined as riding atoms: C—H = 0.93 Å and U iso(H) = 1.2U eq(C) for methine groups and C—H = 0.96 Å and U iso(H) = 1.5U eq(C) for methyl groups. The refined Flack parameter (Parsons et al., 2013) of −0.015 (7) indicates the correct determination of the absolute structure.

Table 2. Experimental details.

Crystal data
Chemical formula [Eu(C3H7NO)8][PMo12O40]
M r 2558.97
Crystal system, space group Orthorhombic, P n a21
Temperature (K) 296
a, b, c (Å) 26.9108 (10), 18.3506 (6), 13.4494 (4)
V3) 6641.7 (4)
Z 4
Radiation type Mo Kα
μ (mm−1) 3.24
Crystal size (mm) 0.20 × 0.18 × 0.17
 
Data collection
Diffractometer Bruker APEXII CCD
Absorption correction Multi-scan (SADABS; Bruker, 2006)
T min, T max 0.667, 0.747
No. of measured, independent and observed [I > 2σ(I)] reflections 88354, 33285, 19583
R int 0.075
(sin θ/λ)max−1) 0.849
 
Refinement
R[F 2 > 2σ(F 2)], wR(F 2), S 0.047, 0.095, 0.98
No. of reflections 33285
No. of parameters 863
No. of restraints 1
H-atom treatment H-atom parameters constrained
Δρmax, Δρmin (e Å−3) 2.08, −1.80
Absolute structure Flack x determined using 6924 quotients [(I +)−(I )]/[(I +)+(I )]
Absolute structure parameter −0.015 (7)

Computer programs: APEX2 and SAINT (Bruker, 2006), SIR2004 (Burla et al., 2005), SHELXL2014 (Sheldrick, 2015), ORTEP-3 for Windows (Farrugia, 2012), DIAMOND (Putz & Brandenburg, 2014) and WinGX (Farrugia, 2012).

Supplementary Material

Crystal structure: contains datablock(s) I. DOI: 10.1107/S2056989016003546/wm5274sup1.cif

e-72-00448-sup1.cif (2.6MB, cif)

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989016003546/wm5274Isup2.hkl

e-72-00448-Isup2.hkl (2.6MB, hkl)

CCDC reference: 1456619

Additional supporting information: crystallographic information; 3D view; checkCIF report

Acknowledgments

The authors gratefully acknowledge financial support from the Ministry of Higher Education and Scientific Research of Tunisia. The authors are grateful to the Portuguese Fundacão para a Ciencias e Tecnologia (FCT) for support through projects SFRH/BPD/24889/2005 and PTDC/BIAPRO/ 103980/2008 and for funding the purchase of the single-crystal diffractometer.

supplementary crystallographic information

Crystal data

[Eu(C3H7NO)8][PMo12O40] Dx = 2.559 Mg m3
Mr = 2558.97 Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pna21 Cell parameters from 9528 reflections
a = 26.9108 (10) Å θ = 3.0–32.3°
b = 18.3506 (6) Å µ = 3.24 mm1
c = 13.4494 (4) Å T = 296 K
V = 6641.7 (4) Å3 Prism, yellow
Z = 4 0.20 × 0.18 × 0.17 mm
F(000) = 4888

Data collection

Bruker APEXII CCD diffractometer 19583 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube Rint = 0.075
φ and ω scans θmax = 37.1°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2006) h = −41→45
Tmin = 0.667, Tmax = 0.747 k = −31→31
88354 measured reflections l = −21→22
33285 independent reflections

Refinement

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)] = 0.047 H-atom parameters constrained
wR(F2) = 0.095 w = 1/[σ2(Fo2) + (0.035P)2] where P = (Fo2 + 2Fc2)/3
S = 0.98 (Δ/σ)max = 0.001
33285 reflections Δρmax = 2.08 e Å3
863 parameters Δρmin = −1.80 e Å3
1 restraint Absolute structure: Flack x determined using 6924 quotients [(I+)-(I-)]/[(I+)+(I-)]
Primary atom site location: structure-invariant direct methods Absolute structure parameter: −0.015 (7)

Special details

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 > 2σ(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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

x y z Uiso*/Ueq
Eu1 0.62226 (2) 0.24667 (2) 0.27301 (3) 0.03117 (7)
Mo1 0.26680 (2) 0.18597 (3) 0.63650 (5) 0.03332 (13)
Mo2 0.30169 (2) 0.35458 (3) 0.55755 (5) 0.03366 (13)
Mo3 0.41829 (3) 0.43690 (3) 0.64996 (5) 0.03387 (13)
Mo4 0.47559 (2) 0.36195 (3) 0.85122 (5) 0.03004 (12)
Mo5 0.49335 (2) 0.20234 (3) 0.68682 (5) 0.03324 (13)
Mo6 0.39245 (3) 0.10613 (3) 0.60967 (5) 0.03505 (14)
Mo7 0.32991 (3) 0.10420 (3) 0.85410 (5) 0.03838 (15)
Mo8 0.43839 (3) 0.17833 (4) 0.93808 (5) 0.03661 (14)
Mo9 0.32843 (3) 0.26018 (4) 0.99282 (5) 0.04260 (17)
Mo10 0.36044 (2) 0.43617 (3) 0.87490 (5) 0.03517 (14)
Mo11 0.25072 (2) 0.33286 (4) 0.78760 (5) 0.03541 (14)
Mo12 0.42166 (3) 0.26738 (4) 0.49994 (5) 0.03432 (13)
P1 0.37299 (6) 0.26883 (8) 0.74508 (12) 0.0207 (3)
O1 0.6764 (2) 0.1551 (4) 0.2093 (5) 0.0526 (16)
O2 0.2228 (2) 0.1295 (3) 0.5946 (5) 0.0453 (14)
O3 0.26515 (19) 0.2607 (3) 0.5440 (4) 0.0350 (11)
O4 0.34964 (18) 0.4169 (3) 0.6033 (4) 0.0320 (10)
O5 0.47195 (19) 0.4273 (3) 0.7347 (4) 0.0325 (11)
O6 0.5310 (2) 0.3873 (3) 0.8969 (4) 0.0420 (13)
O7 0.49746 (19) 0.2908 (3) 0.7483 (4) 0.0330 (11)
O8 0.45951 (19) 0.1127 (2) 0.6394 (4) 0.0355 (11)
O9 0.32412 (19) 0.1439 (3) 0.5897 (4) 0.0333 (11)
O10 0.3722 (2) 0.0854 (3) 0.7370 (4) 0.0372 (12)
O11 0.3952 (2) 0.1009 (3) 0.9240 (4) 0.0407 (13)
O12 0.45956 (19) 0.2814 (3) 0.9252 (4) 0.0349 (11)
O13 0.3888 (2) 0.2209 (3) 1.0310 (4) 0.0420 (13)
O14 0.3515 (2) 0.3523 (3) 0.9652 (4) 0.0374 (12)
O15 0.30057 (19) 0.4081 (3) 0.8207 (4) 0.0337 (11)
O16 0.1992 (2) 0.3743 (4) 0.8289 (5) 0.0527 (16)
O17 0.25496 (19) 0.3787 (3) 0.6547 (4) 0.0363 (11)
O18 0.22650 (19) 0.2506 (3) 0.7233 (4) 0.0377 (12)
O19 0.32137 (16) 0.2804 (2) 0.7018 (3) 0.0231 (9)
O20 0.36948 (17) 0.2233 (2) 0.8397 (3) 0.0257 (9)
O21 0.39628 (16) 0.3431 (2) 0.7695 (3) 0.0241 (8)
O22 0.40539 (17) 0.2288 (2) 0.6696 (3) 0.0248 (9)
O23 0.35674 (19) 0.2989 (3) 0.5004 (4) 0.0344 (11)
O24 0.4401 (3) 0.2850 (4) 0.3828 (4) 0.0512 (15)
O25 0.43539 (19) 0.3610 (3) 0.5671 (4) 0.0342 (11)
O26 0.48598 (18) 0.2386 (3) 0.5597 (4) 0.0340 (11)
O27 0.4063 (2) 0.1693 (3) 0.4917 (4) 0.0349 (11)
O28 0.3447 (2) 0.5055 (3) 0.9514 (5) 0.0499 (15)
O29 0.38277 (19) 0.4838 (2) 0.7624 (4) 0.0361 (11)
O30 0.43123 (19) 0.4244 (3) 0.9129 (4) 0.0344 (11)
O31 0.3075 (2) 0.1592 (3) 0.9607 (4) 0.0440 (14)
O32 0.4708 (2) 0.1659 (3) 0.8178 (4) 0.0341 (11)
O33 0.4791 (3) 0.1462 (4) 1.0216 (5) 0.0547 (16)
O34 0.2843 (2) 0.1389 (3) 0.7637 (4) 0.0367 (11)
O35 0.4338 (2) 0.5098 (3) 0.5822 (5) 0.0488 (15)
O36 0.2790 (2) 0.3974 (3) 0.4560 (4) 0.0446 (14)
N1 0.6761 (3) 0.4097 (4) 0.0486 (6) 0.0457 (17)
N2 0.5963 (3) 0.3569 (4) 0.5746 (5) 0.0438 (16)
N3 0.7647 (3) 0.3614 (4) 0.3484 (6) 0.0437 (16)
N4 0.5971 (3) 0.1673 (3) −0.0459 (5) 0.0390 (15)
N5 0.4821 (3) 0.3901 (4) 0.2356 (6) 0.0476 (18)
O47 0.6329 (3) 0.1665 (4) 0.4103 (5) 0.0617 (19)
N7 0.6224 (3) 0.0801 (4) 0.5252 (5) 0.0400 (15)
N8 0.4832 (3) 0.1029 (4) 0.2582 (6) 0.0474 (17)
N9 0.7415 (3) 0.0838 (4) 0.1778 (6) 0.0471 (17)
O37 0.2743 (2) 0.2842 (3) 0.8971 (4) 0.0382 (12)
O38 0.2989 (3) 0.2710 (4) 1.1019 (4) 0.0632 (19)
O39 0.3086 (3) 0.0201 (3) 0.8810 (5) 0.0559 (17)
O55 0.5523 (2) 0.1732 (3) 0.6856 (5) 0.0459 (14)
O40 0.6550 (2) 0.3481 (3) 0.1859 (5) 0.0490 (14)
C2 0.6452 (3) 0.3714 (4) 0.1012 (7) 0.046 (2)
H8 0.6142 0.3609 0.0743 0.055*
C3 0.7237 (4) 0.4299 (5) 0.0907 (9) 0.061 (3)
H2 0.7185 0.4556 0.1520 0.092*
H3 0.7412 0.4606 0.0448 0.092*
H4 0.7429 0.3867 0.1032 0.092*
C4 0.6638 (5) 0.4329 (6) −0.0517 (7) 0.067 (3)
H6 0.6861 0.4101 −0.0980 0.101*
H7 0.6670 0.4849 −0.0564 0.101*
H5 0.6303 0.4191 −0.0668 0.101*
O41 0.6001 (3) 0.3175 (4) 0.4158 (5) 0.0580 (17)
C6 0.6147 (3) 0.3158 (5) 0.5037 (7) 0.051 (2)
H10 0.6400 0.2836 0.5200 0.062*
C7 0.6139 (4) 0.3522 (7) 0.6749 (7) 0.067 (3)
H12 0.6340 0.3092 0.6823 0.100*
H13 0.5861 0.3496 0.7195 0.100*
H11 0.6335 0.3945 0.6902 0.100*
C8 0.5581 (4) 0.4096 (6) 0.5489 (8) 0.068 (3)
H15 0.5724 0.4481 0.5099 0.102*
H16 0.5441 0.4297 0.6086 0.102*
H14 0.5324 0.3860 0.5112 0.102*
O42 0.7020 (2) 0.2798 (3) 0.3417 (5) 0.0472 (14)
C10 0.7180 (3) 0.3417 (4) 0.3558 (6) 0.0430 (18)
H18 0.6951 0.3774 0.3731 0.052*
C11 0.8025 (4) 0.3079 (6) 0.3206 (8) 0.062 (3)
H19 0.7881 0.2600 0.3203 0.093*
H20 0.8293 0.3093 0.3678 0.093*
H21 0.8151 0.3190 0.2555 0.093*
C12 0.7807 (4) 0.4351 (6) 0.3660 (9) 0.067 (3)
H22 0.7522 0.4657 0.3761 0.100*
H23 0.7992 0.4523 0.3096 0.100*
H24 0.8014 0.4365 0.4241 0.100*
O43 0.6047 (3) 0.2262 (3) 0.0990 (4) 0.0514 (15)
C14 0.5960 (3) 0.1715 (4) 0.0515 (6) 0.0422 (18)
H26 0.5881 0.1294 0.0866 0.051*
C15 0.5833 (4) 0.1013 (4) −0.0986 (6) 0.046 (2)
H28 0.5798 0.0620 −0.0519 0.069*
H29 0.6087 0.0894 −0.1461 0.069*
H27 0.5523 0.1088 −0.1325 0.069*
C16 0.6085 (4) 0.2314 (5) −0.1036 (7) 0.055 (2)
H31 0.5807 0.2641 −0.1021 0.082*
H30 0.6153 0.2175 −0.1710 0.082*
H32 0.6372 0.2551 −0.0759 0.082*
O44 0.5498 (2) 0.3180 (4) 0.2319 (5) 0.0528 (16)
C18 0.5248 (3) 0.3674 (4) 0.2680 (8) 0.0468 (19)
H34 0.5377 0.3907 0.3237 0.056*
C19 0.4532 (4) 0.4425 (5) 0.2893 (9) 0.065 (3)
H35 0.4220 0.4211 0.3081 0.098*
H36 0.4472 0.4842 0.2479 0.098*
H37 0.4709 0.4573 0.3478 0.098*
C20 0.4613 (6) 0.3597 (9) 0.1481 (9) 0.114 (6)
H39 0.4498 0.3982 0.1055 0.171*
H40 0.4338 0.3289 0.1656 0.171*
H38 0.4861 0.3316 0.1140 0.171*
C21 0.6486 (4) 0.1287 (5) 0.4775 (6) 0.0453 (19)
H47 0.6816 0.1349 0.4962 0.054*
C22 0.5722 (3) 0.0645 (5) 0.4960 (9) 0.058 (2)
H41 0.5499 0.0791 0.5481 0.087*
H42 0.5687 0.0132 0.4841 0.087*
H43 0.5645 0.0909 0.4364 0.087*
C23 0.6432 (4) 0.0379 (6) 0.6040 (8) 0.064 (3)
H44 0.6776 0.0503 0.6120 0.096*
H46 0.6403 −0.0130 0.5884 0.096*
H45 0.6257 0.0480 0.6646 0.096*
O45 0.5562 (2) 0.1600 (3) 0.2673 (5) 0.0503 (14)
C25 0.5106 (3) 0.1617 (4) 0.2671 (7) 0.0449 (19)
H55 0.4948 0.2066 0.2735 0.054*
C26 0.5044 (5) 0.0336 (5) 0.2361 (11) 0.088 (4)
H49 0.5385 0.0398 0.2165 0.133*
H51 0.4862 0.0111 0.1830 0.133*
H50 0.5029 0.0031 0.2941 0.133*
C27 0.4286 (4) 0.1112 (7) 0.2546 (9) 0.080 (4)
H52 0.4201 0.1618 0.2609 0.120*
H53 0.4139 0.0842 0.3081 0.120*
H54 0.4164 0.0930 0.1923 0.120*
C28 0.7155 (4) 0.1265 (5) 0.2333 (7) 0.050 (2)
H56 0.7275 0.1363 0.2968 0.060*
C29 0.7248 (4) 0.0661 (8) 0.0795 (9) 0.084 (4)
H58 0.7093 0.1081 0.0501 0.126*
H59 0.7012 0.0270 0.0829 0.126*
H57 0.7526 0.0514 0.0396 0.126*
C30 0.7896 (5) 0.0544 (8) 0.2084 (9) 0.088 (4)
H61 0.8144 0.0676 0.1603 0.132*
H62 0.7875 0.0023 0.2129 0.132*
H60 0.7985 0.0741 0.2721 0.132*
O52 0.3886 (3) 0.0253 (3) 0.5521 (5) 0.0571 (17)

Atomic displacement parameters (Å2)

U11 U22 U33 U12 U13 U23
Eu1 0.03342 (16) 0.02974 (14) 0.03036 (15) −0.00241 (13) −0.00034 (15) −0.00084 (15)
Mo1 0.0306 (3) 0.0302 (3) 0.0392 (3) −0.0058 (2) −0.0060 (3) −0.0007 (3)
Mo2 0.0306 (3) 0.0352 (3) 0.0352 (3) 0.0008 (2) −0.0079 (3) 0.0104 (3)
Mo3 0.0381 (3) 0.0250 (3) 0.0385 (3) −0.0063 (2) −0.0028 (3) 0.0059 (3)
Mo4 0.0258 (3) 0.0310 (3) 0.0333 (3) 0.0000 (2) −0.0034 (2) −0.0058 (3)
Mo5 0.0281 (3) 0.0369 (3) 0.0347 (3) 0.0098 (2) −0.0026 (3) −0.0085 (3)
Mo6 0.0397 (3) 0.0252 (3) 0.0403 (3) 0.0005 (2) 0.0023 (3) −0.0095 (3)
Mo7 0.0455 (4) 0.0297 (3) 0.0399 (4) −0.0055 (3) 0.0003 (3) 0.0121 (3)
Mo8 0.0409 (4) 0.0384 (3) 0.0306 (3) 0.0043 (3) −0.0081 (3) 0.0091 (3)
Mo9 0.0560 (4) 0.0450 (4) 0.0268 (3) 0.0115 (3) 0.0128 (3) 0.0052 (3)
Mo10 0.0317 (3) 0.0291 (3) 0.0447 (4) 0.0035 (2) 0.0021 (3) −0.0131 (3)
Mo11 0.0238 (3) 0.0406 (3) 0.0419 (4) 0.0031 (2) 0.0032 (3) −0.0048 (3)
Mo12 0.0406 (3) 0.0386 (3) 0.0238 (3) 0.0044 (3) 0.0064 (3) 0.0030 (3)
P1 0.0222 (7) 0.0199 (6) 0.0198 (7) 0.0017 (5) −0.0004 (5) 0.0009 (5)
O1 0.050 (4) 0.057 (4) 0.051 (4) 0.014 (3) −0.006 (3) −0.014 (3)
O2 0.040 (3) 0.040 (3) 0.056 (4) −0.009 (2) −0.007 (3) −0.006 (3)
O3 0.034 (3) 0.036 (3) 0.035 (3) 0.000 (2) −0.009 (2) 0.001 (2)
O4 0.034 (3) 0.027 (2) 0.035 (3) 0.0005 (19) −0.003 (2) 0.005 (2)
O5 0.032 (3) 0.029 (2) 0.037 (3) −0.0049 (19) 0.000 (2) −0.002 (2)
O6 0.031 (3) 0.043 (3) 0.052 (3) −0.004 (2) −0.013 (2) −0.009 (3)
O7 0.030 (3) 0.032 (2) 0.037 (3) 0.0019 (19) 0.002 (2) −0.004 (2)
O8 0.038 (3) 0.027 (2) 0.042 (3) 0.008 (2) 0.002 (2) −0.007 (2)
O9 0.035 (3) 0.031 (2) 0.033 (3) 0.001 (2) −0.005 (2) −0.006 (2)
O10 0.044 (3) 0.029 (2) 0.039 (3) 0.004 (2) 0.000 (2) 0.001 (2)
O11 0.051 (3) 0.032 (3) 0.040 (3) 0.004 (2) −0.005 (3) 0.009 (2)
O12 0.037 (3) 0.035 (3) 0.032 (3) 0.004 (2) 0.001 (2) 0.000 (2)
O13 0.054 (3) 0.051 (3) 0.021 (2) 0.007 (3) −0.003 (2) 0.004 (2)
O14 0.043 (3) 0.040 (3) 0.030 (3) 0.006 (2) 0.002 (2) −0.003 (2)
O15 0.029 (3) 0.032 (2) 0.040 (3) 0.003 (2) 0.002 (2) −0.003 (2)
O16 0.032 (3) 0.061 (4) 0.065 (4) 0.007 (3) 0.011 (3) −0.009 (3)
O17 0.031 (3) 0.034 (2) 0.044 (3) 0.007 (2) −0.002 (2) 0.005 (2)
O18 0.026 (3) 0.040 (3) 0.047 (3) −0.004 (2) 0.003 (2) 0.000 (2)
O19 0.025 (2) 0.0205 (19) 0.024 (2) 0.0017 (16) −0.0012 (17) 0.0037 (17)
O20 0.031 (2) 0.023 (2) 0.023 (2) 0.0016 (17) 0.0007 (18) 0.0042 (18)
O21 0.027 (2) 0.0232 (18) 0.022 (2) 0.0028 (16) 0.0001 (19) −0.0043 (18)
O22 0.030 (2) 0.0222 (19) 0.022 (2) 0.0018 (17) −0.0004 (18) −0.0021 (17)
O23 0.035 (3) 0.038 (3) 0.031 (3) 0.002 (2) −0.003 (2) −0.001 (2)
O24 0.064 (4) 0.061 (4) 0.028 (3) 0.005 (3) 0.016 (3) 0.006 (3)
O25 0.032 (3) 0.035 (2) 0.036 (3) −0.001 (2) 0.000 (2) −0.003 (2)
O26 0.029 (2) 0.039 (3) 0.033 (3) 0.006 (2) 0.007 (2) −0.004 (2)
O27 0.042 (3) 0.038 (3) 0.025 (2) 0.006 (2) −0.002 (2) −0.008 (2)
O28 0.050 (4) 0.038 (3) 0.062 (4) 0.006 (3) 0.004 (3) −0.024 (3)
O29 0.038 (3) 0.0220 (19) 0.048 (3) 0.0043 (19) −0.001 (2) −0.002 (2)
O30 0.032 (3) 0.035 (2) 0.036 (3) 0.005 (2) −0.003 (2) −0.013 (2)
O31 0.051 (4) 0.039 (3) 0.042 (3) −0.002 (2) 0.014 (3) 0.013 (2)
O32 0.042 (3) 0.030 (2) 0.030 (2) 0.011 (2) −0.002 (2) 0.001 (2)
O33 0.060 (4) 0.061 (4) 0.043 (3) 0.013 (3) −0.018 (3) 0.010 (3)
O34 0.041 (3) 0.029 (2) 0.039 (3) −0.005 (2) 0.005 (2) 0.006 (2)
O35 0.054 (4) 0.038 (3) 0.055 (4) −0.012 (3) −0.002 (3) 0.014 (3)
O36 0.047 (3) 0.047 (3) 0.040 (3) 0.001 (3) −0.016 (3) 0.015 (3)
N1 0.060 (5) 0.033 (3) 0.044 (4) −0.002 (3) 0.008 (4) 0.000 (3)
N2 0.040 (4) 0.056 (4) 0.035 (3) 0.000 (3) 0.004 (3) −0.007 (3)
N3 0.040 (4) 0.041 (3) 0.050 (4) −0.002 (3) −0.010 (3) −0.007 (3)
N4 0.041 (4) 0.034 (3) 0.043 (4) 0.005 (3) −0.008 (3) −0.001 (3)
N5 0.049 (4) 0.039 (3) 0.054 (4) 0.007 (3) 0.000 (3) 0.012 (3)
O47 0.072 (5) 0.053 (4) 0.060 (4) −0.010 (3) −0.008 (4) 0.023 (3)
N7 0.043 (4) 0.037 (3) 0.040 (4) −0.005 (3) 0.004 (3) −0.002 (3)
N8 0.045 (4) 0.047 (4) 0.050 (4) −0.016 (3) 0.006 (3) −0.013 (3)
N9 0.052 (4) 0.043 (4) 0.047 (4) 0.005 (3) 0.002 (3) 0.001 (3)
O37 0.040 (3) 0.038 (3) 0.036 (3) 0.003 (2) 0.011 (2) 0.003 (2)
O38 0.075 (5) 0.085 (5) 0.030 (3) 0.017 (4) 0.026 (3) 0.003 (3)
O39 0.072 (4) 0.034 (3) 0.061 (4) −0.017 (3) −0.003 (3) 0.017 (3)
O55 0.036 (3) 0.054 (3) 0.048 (3) 0.017 (3) −0.003 (3) −0.015 (3)
O40 0.059 (4) 0.041 (3) 0.047 (3) −0.016 (3) −0.004 (3) 0.011 (3)
C2 0.049 (5) 0.029 (3) 0.060 (6) −0.006 (3) −0.002 (4) −0.003 (4)
C3 0.051 (6) 0.053 (5) 0.079 (7) −0.004 (4) 0.017 (5) 0.007 (5)
C4 0.105 (9) 0.059 (6) 0.037 (5) −0.012 (6) 0.002 (5) 0.008 (5)
O41 0.057 (4) 0.077 (4) 0.040 (3) 0.019 (4) −0.004 (3) −0.016 (3)
C6 0.050 (5) 0.058 (5) 0.046 (5) 0.014 (4) −0.006 (4) −0.009 (4)
C7 0.062 (7) 0.103 (9) 0.036 (5) −0.012 (6) 0.012 (5) −0.015 (5)
C8 0.067 (7) 0.080 (7) 0.056 (6) 0.019 (6) 0.018 (5) −0.007 (6)
O42 0.041 (3) 0.045 (3) 0.056 (4) −0.006 (3) −0.012 (3) −0.001 (3)
C10 0.040 (4) 0.042 (4) 0.046 (5) 0.000 (3) −0.003 (4) −0.005 (4)
C11 0.047 (6) 0.074 (7) 0.066 (6) 0.006 (5) −0.002 (5) −0.018 (5)
C12 0.057 (6) 0.065 (6) 0.078 (7) −0.023 (5) −0.004 (6) −0.009 (6)
O43 0.073 (4) 0.047 (3) 0.033 (3) 0.003 (3) −0.010 (3) −0.007 (3)
C14 0.053 (5) 0.039 (4) 0.034 (4) 0.003 (4) −0.010 (4) 0.000 (4)
C15 0.061 (6) 0.040 (4) 0.038 (4) 0.011 (4) −0.013 (4) −0.003 (3)
C16 0.078 (7) 0.042 (4) 0.045 (5) 0.005 (5) −0.003 (5) 0.004 (4)
O44 0.052 (4) 0.058 (4) 0.049 (4) 0.019 (3) −0.002 (3) 0.000 (3)
C18 0.045 (5) 0.042 (4) 0.053 (5) −0.003 (3) −0.008 (4) 0.000 (4)
C19 0.058 (6) 0.044 (5) 0.093 (8) 0.007 (4) 0.007 (6) 0.016 (5)
C20 0.128 (13) 0.149 (14) 0.064 (8) 0.055 (11) −0.058 (9) −0.021 (9)
C21 0.049 (5) 0.045 (4) 0.042 (5) −0.010 (4) 0.001 (4) 0.007 (4)
C22 0.050 (5) 0.044 (5) 0.081 (7) −0.011 (4) 0.005 (5) −0.006 (5)
C23 0.075 (7) 0.065 (6) 0.051 (6) −0.018 (5) −0.011 (5) 0.023 (5)
O45 0.041 (3) 0.046 (3) 0.064 (4) −0.013 (3) −0.001 (3) 0.008 (3)
C25 0.050 (5) 0.039 (4) 0.046 (5) −0.014 (3) 0.003 (4) −0.007 (4)
C26 0.084 (9) 0.041 (5) 0.140 (13) −0.009 (6) 0.007 (8) −0.008 (6)
C27 0.052 (6) 0.106 (9) 0.083 (9) −0.023 (6) 0.014 (6) −0.027 (7)
C28 0.065 (6) 0.044 (4) 0.042 (5) 0.009 (4) 0.001 (4) −0.013 (4)
C29 0.070 (8) 0.119 (10) 0.063 (7) 0.003 (7) 0.001 (6) −0.047 (7)
C30 0.095 (10) 0.100 (9) 0.069 (8) 0.057 (8) −0.008 (7) −0.006 (7)
O52 0.069 (4) 0.035 (3) 0.067 (4) −0.004 (3) 0.007 (4) −0.025 (3)

Geometric parameters (Å, º)

Eu1—O40 2.369 (5) N1—C3 1.450 (12)
Eu1—O47 2.378 (6) N1—C4 1.452 (12)
Eu1—O1 2.383 (6) N2—C6 1.311 (11)
Eu1—O45 2.387 (5) N2—C7 1.433 (12)
Eu1—O41 2.395 (6) N2—C8 1.455 (12)
Eu1—O44 2.413 (6) N3—C10 1.312 (11)
Eu1—O42 2.415 (6) N3—C12 1.438 (11)
Eu1—O43 2.416 (6) N3—C11 1.463 (12)
Mo1—O2 1.672 (5) N4—C14 1.313 (10)
Mo1—O9 1.836 (5) N4—C16 1.441 (11)
Mo1—O3 1.852 (5) N4—C15 1.452 (10)
Mo1—O34 1.973 (5) N5—C18 1.297 (11)
Mo1—O18 1.986 (5) N5—C20 1.417 (14)
Mo1—O19 2.436 (4) N5—C19 1.433 (12)
Mo2—O36 1.690 (5) O47—C21 1.214 (11)
Mo2—O4 1.831 (5) N7—C21 1.307 (10)
Mo2—O17 1.866 (5) N7—C23 1.427 (12)
Mo2—O23 1.957 (5) N7—C22 1.435 (11)
Mo2—O3 1.993 (5) N8—C25 1.313 (10)
Mo2—O19 2.429 (4) N8—C26 1.427 (13)
Mo3—O35 1.672 (5) N8—C27 1.477 (13)
Mo3—O25 1.842 (5) N9—C28 1.290 (11)
Mo3—O5 1.848 (5) N9—C29 1.435 (13)
Mo3—O4 1.985 (5) N9—C30 1.461 (14)
Mo3—O29 1.985 (5) O40—C2 1.245 (11)
Mo3—O21 2.428 (4) C2—H8 0.9300
Mo4—O6 1.677 (5) C3—H2 0.9600
Mo4—O12 1.834 (5) C3—H3 0.9600
Mo4—O30 1.851 (5) C3—H4 0.9600
Mo4—O5 1.976 (5) C4—H6 0.9600
Mo4—O7 1.992 (5) C4—H7 0.9600
Mo4—O21 2.426 (4) C4—H5 0.9600
Mo5—O55 1.675 (5) O41—C6 1.245 (11)
Mo5—O7 1.825 (5) C6—H10 0.9300
Mo5—O26 1.845 (5) C7—H12 0.9600
Mo5—O32 1.979 (5) C7—H13 0.9600
Mo5—O8 1.985 (5) C7—H11 0.9600
Mo5—O22 2.428 (5) C8—H15 0.9600
Mo6—O52 1.676 (5) C8—H16 0.9600
Mo6—O10 1.837 (5) C8—H14 0.9600
Mo6—O8 1.852 (5) O42—C10 1.228 (9)
Mo6—O9 1.983 (5) C10—H18 0.9300
Mo6—O27 2.000 (5) C11—H19 0.9600
Mo6—O22 2.416 (4) C11—H20 0.9600
Mo7—O39 1.686 (5) C11—H21 0.9600
Mo7—O34 1.842 (6) C12—H22 0.9600
Mo7—O31 1.854 (6) C12—H23 0.9600
Mo7—O10 1.973 (6) C12—H24 0.9600
Mo7—O11 1.994 (6) O43—C14 1.214 (10)
Mo7—O20 2.438 (4) C14—H26 0.9300
Mo8—O33 1.675 (6) C15—H28 0.9600
Mo8—O11 1.844 (6) C15—H29 0.9600
Mo8—O32 1.853 (5) C15—H27 0.9600
Mo8—O12 1.983 (5) C16—H31 0.9600
Mo8—O13 1.987 (6) C16—H30 0.9600
Mo8—O20 2.423 (4) C16—H32 0.9600
Mo9—O38 1.680 (6) O44—C18 1.229 (10)
Mo9—O14 1.838 (6) C18—H34 0.9300
Mo9—O13 1.851 (6) C19—H35 0.9600
Mo9—O31 1.984 (6) C19—H36 0.9600
Mo9—O37 1.993 (6) C19—H37 0.9600
Mo9—O20 2.433 (5) C20—H39 0.9600
Mo10—O28 1.690 (5) C20—H40 0.9600
Mo10—O15 1.842 (5) C20—H38 0.9600
Mo10—O29 1.847 (6) C21—H47 0.9300
Mo10—O14 1.976 (5) C22—H41 0.9600
Mo10—O30 1.984 (5) C22—H42 0.9600
Mo10—O21 2.420 (4) C22—H43 0.9600
Mo11—O16 1.676 (6) C23—H44 0.9600
Mo11—O37 1.836 (5) C23—H46 0.9600
Mo11—O18 1.857 (5) C23—H45 0.9600
Mo11—O15 1.976 (5) O45—C25 1.227 (10)
Mo11—O17 1.979 (5) C25—H55 0.9300
Mo11—O19 2.423 (4) C26—H49 0.9600
Mo12—O24 1.684 (5) C26—H51 0.9600
Mo12—O23 1.840 (5) C26—H50 0.9600
Mo12—O27 1.850 (5) C27—H52 0.9600
Mo12—O25 1.976 (5) C27—H53 0.9600
Mo12—O26 1.980 (5) C27—H54 0.9600
Mo12—O22 2.428 (4) C28—H56 0.9300
P1—O19 1.521 (5) C29—H58 0.9600
P1—O20 1.526 (5) C29—H59 0.9600
P1—O22 1.527 (5) C29—H57 0.9600
P1—O21 1.536 (4) C30—H61 0.9600
O1—C28 1.219 (11) C30—H62 0.9600
N1—C2 1.297 (11) C30—H60 0.9600
O40—Eu1—O47 145.6 (2) O26—Mo12—O22 72.45 (18)
O40—Eu1—O1 98.6 (2) O19—P1—O20 109.8 (3)
O47—Eu1—O1 76.7 (2) O19—P1—O22 109.5 (3)
O40—Eu1—O45 141.7 (2) O20—P1—O22 109.1 (2)
O47—Eu1—O45 72.7 (2) O19—P1—O21 109.3 (2)
O1—Eu1—O45 88.5 (2) O20—P1—O21 109.5 (3)
O40—Eu1—O41 93.6 (2) O22—P1—O21 109.6 (3)
O47—Eu1—O41 75.1 (3) C28—O1—Eu1 137.4 (6)
O1—Eu1—O41 145.4 (2) Mo1—O3—Mo2 124.5 (3)
O45—Eu1—O41 101.7 (2) Mo2—O4—Mo3 151.4 (3)
O40—Eu1—O44 76.2 (2) Mo3—O5—Mo4 125.8 (3)
O47—Eu1—O44 127.6 (2) Mo5—O7—Mo4 151.7 (3)
O1—Eu1—O44 142.6 (2) Mo6—O8—Mo5 124.8 (2)
O45—Eu1—O44 75.6 (2) Mo1—O9—Mo6 151.6 (3)
O41—Eu1—O44 71.8 (2) Mo6—O10—Mo7 151.5 (3)
O40—Eu1—O42 70.2 (2) Mo8—O11—Mo7 125.5 (3)
O47—Eu1—O42 75.6 (2) Mo4—O12—Mo8 152.1 (3)
O1—Eu1—O42 76.8 (2) Mo9—O13—Mo8 124.6 (3)
O45—Eu1—O42 147.4 (2) Mo9—O14—Mo10 151.8 (3)
O41—Eu1—O42 77.2 (2) Mo10—O15—Mo11 151.4 (3)
O44—Eu1—O42 132.0 (2) Mo2—O17—Mo11 124.8 (3)
O40—Eu1—O43 73.5 (2) Mo11—O18—Mo1 124.6 (3)
O47—Eu1—O43 132.8 (2) P1—O19—Mo11 126.2 (2)
O1—Eu1—O43 70.2 (2) P1—O19—Mo2 125.7 (2)
O45—Eu1—O43 73.7 (2) Mo11—O19—Mo2 89.23 (14)
O41—Eu1—O43 144.3 (2) P1—O19—Mo1 126.1 (2)
O44—Eu1—O43 72.8 (2) Mo11—O19—Mo1 88.93 (15)
O42—Eu1—O43 125.7 (2) Mo2—O19—Mo1 88.80 (15)
O2—Mo1—O9 102.7 (3) P1—O20—Mo8 126.5 (3)
O2—Mo1—O3 102.4 (3) P1—O20—Mo9 125.6 (2)
O9—Mo1—O3 95.8 (2) Mo8—O20—Mo9 88.87 (15)
O2—Mo1—O34 101.0 (3) P1—O20—Mo7 125.7 (3)
O9—Mo1—O34 85.0 (2) Mo8—O20—Mo7 89.20 (14)
O3—Mo1—O34 155.8 (2) Mo9—O20—Mo7 89.09 (15)
O2—Mo1—O18 100.5 (3) P1—O21—Mo10 126.1 (3)
O9—Mo1—O18 155.7 (2) P1—O21—Mo4 125.6 (2)
O3—Mo1—O18 86.5 (2) Mo10—O21—Mo4 89.12 (14)
O34—Mo1—O18 83.2 (2) P1—O21—Mo3 126.0 (3)
O2—Mo1—O19 171.9 (2) Mo10—O21—Mo3 89.13 (13)
O9—Mo1—O19 85.20 (18) Mo4—O21—Mo3 89.11 (14)
O3—Mo1—O19 74.36 (18) P1—O22—Mo6 126.0 (3)
O34—Mo1—O19 81.65 (18) P1—O22—Mo5 126.1 (3)
O18—Mo1—O19 72.08 (18) Mo6—O22—Mo5 89.19 (14)
O36—Mo2—O4 103.7 (2) P1—O22—Mo12 126.0 (2)
O36—Mo2—O17 102.2 (3) Mo6—O22—Mo12 89.10 (14)
O4—Mo2—O17 95.3 (2) Mo5—O22—Mo12 88.42 (15)
O36—Mo2—O23 101.5 (3) Mo12—O23—Mo2 152.1 (3)
O4—Mo2—O23 85.7 (2) Mo3—O25—Mo12 152.5 (3)
O17—Mo2—O23 155.4 (2) Mo5—O26—Mo12 124.5 (3)
O36—Mo2—O3 98.6 (3) Mo12—O27—Mo6 123.9 (3)
O4—Mo2—O3 156.8 (2) Mo10—O29—Mo3 125.1 (2)
O17—Mo2—O3 86.4 (2) Mo4—O30—Mo10 124.8 (3)
O23—Mo2—O3 83.5 (2) Mo7—O31—Mo9 125.8 (3)
O36—Mo2—O19 170.1 (2) Mo8—O32—Mo5 151.7 (3)
O4—Mo2—O19 85.87 (18) Mo7—O34—Mo1 152.0 (3)
O17—Mo2—O19 73.79 (19) C2—N1—C3 119.4 (8)
O23—Mo2—O19 81.74 (18) C2—N1—C4 121.4 (9)
O3—Mo2—O19 72.30 (18) C3—N1—C4 119.2 (8)
O35—Mo3—O25 102.3 (3) C6—N2—C7 121.7 (8)
O35—Mo3—O5 102.5 (3) C6—N2—C8 118.4 (8)
O25—Mo3—O5 96.1 (2) C7—N2—C8 119.9 (8)
O35—Mo3—O4 102.0 (3) C10—N3—C12 122.2 (8)
O25—Mo3—O4 84.4 (2) C10—N3—C11 120.0 (7)
O5—Mo3—O4 154.8 (2) C12—N3—C11 117.8 (8)
O35—Mo3—O29 100.9 (3) C14—N4—C16 119.6 (7)
O25—Mo3—O29 155.3 (2) C14—N4—C15 122.0 (7)
O5—Mo3—O29 87.0 (2) C16—N4—C15 118.2 (7)
O4—Mo3—O29 82.7 (2) C18—N5—C20 120.2 (9)
O35—Mo3—O21 171.5 (2) C18—N5—C19 121.8 (9)
O25—Mo3—O21 85.71 (19) C20—N5—C19 117.9 (10)
O5—Mo3—O21 73.44 (19) C21—O47—Eu1 166.5 (7)
O4—Mo3—O21 81.45 (17) C21—N7—C23 121.6 (8)
O29—Mo3—O21 71.66 (17) C21—N7—C22 120.6 (8)
O6—Mo4—O12 103.5 (3) C23—N7—C22 117.7 (8)
O6—Mo4—O30 103.7 (2) C25—N8—C26 121.7 (9)
O12—Mo4—O30 96.0 (2) C25—N8—C27 118.5 (9)
O6—Mo4—O5 99.6 (2) C26—N8—C27 118.9 (9)
O12—Mo4—O5 155.3 (2) C28—N9—C29 120.0 (9)
O30—Mo4—O5 87.0 (2) C28—N9—C30 122.9 (9)
O6—Mo4—O7 100.0 (2) C29—N9—C30 117.0 (9)
O12—Mo4—O7 85.3 (2) Mo11—O37—Mo9 151.5 (3)
O30—Mo4—O7 155.2 (2) C2—O40—Eu1 130.2 (5)
O5—Mo4—O7 82.0 (2) O40—C2—N1 123.4 (9)
O6—Mo4—O21 170.8 (2) O40—C2—H8 118.3
O12—Mo4—O21 85.6 (2) N1—C2—H8 118.3
O30—Mo4—O21 73.97 (19) N1—C3—H2 109.5
O5—Mo4—O21 71.54 (18) N1—C3—H3 109.5
O7—Mo4—O21 81.47 (18) H2—C3—H3 109.5
O55—Mo5—O7 103.4 (3) N1—C3—H4 109.5
O55—Mo5—O26 102.0 (3) H2—C3—H4 109.5
O7—Mo5—O26 96.1 (2) H3—C3—H4 109.5
O55—Mo5—O32 101.0 (3) N1—C4—H6 109.5
O7—Mo5—O32 85.1 (2) N1—C4—H7 109.5
O26—Mo5—O32 156.0 (2) H6—C4—H7 109.5
O55—Mo5—O8 99.6 (3) N1—C4—H5 109.5
O7—Mo5—O8 155.5 (2) H6—C4—H5 109.5
O26—Mo5—O8 87.2 (2) H7—C4—H5 109.5
O32—Mo5—O8 82.3 (2) C6—O41—Eu1 132.0 (6)
O55—Mo5—O22 170.7 (2) O41—C6—N2 123.9 (9)
O7—Mo5—O22 85.67 (19) O41—C6—H10 118.1
O26—Mo5—O22 74.59 (18) N2—C6—H10 118.1
O32—Mo5—O22 81.61 (18) N2—C7—H12 109.5
O8—Mo5—O22 71.80 (17) N2—C7—H13 109.5
O52—Mo6—O10 103.3 (3) H12—C7—H13 109.5
O52—Mo6—O8 102.5 (3) N2—C7—H11 109.5
O10—Mo6—O8 95.8 (2) H12—C7—H11 109.5
O52—Mo6—O9 100.9 (3) H13—C7—H11 109.5
O10—Mo6—O9 85.6 (2) N2—C8—H15 109.5
O8—Mo6—O9 155.5 (2) N2—C8—H16 109.5
O52—Mo6—O27 99.1 (3) H15—C8—H16 109.5
O10—Mo6—O27 156.2 (2) N2—C8—H14 109.5
O8—Mo6—O27 87.2 (2) H15—C8—H14 109.5
O9—Mo6—O27 82.1 (2) H16—C8—H14 109.5
O52—Mo6—O22 170.8 (3) C10—O42—Eu1 127.1 (5)
O10—Mo6—O22 85.69 (19) O42—C10—N3 125.4 (8)
O8—Mo6—O22 74.14 (18) O42—C10—H18 117.3
O9—Mo6—O22 81.56 (18) N3—C10—H18 117.3
O27—Mo6—O22 72.40 (17) N3—C11—H19 109.5
O39—Mo7—O34 103.4 (3) N3—C11—H20 109.5
O39—Mo7—O31 102.8 (3) H19—C11—H20 109.5
O34—Mo7—O31 96.1 (3) N3—C11—H21 109.5
O39—Mo7—O10 102.0 (3) H19—C11—H21 109.5
O34—Mo7—O10 85.3 (2) H20—C11—H21 109.5
O31—Mo7—O10 154.1 (2) N3—C12—H22 109.5
O39—Mo7—O11 99.8 (3) N3—C12—H23 109.5
O34—Mo7—O11 155.4 (2) H22—C12—H23 109.5
O31—Mo7—O11 86.4 (3) N3—C12—H24 109.5
O10—Mo7—O11 82.1 (2) H22—C12—H24 109.5
O39—Mo7—O20 170.4 (3) H23—C12—H24 109.5
O34—Mo7—O20 85.93 (18) C14—O43—Eu1 132.6 (5)
O31—Mo7—O20 73.5 (2) O43—C14—N4 124.7 (8)
O10—Mo7—O20 80.88 (19) O43—C14—H26 117.6
O11—Mo7—O20 71.30 (18) N4—C14—H26 117.6
O33—Mo8—O11 102.1 (3) N4—C15—H28 109.5
O33—Mo8—O32 103.5 (3) N4—C15—H29 109.5
O11—Mo8—O32 96.5 (2) H28—C15—H29 109.5
O33—Mo8—O12 101.9 (3) N4—C15—H27 109.5
O11—Mo8—O12 155.0 (2) H28—C15—H27 109.5
O32—Mo8—O12 84.6 (2) H29—C15—H27 109.5
O33—Mo8—O13 98.9 (3) N4—C16—H31 109.5
O11—Mo8—O13 86.8 (3) N4—C16—H30 109.5
O32—Mo8—O13 156.0 (2) H31—C16—H30 109.5
O12—Mo8—O13 82.7 (2) N4—C16—H32 109.5
O33—Mo8—O20 170.4 (3) H31—C16—H32 109.5
O11—Mo8—O20 74.0 (2) H30—C16—H32 109.5
O32—Mo8—O20 85.74 (19) C18—O44—Eu1 138.8 (6)
O12—Mo8—O20 81.23 (18) O44—C18—N5 126.1 (9)
O13—Mo8—O20 72.31 (19) O44—C18—H34 117.0
O38—Mo9—O14 103.1 (3) N5—C18—H34 117.0
O38—Mo9—O13 102.6 (3) N5—C19—H35 109.5
O14—Mo9—O13 96.7 (3) N5—C19—H36 109.5
O38—Mo9—O31 99.6 (3) H35—C19—H36 109.5
O14—Mo9—O31 155.6 (2) N5—C19—H37 109.5
O13—Mo9—O31 86.9 (3) H35—C19—H37 109.5
O38—Mo9—O37 101.1 (3) H36—C19—H37 109.5
O14—Mo9—O37 85.0 (2) N5—C20—H39 109.5
O13—Mo9—O37 155.1 (2) N5—C20—H40 109.5
O31—Mo9—O37 81.9 (2) H39—C20—H40 109.5
O38—Mo9—O20 170.6 (3) N5—C20—H38 109.5
O14—Mo9—O20 86.07 (19) H39—C20—H38 109.5
O13—Mo9—O20 74.19 (19) H40—C20—H38 109.5
O31—Mo9—O20 71.60 (19) O47—C21—N7 124.6 (9)
O37—Mo9—O20 81.18 (18) O47—C21—H47 117.7
O28—Mo10—O15 103.4 (3) N7—C21—H47 117.7
O28—Mo10—O29 103.0 (3) N7—C22—H41 109.5
O15—Mo10—O29 95.3 (2) N7—C22—H42 109.5
O28—Mo10—O14 100.5 (3) H41—C22—H42 109.5
O15—Mo10—O14 85.4 (2) N7—C22—H43 109.5
O29—Mo10—O14 155.7 (2) H41—C22—H43 109.5
O28—Mo10—O30 99.6 (3) H42—C22—H43 109.5
O15—Mo10—O30 155.7 (2) N7—C23—H44 109.5
O29—Mo10—O30 87.1 (2) N7—C23—H46 109.5
O14—Mo10—O30 82.7 (2) H44—C23—H46 109.5
O28—Mo10—O21 171.0 (2) N7—C23—H45 109.5
O15—Mo10—O21 85.38 (19) H44—C23—H45 109.5
O29—Mo10—O21 74.00 (18) H46—C23—H45 109.5
O14—Mo10—O21 81.87 (18) C25—O45—Eu1 136.7 (6)
O30—Mo10—O21 72.04 (17) O45—C25—N8 122.8 (8)
O16—Mo11—O37 104.0 (3) O45—C25—H55 118.6
O16—Mo11—O18 103.5 (3) N8—C25—H55 118.6
O37—Mo11—O18 95.7 (2) N8—C26—H49 109.5
O16—Mo11—O15 99.8 (3) N8—C26—H51 109.5
O37—Mo11—O15 85.6 (2) H49—C26—H51 109.5
O18—Mo11—O15 155.6 (2) N8—C26—H50 109.5
O16—Mo11—O17 98.8 (3) H49—C26—H50 109.5
O37—Mo11—O17 155.7 (2) H51—C26—H50 109.5
O18—Mo11—O17 86.8 (2) N8—C27—H52 109.5
O15—Mo11—O17 82.4 (2) N8—C27—H53 109.5
O16—Mo11—O19 170.7 (3) H52—C27—H53 109.5
O37—Mo11—O19 85.24 (19) N8—C27—H54 109.5
O18—Mo11—O19 74.38 (19) H52—C27—H54 109.5
O15—Mo11—O19 81.50 (18) H53—C27—H54 109.5
O17—Mo11—O19 72.16 (18) O1—C28—N9 125.3 (9)
O24—Mo12—O23 102.9 (3) O1—C28—H56 117.4
O24—Mo12—O27 101.4 (3) N9—C28—H56 117.4
O23—Mo12—O27 95.4 (2) N9—C29—H58 109.5
O24—Mo12—O25 101.9 (3) N9—C29—H59 109.5
O23—Mo12—O25 84.4 (2) H58—C29—H59 109.5
O27—Mo12—O25 156.2 (2) N9—C29—H57 109.5
O24—Mo12—O26 100.0 (3) H58—C29—H57 109.5
O23—Mo12—O26 155.8 (2) H59—C29—H57 109.5
O27—Mo12—O26 87.7 (2) N9—C30—H61 109.5
O25—Mo12—O26 83.2 (2) N9—C30—H62 109.5
O24—Mo12—O22 171.3 (3) H61—C30—H62 109.5
O23—Mo12—O22 85.27 (19) N9—C30—H60 109.5
O27—Mo12—O22 74.48 (18) H61—C30—H60 109.5
O25—Mo12—O22 81.80 (18) H62—C30—H60 109.5
O2—Mo1—O3—Mo2 171.0 (3) O22—P1—O21—Mo10 175.5 (3)
O9—Mo1—O3—Mo2 −84.6 (3) O19—P1—O21—Mo4 175.3 (3)
O34—Mo1—O3—Mo2 6.0 (8) O20—P1—O21—Mo4 55.0 (4)
O18—Mo1—O3—Mo2 71.1 (3) O22—P1—O21—Mo4 −64.6 (4)
O19—Mo1—O3—Mo2 −1.3 (3) O19—P1—O21—Mo3 −64.9 (3)
O36—Mo2—O4—Mo3 −129.9 (6) O20—P1—O21—Mo3 174.7 (3)
O17—Mo2—O4—Mo3 126.1 (6) O22—P1—O21—Mo3 55.1 (3)
O23—Mo2—O4—Mo3 −29.1 (6) O19—P1—O22—Mo6 −64.7 (3)
O3—Mo2—O4—Mo3 33.1 (10) O20—P1—O22—Mo6 55.5 (4)
O19—Mo2—O4—Mo3 52.9 (6) O21—P1—O22—Mo6 175.3 (3)
O35—Mo3—O5—Mo4 169.8 (3) O19—P1—O22—Mo5 174.7 (3)
O25—Mo3—O5—Mo4 −86.2 (3) O20—P1—O22—Mo5 −65.1 (3)
O4—Mo3—O5—Mo4 3.4 (7) O21—P1—O22—Mo5 54.8 (4)
O29—Mo3—O5—Mo4 69.3 (3) O19—P1—O22—Mo12 55.5 (4)
O21—Mo3—O5—Mo4 −2.5 (3) O20—P1—O22—Mo12 175.7 (3)
O55—Mo5—O7—Mo4 −129.4 (6) O21—P1—O22—Mo12 −64.4 (4)
O26—Mo5—O7—Mo4 126.7 (6) O24—Mo12—O23—Mo2 −130.2 (6)
O32—Mo5—O7—Mo4 −29.2 (6) O27—Mo12—O23—Mo2 126.8 (6)
O8—Mo5—O7—Mo4 30.1 (10) O25—Mo12—O23—Mo2 −29.3 (6)
O22—Mo5—O7—Mo4 52.8 (6) O26—Mo12—O23—Mo2 30.3 (10)
O52—Mo6—O8—Mo5 168.5 (4) O22—Mo12—O23—Mo2 52.9 (6)
O10—Mo6—O8—Mo5 −86.5 (3) O35—Mo3—O25—Mo12 −132.4 (7)
O9—Mo6—O8—Mo5 5.7 (8) O5—Mo3—O25—Mo12 123.3 (7)
O27—Mo6—O8—Mo5 69.8 (3) O4—Mo3—O25—Mo12 −31.3 (6)
O22—Mo6—O8—Mo5 −2.7 (3) O29—Mo3—O25—Mo12 27.3 (10)
O2—Mo1—O9—Mo6 −129.2 (6) O21—Mo3—O25—Mo12 50.5 (6)
O3—Mo1—O9—Mo6 126.6 (6) O55—Mo5—O26—Mo12 169.1 (3)
O34—Mo1—O9—Mo6 −29.1 (6) O7—Mo5—O26—Mo12 −85.8 (3)
O18—Mo1—O9—Mo6 32.2 (10) O32—Mo5—O26—Mo12 5.8 (7)
O19—Mo1—O9—Mo6 52.9 (6) O8—Mo5—O26—Mo12 69.8 (3)
O52—Mo6—O10—Mo7 −128.1 (7) O22—Mo5—O26—Mo12 −2.0 (3)
O8—Mo6—O10—Mo7 127.5 (7) O24—Mo12—O27—Mo6 169.1 (3)
O9—Mo6—O10—Mo7 −27.9 (7) O23—Mo12—O27—Mo6 −86.6 (3)
O27—Mo6—O10—Mo7 31.2 (11) O25—Mo12—O27—Mo6 1.8 (8)
O22—Mo6—O10—Mo7 54.0 (7) O26—Mo12—O27—Mo6 69.4 (3)
O33—Mo8—O11—Mo7 168.8 (4) O22—Mo12—O27—Mo6 −3.0 (3)
O32—Mo8—O11—Mo7 −85.8 (4) O28—Mo10—O29—Mo3 168.8 (3)
O12—Mo8—O11—Mo7 5.2 (8) O15—Mo10—O29—Mo3 −86.1 (3)
O13—Mo8—O11—Mo7 70.3 (4) O14—Mo10—O29—Mo3 4.4 (8)
O20—Mo8—O11—Mo7 −2.2 (3) O30—Mo10—O29—Mo3 69.6 (3)
O6—Mo4—O12—Mo8 −128.2 (6) O21—Mo10—O29—Mo3 −2.5 (3)
O30—Mo4—O12—Mo8 126.1 (6) O6—Mo4—O30—Mo10 168.6 (3)
O5—Mo4—O12—Mo8 30.3 (10) O12—Mo4—O30—Mo10 −85.9 (4)
O7—Mo4—O12—Mo8 −29.0 (6) O5—Mo4—O30—Mo10 69.4 (3)
O21—Mo4—O12—Mo8 52.8 (6) O7—Mo4—O30—Mo10 5.8 (8)
O38—Mo9—O13—Mo8 169.0 (4) O21—Mo4—O30—Mo10 −2.2 (3)
O14—Mo9—O13—Mo8 −85.8 (4) O39—Mo7—O31—Mo9 168.4 (4)
O31—Mo9—O13—Mo8 69.9 (4) O34—Mo7—O31—Mo9 −86.3 (4)
O37—Mo9—O13—Mo8 6.8 (9) O10—Mo7—O31—Mo9 5.5 (8)
O20—Mo9—O13—Mo8 −1.9 (3) O11—Mo7—O31—Mo9 69.2 (4)
O38—Mo9—O14—Mo10 −131.0 (7) O20—Mo7—O31—Mo9 −2.4 (3)
O13—Mo9—O14—Mo10 124.3 (7) O33—Mo8—O32—Mo5 −132.1 (7)
O31—Mo9—O14—Mo10 27.0 (11) O11—Mo8—O32—Mo5 123.8 (7)
O37—Mo9—O14—Mo10 −30.7 (6) O12—Mo8—O32—Mo5 −31.1 (7)
O20—Mo9—O14—Mo10 50.8 (6) O13—Mo8—O32—Mo5 27.1 (11)
O28—Mo10—O15—Mo11 −128.4 (6) O20—Mo8—O32—Mo5 50.5 (6)
O29—Mo10—O15—Mo11 126.9 (6) O39—Mo7—O34—Mo1 −131.2 (6)
O14—Mo10—O15—Mo11 −28.7 (6) O31—Mo7—O34—Mo1 124.0 (6)
O30—Mo10—O15—Mo11 32.1 (10) O10—Mo7—O34—Mo1 −30.0 (6)
O21—Mo10—O15—Mo11 53.5 (6) O11—Mo7—O34—Mo1 29.3 (10)
O36—Mo2—O17—Mo11 168.2 (3) O20—Mo7—O34—Mo1 51.1 (6)
O4—Mo2—O17—Mo11 −86.5 (3) O16—Mo11—O37—Mo9 −127.0 (6)
O23—Mo2—O17—Mo11 4.5 (7) O18—Mo11—O37—Mo9 127.6 (6)
O3—Mo2—O17—Mo11 70.2 (3) O15—Mo11—O37—Mo9 −28.0 (6)
O19—Mo2—O17—Mo11 −2.4 (3) O17—Mo11—O37—Mo9 32.5 (10)
O16—Mo11—O18—Mo1 168.6 (4) O19—Mo11—O37—Mo9 53.8 (6)
O37—Mo11—O18—Mo1 −85.5 (4) Eu1—O40—C2—N1 −154.9 (6)
O15—Mo11—O18—Mo1 6.6 (8) C3—N1—C2—O40 −3.1 (13)
O17—Mo11—O18—Mo1 70.3 (3) C4—N1—C2—O40 177.2 (8)
O19—Mo11—O18—Mo1 −2.1 (3) Eu1—O41—C6—N2 −176.3 (7)
O20—P1—O19—Mo11 55.7 (3) C7—N2—C6—O41 179.1 (10)
O22—P1—O19—Mo11 175.5 (3) C8—N2—C6—O41 −2.5 (15)
O21—P1—O19—Mo11 −64.4 (3) Eu1—O42—C10—N3 −146.6 (7)
O20—P1—O19—Mo2 175.9 (3) C12—N3—C10—O42 180.0 (9)
O22—P1—O19—Mo2 −64.3 (3) C11—N3—C10—O42 0.5 (14)
O21—P1—O19—Mo2 55.8 (4) Eu1—O43—C14—N4 −165.4 (6)
O20—P1—O19—Mo1 −64.6 (3) C16—N4—C14—O43 −0.9 (14)
O22—P1—O19—Mo1 55.2 (3) C15—N4—C14—O43 −176.1 (8)
O21—P1—O19—Mo1 175.3 (3) Eu1—O44—C18—N5 −169.7 (7)
O19—P1—O20—Mo8 175.4 (3) C20—N5—C18—O44 −3.2 (16)
O22—P1—O20—Mo8 55.4 (4) C19—N5—C18—O44 172.7 (9)
O21—P1—O20—Mo8 −64.6 (4) Eu1—O47—C21—N7 −167 (2)
O19—P1—O20—Mo9 −64.7 (4) C23—N7—C21—O47 −179.5 (9)
O22—P1—O20—Mo9 175.3 (3) C22—N7—C21—O47 4.0 (14)
O21—P1—O20—Mo9 55.3 (4) Eu1—O45—C25—N8 176.5 (6)
O19—P1—O20—Mo7 54.7 (4) C26—N8—C25—O45 −7.7 (16)
O22—P1—O20—Mo7 −65.4 (4) C27—N8—C25—O45 −177.4 (9)
O21—P1—O20—Mo7 174.7 (3) Eu1—O1—C28—N9 −169.7 (7)
O19—P1—O21—Mo10 55.4 (4) C29—N9—C28—O1 −0.5 (16)
O20—P1—O21—Mo10 −64.9 (3) C30—N9—C28—O1 176.3 (11)

Hydrogen-bond geometry (Å, º)

D—H···A D—H H···A D···A D—H···A
C3—H4···O31i 0.96 2.72 3.289 (11) 118
C4—H7···O36ii 0.96 2.61 3.476 (12) 150
C7—H13···O7 0.96 2.65 3.473 (12) 145
C8—H15···O28ii 0.96 2.51 3.316 (13) 141
C8—H16···O5 0.96 2.58 3.424 (11) 147
C10—H18···O28ii 0.93 2.62 3.516 (10) 162
C15—H29···O16i 0.96 2.55 3.299 (12) 135
C15—H27···O32iii 0.96 2.52 3.440 (10) 160
C15—H28···O52iv 0.96 2.29 3.174 (10) 153
C16—H31···O6iii 0.96 2.63 3.541 (11) 159
C22—H41···O55 0.96 2.53 3.280 (12) 135
C22—H42···O11iv 0.96 2.45 3.305 (11) 149
C22—H43···O45 0.96 2.61 3.567 (13) 172
C23—H44···O17v 0.96 2.52 3.443 (11) 161
C25—H55···O24 0.93 2.53 3.337 (11) 145
C25—H55···O44 0.93 2.58 3.091 (10) 115
C28—H56···O36v 0.93 2.62 3.476 (11) 153
C30—H60···O36v 0.96 2.58 3.458 (14) 152

Symmetry codes: (i) x+1/2, −y+1/2, z−1; (ii) −x+1, −y+1, z−1/2; (iii) x, y, z−1; (iv) −x+1, −y, z−1/2; (v) x+1/2, −y+1/2, z.

References

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Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

Crystal structure: contains datablock(s) I. DOI: 10.1107/S2056989016003546/wm5274sup1.cif

e-72-00448-sup1.cif (2.6MB, cif)

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989016003546/wm5274Isup2.hkl

e-72-00448-Isup2.hkl (2.6MB, hkl)

CCDC reference: 1456619

Additional supporting information: crystallographic information; 3D view; checkCIF report


Articles from Acta Crystallographica Section E: Crystallographic Communications are provided here courtesy of International Union of Crystallography

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