Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101003560/vj1129sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101003560/vj1129Isup2.hkl |
CCDC reference: 166960
For related literature, see: Jin et al. (1994); Li, Bian & Jin (2000); Li, Zheng & Jin (2000); Wang et al. (1995).
4-Methylbenzoic acid (3 mmol) was dissolved in 95% ethanol (25 ml) and its pH was maintaineded in the range 6–7 with NaOH (2 mol l-1) solution. Then Eu(NO3)3 (1 mmol) dissolved in H2O (5 ml) was added to the solution. The mixture was heated at 353 K under reflux with stirring for 6 h. A white precipitate was formed which was then filtered off. White prism-shaped crystals were obtained from the mother liquor after 2 weeks.
Data collection: XSCANS (Fait, 1991); cell refinement: XSCANS; data reduction: SHELXTL (Sheldrick, 1997a); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Eu3(C8H7O2)9] | F(000) = 3312 |
Mr = 1672.10 | Dx = 1.665 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 12.988 (1) Å | Cell parameters from 28 reflections |
b = 21.823 (2) Å | θ = 3.2–16.4° |
c = 23.542 (4) Å | µ = 2.86 mm−1 |
β = 90.84 (1)° | T = 298 K |
V = 6672.0 (14) Å3 | Prism, white |
Z = 4 | 0.32 × 0.20 × 0.18 mm |
Siemens P4 diffractometer | 8293 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.020 |
Graphite monochromator | θmax = 25.0°, θmin = 1.7° |
ω scans | h = 0→15 |
Absorption correction: empirical (using intensity measurements) (Kopfman & Huber, 1968) | k = 0→25 |
Tmin = 0.571, Tmax = 0.629 | l = −27→27 |
13082 measured reflections | 3 standard reflections every 97 reflections |
11743 independent reflections | intensity decay: 5.1% |
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)] = 0.031 | H-atom parameters constrained |
wR(F2) = 0.060 | w = 1/[σ2(Fo2) + (0.0235P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.90 | (Δ/σ)max = 0.005 |
11743 reflections | Δρmax = 0.81 e Å−3 |
848 parameters | Δρmin = −0.55 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.000078 (6) |
[Eu3(C8H7O2)9] | V = 6672.0 (14) Å3 |
Mr = 1672.10 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 12.988 (1) Å | µ = 2.86 mm−1 |
b = 21.823 (2) Å | T = 298 K |
c = 23.542 (4) Å | 0.32 × 0.20 × 0.18 mm |
β = 90.84 (1)° |
Siemens P4 diffractometer | 8293 reflections with I > 2σ(I) |
Absorption correction: empirical (using intensity measurements) (Kopfman & Huber, 1968) | Rint = 0.020 |
Tmin = 0.571, Tmax = 0.629 | 3 standard reflections every 97 reflections |
13082 measured reflections | intensity decay: 5.1% |
11743 independent reflections |
R[F2 > 2σ(F2)] = 0.031 | 0 restraints |
wR(F2) = 0.060 | H-atom parameters constrained |
S = 0.90 | Δρmax = 0.81 e Å−3 |
11743 reflections | Δρmin = −0.55 e Å−3 |
848 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 | ||
Eu1 | −0.714116 (19) | 1.312782 (10) | 0.258538 (9) | 0.02961 (7) | |
Eu2 | −0.783652 (17) | 1.482469 (11) | 0.273650 (9) | 0.02842 (6) | |
Eu3 | −0.710338 (18) | 1.648647 (10) | 0.266596 (10) | 0.03110 (7) | |
O1 | −0.6764 (2) | 1.20403 (14) | 0.29244 (12) | 0.0379 (8) | |
O2 | −0.5622 (2) | 1.27554 (15) | 0.31032 (14) | 0.0443 (9) | |
O3 | −0.5661 (3) | 1.35361 (15) | 0.21068 (14) | 0.0455 (9) | |
O4 | −0.6312 (2) | 1.42125 (14) | 0.26859 (13) | 0.0393 (8) | |
O5 | −0.7565 (3) | 1.31085 (16) | 0.35960 (13) | 0.0504 (10) | |
O6 | −0.8270 (2) | 1.38653 (13) | 0.31214 (12) | 0.0320 (7) | |
O7 | −0.7997 (3) | 1.3779 (2) | 0.19376 (15) | 0.0726 (13) | |
O8 | −0.8963 (3) | 1.4601 (2) | 0.19565 (16) | 0.0712 (13) | |
O9 | −0.9557 (2) | 1.51057 (15) | 0.30221 (14) | 0.0479 (9) | |
O10 | −0.8623 (2) | 1.59064 (14) | 0.28238 (13) | 0.0394 (8) | |
O11 | −0.7445 (3) | 1.49540 (15) | 0.37353 (13) | 0.0439 (9) | |
O12 | −0.6597 (2) | 1.56006 (13) | 0.32048 (12) | 0.0332 (7) | |
O13 | −0.7076 (3) | 1.54703 (15) | 0.20668 (13) | 0.0456 (9) | |
O14 | −0.6446 (3) | 1.63074 (17) | 0.17091 (15) | 0.0589 (11) | |
O15 | −0.7129 (3) | 1.67799 (16) | 0.36381 (14) | 0.0573 (11) | |
O16 | −0.8087 (3) | 1.74393 (16) | 0.31867 (13) | 0.0481 (9) | |
O17 | −0.5308 (2) | 1.67504 (15) | 0.27231 (14) | 0.0479 (9) | |
O18 | −0.6310 (2) | 1.75258 (14) | 0.24901 (13) | 0.0371 (8) | |
C1 | −0.3919 (4) | 1.0626 (3) | 0.4813 (2) | 0.0663 (18) | |
H1A | −0.3319 | 1.0829 | 0.4964 | 0.080* | |
H1B | −0.3722 | 1.0245 | 0.4642 | 0.080* | |
H1C | −0.4393 | 1.0549 | 0.5113 | 0.080* | |
C2 | −0.4429 (4) | 1.1030 (3) | 0.4369 (2) | 0.0441 (13) | |
C3 | −0.5240 (4) | 1.0825 (2) | 0.4045 (2) | 0.0493 (14) | |
H3 | −0.5478 | 1.0426 | 0.4091 | 0.059* | |
C4 | −0.5714 (4) | 1.1206 (2) | 0.3646 (2) | 0.0467 (14) | |
H4 | −0.6260 | 1.1056 | 0.3427 | 0.056* | |
C5 | −0.5391 (4) | 1.1799 (2) | 0.35706 (18) | 0.0343 (11) | |
C6 | −0.4570 (4) | 1.2011 (2) | 0.3899 (2) | 0.0456 (13) | |
H6 | −0.4342 | 1.2413 | 0.3859 | 0.055* | |
C7 | −0.4089 (4) | 1.1621 (3) | 0.4288 (2) | 0.0514 (15) | |
H7 | −0.3526 | 1.1763 | 0.4498 | 0.062* | |
C8 | −0.5941 (4) | 1.2222 (2) | 0.31802 (18) | 0.0327 (11) | |
C9 | −0.2045 (5) | 1.5572 (3) | 0.1936 (3) | 0.092 (2) | |
H9A | −0.1422 | 1.5342 | 0.1994 | 0.111* | |
H9B | −0.2045 | 1.5919 | 0.2187 | 0.111* | |
H9C | −0.2085 | 1.5712 | 0.1550 | 0.111* | |
C10 | −0.2960 (4) | 1.5169 (3) | 0.2059 (2) | 0.0597 (16) | |
C11 | −0.3761 (4) | 1.5386 (3) | 0.2383 (2) | 0.0581 (16) | |
H11 | −0.3728 | 1.5780 | 0.2533 | 0.070* | |
C12 | −0.4616 (4) | 1.5021 (2) | 0.2487 (2) | 0.0491 (14) | |
H12 | −0.5136 | 1.5166 | 0.2718 | 0.059* | |
C13 | −0.4697 (4) | 1.4445 (2) | 0.22490 (19) | 0.0361 (12) | |
C14 | −0.3895 (4) | 1.4233 (3) | 0.1930 (2) | 0.0583 (16) | |
H14 | −0.3933 | 1.3843 | 0.1770 | 0.070* | |
C15 | −0.3042 (5) | 1.4585 (3) | 0.1843 (3) | 0.074 (2) | |
H15 | −0.2504 | 1.4427 | 0.1632 | 0.089* | |
C16 | −0.5598 (4) | 1.4047 (2) | 0.2351 (2) | 0.0365 (12) | |
C17 | −1.0720 (5) | 1.4138 (3) | 0.5507 (2) | 0.0732 (19) | |
H17A | −1.0598 | 1.3847 | 0.5806 | 0.088* | |
H17B | −1.1430 | 1.4120 | 0.5389 | 0.088* | |
H17C | −1.0561 | 1.4543 | 0.5641 | 0.088* | |
C18 | −1.0044 (4) | 1.3987 (3) | 0.5010 (2) | 0.0521 (15) | |
C19 | −1.0233 (4) | 1.4245 (2) | 0.4480 (2) | 0.0564 (15) | |
H19 | −1.0786 | 1.4512 | 0.4432 | 0.068* | |
C20 | −0.9619 (4) | 1.4117 (2) | 0.4025 (2) | 0.0499 (14) | |
H20 | −0.9749 | 1.4306 | 0.3677 | 0.060* | |
C21 | −0.8815 (4) | 1.3711 (2) | 0.40787 (19) | 0.0387 (12) | |
C22 | −0.8621 (4) | 1.3437 (3) | 0.4603 (2) | 0.0570 (16) | |
H22 | −0.8087 | 1.3156 | 0.4646 | 0.068* | |
C23 | −0.9238 (5) | 1.3589 (3) | 0.5062 (2) | 0.0638 (17) | |
H23 | −0.9096 | 1.3414 | 0.5415 | 0.077* | |
C24 | −0.8170 (4) | 1.3550 (2) | 0.35879 (19) | 0.0368 (12) | |
C25 | −1.1514 (5) | 1.3037 (3) | 0.0059 (2) | 0.076 (2) | |
H25A | −1.1493 | 1.3294 | −0.0272 | 0.091* | |
H25B | −1.2205 | 1.3024 | 0.0198 | 0.091* | |
H25C | −1.1296 | 1.2631 | −0.0038 | 0.091* | |
C26 | −1.0795 (4) | 1.3298 (3) | 0.0520 (2) | 0.0475 (14) | |
C27 | −1.1025 (4) | 1.3851 (3) | 0.0772 (2) | 0.0510 (14) | |
H27 | −1.1626 | 1.4057 | 0.0669 | 0.061* | |
C28 | −1.0373 (4) | 1.4101 (2) | 0.1176 (2) | 0.0425 (13) | |
H28 | −1.0532 | 1.4476 | 0.1341 | 0.051* | |
C29 | −0.9481 (4) | 1.3796 (2) | 0.13361 (19) | 0.0369 (12) | |
C30 | −0.9264 (4) | 1.3252 (2) | 0.1087 (2) | 0.0540 (15) | |
H30 | −0.8659 | 1.3049 | 0.1187 | 0.065* | |
C31 | −0.9918 (5) | 1.2993 (3) | 0.0687 (2) | 0.0621 (17) | |
H31 | −0.9765 | 1.2613 | 0.0531 | 0.075* | |
C32 | −0.8768 (4) | 1.4090 (3) | 0.1767 (2) | 0.0509 (15) | |
C33 | −1.2904 (5) | 1.7206 (3) | 0.3634 (3) | 0.107 (3) | |
H33A | −1.3530 | 1.7079 | 0.3447 | 0.129* | |
H33B | −1.2761 | 1.7625 | 0.3541 | 0.129* | |
H33C | −1.2977 | 1.7167 | 0.4038 | 0.129* | |
C34 | −1.2023 (5) | 1.6804 (3) | 0.3441 (2) | 0.0674 (19) | |
C35 | −1.2070 (4) | 1.6178 (4) | 0.3502 (2) | 0.074 (2) | |
H35 | −1.2656 | 1.5998 | 0.3651 | 0.089* | |
C36 | −1.1255 (4) | 1.5813 (3) | 0.3344 (2) | 0.0563 (15) | |
H36 | −1.1302 | 1.5390 | 0.3384 | 0.068* | |
C37 | −1.0363 (4) | 1.6070 (2) | 0.31259 (19) | 0.0392 (12) | |
C38 | −1.0326 (4) | 1.6696 (2) | 0.3062 (2) | 0.0476 (14) | |
H38 | −0.9741 | 1.6879 | 0.2914 | 0.057* | |
C39 | −1.1154 (5) | 1.7057 (3) | 0.3217 (2) | 0.0644 (17) | |
H39 | −1.1119 | 1.7479 | 0.3167 | 0.077* | |
C40 | −0.9479 (4) | 1.5677 (2) | 0.29833 (18) | 0.0367 (12) | |
C41 | −0.4506 (5) | 1.6164 (3) | 0.5697 (2) | 0.086 (2) | |
H41A | −0.4728 | 1.5936 | 0.6022 | 0.103* | |
H41B | −0.4626 | 1.6593 | 0.5759 | 0.103* | |
H41C | −0.3784 | 1.6096 | 0.5641 | 0.103* | |
C42 | −0.5105 (5) | 1.5956 (2) | 0.5174 (2) | 0.0557 (16) | |
C43 | −0.5919 (4) | 1.5558 (2) | 0.5214 (2) | 0.0535 (15) | |
H43 | −0.6110 | 1.5414 | 0.5569 | 0.064* | |
C44 | −0.6463 (4) | 1.5364 (2) | 0.4734 (2) | 0.0484 (14) | |
H44 | −0.7013 | 1.5094 | 0.4770 | 0.058* | |
C45 | −0.6188 (4) | 1.5569 (2) | 0.42062 (19) | 0.0374 (12) | |
C46 | −0.5368 (4) | 1.5970 (2) | 0.4160 (2) | 0.0494 (14) | |
H46 | −0.5178 | 1.6114 | 0.3805 | 0.059* | |
C47 | −0.4829 (4) | 1.6157 (2) | 0.4644 (2) | 0.0598 (16) | |
H47 | −0.4274 | 1.6422 | 0.4609 | 0.072* | |
C48 | −0.6783 (4) | 1.5362 (2) | 0.36986 (19) | 0.0340 (11) | |
C49 | −0.6229 (5) | 1.4569 (3) | −0.0533 (2) | 0.101 (3) | |
H49A | −0.6815 | 1.4655 | −0.0773 | 0.121* | |
H49B | −0.6168 | 1.4134 | −0.0480 | 0.121* | |
H49C | −0.5618 | 1.4723 | −0.0708 | 0.121* | |
C50 | −0.6365 (4) | 1.4877 (4) | 0.0039 (2) | 0.0610 (16) | |
C51 | −0.6387 (4) | 1.5504 (3) | 0.0082 (2) | 0.0642 (17) | |
H51 | −0.6326 | 1.5740 | −0.0244 | 0.077* | |
C52 | −0.6499 (4) | 1.5794 (3) | 0.0609 (2) | 0.0554 (15) | |
H52 | −0.6505 | 1.6220 | 0.0631 | 0.066* | |
C53 | −0.6600 (4) | 1.5445 (2) | 0.10960 (19) | 0.0396 (12) | |
C54 | −0.6586 (4) | 1.4823 (3) | 0.1051 (2) | 0.0481 (13) | |
H54 | −0.6656 | 1.4585 | 0.1376 | 0.058* | |
C55 | −0.6469 (4) | 1.4539 (3) | 0.0528 (2) | 0.0603 (16) | |
H55 | −0.6461 | 1.4113 | 0.0509 | 0.072* | |
C56 | −0.6700 (4) | 1.5759 (3) | 0.1645 (2) | 0.0422 (13) | |
C57 | −0.9602 (6) | 1.7813 (3) | 0.5804 (3) | 0.107 (3) | |
H57A | −0.9300 | 1.8170 | 0.5975 | 0.129* | |
H57B | −0.9508 | 1.7468 | 0.6053 | 0.129* | |
H57C | −1.0325 | 1.7881 | 0.5739 | 0.129* | |
C58 | −0.9086 (5) | 1.7683 (3) | 0.5240 (2) | 0.0660 (18) | |
C59 | −0.9486 (5) | 1.7922 (3) | 0.4738 (3) | 0.0722 (19) | |
H59 | −1.0056 | 1.8179 | 0.4749 | 0.087* | |
C60 | −0.9051 (4) | 1.7783 (2) | 0.4222 (2) | 0.0549 (15) | |
H60 | −0.9328 | 1.7947 | 0.3888 | 0.066* | |
C61 | −0.8206 (4) | 1.7403 (2) | 0.42008 (19) | 0.0401 (12) | |
C62 | −0.7794 (4) | 1.7170 (2) | 0.4702 (2) | 0.0553 (15) | |
H62 | −0.7220 | 1.6916 | 0.4694 | 0.066* | |
C63 | −0.8241 (5) | 1.7316 (3) | 0.5211 (2) | 0.0662 (18) | |
H63 | −0.7955 | 1.7160 | 0.5546 | 0.079* | |
C64 | −0.7768 (4) | 1.7203 (2) | 0.3650 (2) | 0.0375 (12) | |
C65 | −0.1870 (4) | 1.8615 (3) | 0.1711 (3) | 0.077 (2) | |
H65A | −0.1885 | 1.8568 | 0.1306 | 0.092* | |
H65B | −0.1240 | 1.8448 | 0.1863 | 0.092* | |
H65C | −0.1911 | 1.9042 | 0.1806 | 0.092* | |
C66 | −0.2772 (4) | 1.8280 (3) | 0.1963 (2) | 0.0538 (15) | |
C67 | −0.3661 (4) | 1.8580 (3) | 0.2092 (2) | 0.0550 (15) | |
H67 | −0.3694 | 1.9004 | 0.2052 | 0.066* | |
C68 | −0.4519 (4) | 1.8262 (2) | 0.2282 (2) | 0.0459 (13) | |
H68 | −0.5119 | 1.8475 | 0.2362 | 0.055* | |
C69 | −0.4491 (4) | 1.7637 (2) | 0.23522 (19) | 0.0384 (12) | |
C70 | −0.3585 (4) | 1.7343 (3) | 0.2241 (2) | 0.0552 (15) | |
H70 | −0.3539 | 1.6923 | 0.2303 | 0.066* | |
C71 | −0.2742 (4) | 1.7648 (3) | 0.2040 (2) | 0.0657 (17) | |
H71 | −0.2147 | 1.7431 | 0.1955 | 0.079* | |
C72 | −0.5408 (4) | 1.7287 (2) | 0.25388 (19) | 0.0385 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Eu1 | 0.03373 (15) | 0.02382 (13) | 0.03117 (13) | −0.00119 (11) | −0.00341 (10) | −0.00069 (10) |
Eu2 | 0.03153 (14) | 0.02376 (12) | 0.02997 (12) | 0.00012 (12) | 0.00014 (9) | −0.00014 (11) |
Eu3 | 0.03273 (15) | 0.02390 (13) | 0.03664 (14) | 0.00119 (12) | 0.00003 (10) | 0.00387 (10) |
O1 | 0.036 (2) | 0.038 (2) | 0.0388 (18) | 0.0004 (16) | −0.0131 (15) | −0.0010 (15) |
O2 | 0.039 (2) | 0.036 (2) | 0.058 (2) | −0.0063 (17) | −0.0107 (16) | 0.0102 (17) |
O3 | 0.045 (2) | 0.038 (2) | 0.053 (2) | −0.0055 (18) | 0.0103 (17) | −0.0046 (17) |
O4 | 0.033 (2) | 0.0328 (19) | 0.052 (2) | 0.0026 (16) | 0.0050 (16) | −0.0027 (16) |
O5 | 0.062 (3) | 0.049 (2) | 0.040 (2) | 0.018 (2) | −0.0023 (17) | 0.0041 (17) |
O6 | 0.037 (2) | 0.0301 (18) | 0.0287 (17) | −0.0013 (15) | 0.0044 (14) | 0.0001 (14) |
O7 | 0.041 (2) | 0.120 (4) | 0.057 (3) | −0.007 (2) | −0.0127 (19) | 0.046 (2) |
O8 | 0.080 (3) | 0.082 (3) | 0.051 (3) | −0.015 (3) | −0.020 (2) | −0.013 (2) |
O9 | 0.037 (2) | 0.035 (2) | 0.072 (2) | 0.0013 (17) | 0.0143 (17) | 0.0003 (18) |
O10 | 0.031 (2) | 0.035 (2) | 0.052 (2) | 0.0002 (16) | 0.0083 (16) | 0.0050 (16) |
O11 | 0.047 (2) | 0.049 (2) | 0.0359 (19) | −0.0184 (18) | 0.0000 (16) | −0.0006 (15) |
O12 | 0.0363 (19) | 0.0285 (18) | 0.0348 (18) | 0.0053 (15) | −0.0019 (14) | 0.0015 (14) |
O13 | 0.048 (2) | 0.055 (2) | 0.0335 (19) | −0.0066 (19) | 0.0041 (16) | 0.0072 (17) |
O14 | 0.075 (3) | 0.044 (2) | 0.058 (2) | −0.005 (2) | 0.025 (2) | −0.0068 (19) |
O15 | 0.079 (3) | 0.047 (2) | 0.046 (2) | 0.020 (2) | 0.000 (2) | −0.0036 (17) |
O16 | 0.045 (2) | 0.063 (2) | 0.037 (2) | 0.0019 (19) | 0.0060 (16) | 0.0159 (17) |
O17 | 0.031 (2) | 0.040 (2) | 0.072 (2) | 0.0018 (17) | 0.0005 (17) | 0.0160 (18) |
O18 | 0.0274 (19) | 0.0351 (19) | 0.049 (2) | 0.0022 (15) | −0.0014 (15) | 0.0032 (15) |
C1 | 0.061 (4) | 0.085 (5) | 0.053 (4) | 0.019 (4) | −0.007 (3) | 0.017 (3) |
C2 | 0.041 (3) | 0.055 (4) | 0.036 (3) | 0.017 (3) | −0.005 (2) | 0.001 (3) |
C3 | 0.055 (4) | 0.039 (3) | 0.054 (3) | 0.007 (3) | −0.006 (3) | 0.012 (3) |
C4 | 0.046 (3) | 0.048 (3) | 0.046 (3) | 0.006 (3) | −0.012 (3) | −0.001 (3) |
C5 | 0.034 (3) | 0.037 (3) | 0.032 (3) | 0.004 (2) | 0.004 (2) | 0.000 (2) |
C6 | 0.040 (3) | 0.045 (3) | 0.052 (3) | −0.001 (3) | −0.005 (3) | 0.002 (3) |
C7 | 0.035 (3) | 0.074 (4) | 0.044 (3) | 0.007 (3) | −0.013 (2) | −0.004 (3) |
C8 | 0.032 (3) | 0.037 (3) | 0.030 (3) | 0.009 (2) | 0.005 (2) | −0.003 (2) |
C9 | 0.075 (5) | 0.135 (7) | 0.067 (4) | −0.059 (5) | 0.013 (4) | −0.006 (4) |
C10 | 0.046 (4) | 0.086 (5) | 0.047 (3) | −0.029 (4) | 0.004 (3) | 0.003 (3) |
C11 | 0.049 (4) | 0.057 (4) | 0.069 (4) | −0.021 (3) | 0.001 (3) | −0.010 (3) |
C12 | 0.034 (3) | 0.048 (4) | 0.066 (4) | 0.003 (2) | 0.005 (3) | −0.005 (3) |
C13 | 0.031 (3) | 0.039 (3) | 0.039 (3) | 0.002 (2) | −0.001 (2) | 0.005 (2) |
C14 | 0.051 (4) | 0.065 (4) | 0.060 (4) | −0.011 (3) | 0.021 (3) | −0.010 (3) |
C15 | 0.054 (4) | 0.099 (6) | 0.069 (4) | −0.014 (4) | 0.019 (3) | −0.016 (4) |
C16 | 0.036 (3) | 0.036 (3) | 0.037 (3) | −0.001 (2) | −0.009 (2) | 0.005 (2) |
C17 | 0.082 (5) | 0.091 (5) | 0.047 (4) | −0.020 (4) | 0.018 (3) | −0.012 (3) |
C18 | 0.057 (4) | 0.056 (4) | 0.043 (3) | −0.015 (3) | 0.010 (3) | −0.007 (3) |
C19 | 0.058 (4) | 0.057 (4) | 0.055 (4) | 0.004 (3) | 0.013 (3) | 0.000 (3) |
C20 | 0.057 (4) | 0.052 (4) | 0.041 (3) | 0.003 (3) | 0.012 (3) | 0.008 (3) |
C21 | 0.046 (3) | 0.037 (3) | 0.033 (3) | −0.005 (3) | 0.002 (2) | −0.005 (2) |
C22 | 0.067 (4) | 0.065 (4) | 0.039 (3) | 0.010 (3) | −0.003 (3) | 0.008 (3) |
C23 | 0.077 (5) | 0.085 (5) | 0.029 (3) | 0.003 (4) | 0.000 (3) | 0.007 (3) |
C24 | 0.038 (3) | 0.039 (3) | 0.033 (3) | −0.009 (3) | −0.003 (2) | −0.001 (2) |
C25 | 0.091 (5) | 0.088 (5) | 0.050 (4) | −0.042 (4) | −0.013 (3) | 0.000 (3) |
C26 | 0.048 (4) | 0.059 (4) | 0.035 (3) | −0.020 (3) | −0.001 (2) | 0.008 (3) |
C27 | 0.035 (3) | 0.057 (4) | 0.060 (4) | 0.001 (3) | −0.010 (3) | 0.005 (3) |
C28 | 0.038 (3) | 0.041 (3) | 0.048 (3) | 0.005 (3) | −0.005 (2) | −0.009 (2) |
C29 | 0.034 (3) | 0.045 (3) | 0.031 (3) | −0.003 (3) | −0.001 (2) | 0.006 (2) |
C30 | 0.059 (4) | 0.052 (4) | 0.051 (3) | 0.019 (3) | −0.015 (3) | 0.003 (3) |
C31 | 0.089 (5) | 0.040 (3) | 0.058 (4) | 0.008 (3) | 0.003 (3) | −0.007 (3) |
C32 | 0.037 (3) | 0.089 (5) | 0.027 (3) | −0.015 (3) | −0.005 (2) | 0.016 (3) |
C33 | 0.097 (6) | 0.152 (8) | 0.073 (5) | 0.069 (6) | −0.001 (4) | −0.027 (5) |
C34 | 0.053 (4) | 0.096 (6) | 0.053 (4) | 0.033 (4) | −0.001 (3) | −0.019 (4) |
C35 | 0.038 (4) | 0.123 (6) | 0.063 (4) | 0.004 (4) | 0.016 (3) | −0.009 (4) |
C36 | 0.043 (4) | 0.061 (4) | 0.065 (4) | −0.006 (3) | 0.009 (3) | −0.004 (3) |
C37 | 0.033 (3) | 0.044 (3) | 0.040 (3) | 0.008 (3) | 0.000 (2) | −0.001 (2) |
C38 | 0.041 (3) | 0.048 (3) | 0.053 (3) | 0.010 (3) | 0.000 (3) | −0.001 (3) |
C39 | 0.062 (4) | 0.058 (4) | 0.072 (4) | 0.023 (4) | −0.009 (3) | −0.008 (3) |
C40 | 0.038 (3) | 0.041 (3) | 0.030 (3) | 0.002 (3) | −0.004 (2) | 0.001 (2) |
C41 | 0.094 (5) | 0.091 (5) | 0.071 (4) | 0.016 (4) | −0.039 (4) | −0.032 (4) |
C42 | 0.065 (4) | 0.051 (4) | 0.050 (4) | 0.011 (3) | −0.026 (3) | −0.019 (3) |
C43 | 0.067 (4) | 0.059 (4) | 0.034 (3) | 0.011 (3) | −0.005 (3) | −0.008 (3) |
C44 | 0.053 (4) | 0.054 (4) | 0.038 (3) | 0.002 (3) | −0.004 (3) | −0.009 (2) |
C45 | 0.041 (3) | 0.032 (3) | 0.039 (3) | 0.005 (2) | −0.007 (2) | 0.000 (2) |
C46 | 0.050 (4) | 0.045 (3) | 0.053 (3) | −0.001 (3) | −0.011 (3) | 0.004 (3) |
C47 | 0.057 (4) | 0.051 (4) | 0.071 (4) | −0.010 (3) | −0.023 (3) | −0.009 (3) |
C48 | 0.035 (3) | 0.033 (3) | 0.034 (3) | 0.008 (2) | −0.001 (2) | −0.004 (2) |
C49 | 0.067 (5) | 0.185 (8) | 0.051 (4) | 0.018 (5) | −0.004 (3) | −0.042 (5) |
C50 | 0.040 (3) | 0.098 (5) | 0.045 (4) | 0.006 (4) | −0.004 (3) | −0.012 (4) |
C51 | 0.053 (4) | 0.099 (5) | 0.041 (4) | 0.002 (4) | 0.006 (3) | 0.012 (4) |
C52 | 0.058 (4) | 0.061 (4) | 0.048 (3) | 0.004 (3) | 0.014 (3) | 0.011 (3) |
C53 | 0.041 (3) | 0.044 (3) | 0.033 (3) | 0.002 (3) | 0.004 (2) | 0.004 (2) |
C54 | 0.048 (3) | 0.057 (4) | 0.039 (3) | 0.000 (3) | −0.005 (2) | 0.001 (3) |
C55 | 0.061 (4) | 0.059 (4) | 0.061 (4) | 0.008 (3) | −0.006 (3) | −0.016 (3) |
C56 | 0.034 (3) | 0.058 (4) | 0.035 (3) | 0.002 (3) | 0.003 (2) | 0.005 (3) |
C57 | 0.165 (8) | 0.102 (6) | 0.057 (4) | 0.010 (6) | 0.041 (5) | −0.003 (4) |
C58 | 0.098 (5) | 0.062 (4) | 0.038 (3) | −0.013 (4) | 0.018 (3) | −0.004 (3) |
C59 | 0.086 (5) | 0.064 (4) | 0.067 (4) | 0.022 (4) | 0.024 (4) | −0.004 (3) |
C60 | 0.074 (4) | 0.045 (3) | 0.046 (3) | 0.007 (3) | 0.004 (3) | 0.009 (3) |
C61 | 0.051 (3) | 0.035 (3) | 0.034 (3) | −0.003 (3) | 0.006 (2) | 0.003 (2) |
C62 | 0.072 (4) | 0.052 (4) | 0.042 (3) | 0.005 (3) | −0.006 (3) | 0.000 (3) |
C63 | 0.091 (5) | 0.075 (5) | 0.033 (3) | −0.004 (4) | −0.003 (3) | 0.001 (3) |
C64 | 0.043 (3) | 0.031 (3) | 0.038 (3) | −0.009 (3) | −0.003 (2) | 0.003 (2) |
C65 | 0.050 (4) | 0.098 (5) | 0.083 (5) | −0.028 (4) | 0.012 (3) | 0.003 (4) |
C66 | 0.047 (4) | 0.062 (4) | 0.052 (3) | −0.016 (3) | −0.003 (3) | 0.004 (3) |
C67 | 0.050 (4) | 0.043 (3) | 0.072 (4) | −0.011 (3) | −0.005 (3) | 0.008 (3) |
C68 | 0.029 (3) | 0.051 (3) | 0.057 (3) | 0.000 (3) | −0.002 (2) | 0.004 (3) |
C69 | 0.029 (3) | 0.046 (3) | 0.040 (3) | 0.002 (3) | −0.004 (2) | 0.003 (2) |
C70 | 0.046 (4) | 0.048 (4) | 0.071 (4) | 0.008 (3) | 0.007 (3) | 0.013 (3) |
C71 | 0.028 (3) | 0.086 (5) | 0.084 (5) | 0.009 (3) | 0.018 (3) | 0.007 (4) |
C72 | 0.043 (3) | 0.036 (3) | 0.036 (3) | 0.001 (3) | 0.000 (2) | −0.001 (2) |
Eu1—O7 | 2.351 (4) | C9—C10 | 1.510 (7) |
Eu1—O16i | 2.380 (3) | C10—C15 | 1.376 (8) |
Eu1—O18i | 2.407 (3) | C10—C11 | 1.382 (7) |
Eu1—O3 | 2.413 (3) | C11—C12 | 1.392 (7) |
Eu1—O2 | 2.443 (3) | C12—C13 | 1.378 (6) |
Eu1—O5 | 2.450 (3) | C13—C14 | 1.375 (6) |
Eu1—O6 | 2.527 (3) | C13—C16 | 1.479 (6) |
Eu1—O1 | 2.549 (3) | C14—C15 | 1.366 (7) |
Eu1—O4 | 2.610 (3) | C17—C18 | 1.509 (7) |
Eu1—C8 | 2.870 (4) | C18—C23 | 1.364 (7) |
Eu1—C24 | 2.880 (5) | C18—C19 | 1.387 (7) |
Eu1—C16 | 2.895 (5) | C19—C20 | 1.373 (7) |
Eu2—O13 | 2.343 (3) | C20—C21 | 1.374 (7) |
Eu2—O6 | 2.353 (3) | C21—C22 | 1.390 (6) |
Eu2—O8 | 2.382 (4) | C21—C24 | 1.479 (6) |
Eu2—O4 | 2.393 (3) | C22—C23 | 1.396 (7) |
Eu2—O11 | 2.415 (3) | C25—C26 | 1.530 (6) |
Eu2—O9 | 2.422 (3) | C26—C31 | 1.372 (7) |
Eu2—O12 | 2.573 (3) | C26—C27 | 1.380 (7) |
Eu2—O10 | 2.581 (3) | C27—C28 | 1.376 (6) |
Eu2—C48 | 2.879 (4) | C28—C29 | 1.384 (6) |
Eu2—C40 | 2.895 (5) | C29—C30 | 1.355 (6) |
Eu2—O7 | 2.963 (5) | C29—C32 | 1.508 (7) |
Eu2—C32 | 3.027 (6) | C30—C31 | 1.380 (7) |
Eu3—O1ii | 2.344 (3) | C33—C34 | 1.516 (8) |
Eu3—O15 | 2.377 (3) | C34—C39 | 1.368 (8) |
Eu3—O10 | 2.378 (3) | C34—C35 | 1.376 (8) |
Eu3—O12 | 2.399 (3) | C35—C36 | 1.380 (8) |
Eu3—O17 | 2.403 (3) | C36—C37 | 1.392 (7) |
Eu3—O14 | 2.452 (3) | C37—C38 | 1.376 (6) |
Eu3—O18 | 2.528 (3) | C37—C40 | 1.476 (6) |
Eu3—O13 | 2.629 (3) | C38—C39 | 1.386 (7) |
Eu3—O16 | 2.739 (3) | C41—C42 | 1.516 (7) |
Eu3—C72 | 2.830 (5) | C42—C43 | 1.373 (7) |
Eu3—C56 | 2.933 (5) | C42—C47 | 1.376 (7) |
Eu3—C64 | 2.936 (5) | C43—C44 | 1.391 (6) |
O1—C8 | 1.282 (5) | C44—C45 | 1.372 (6) |
O1—Eu3i | 2.344 (3) | C45—C46 | 1.382 (6) |
O2—C8 | 1.250 (5) | C45—C48 | 1.485 (6) |
O3—C16 | 1.257 (5) | C46—C47 | 1.390 (7) |
O4—C16 | 1.279 (5) | C49—C50 | 1.517 (7) |
O5—C24 | 1.243 (5) | C50—C51 | 1.372 (8) |
O6—C24 | 1.301 (5) | C50—C55 | 1.377 (8) |
O7—C32 | 1.270 (6) | C51—C52 | 1.402 (7) |
O8—C32 | 1.229 (7) | C52—C53 | 1.385 (6) |
O9—C40 | 1.254 (5) | C53—C54 | 1.362 (6) |
O10—C40 | 1.281 (5) | C53—C56 | 1.471 (6) |
O11—C48 | 1.242 (5) | C54—C55 | 1.388 (7) |
O12—C48 | 1.299 (5) | C57—C58 | 1.522 (7) |
O13—C56 | 1.279 (5) | C58—C63 | 1.361 (8) |
O14—C56 | 1.249 (6) | C58—C59 | 1.386 (8) |
O15—C64 | 1.243 (5) | C59—C60 | 1.382 (7) |
O16—C64 | 1.271 (5) | C60—C61 | 1.377 (7) |
O16—Eu1ii | 2.380 (3) | C61—C62 | 1.384 (6) |
O17—C72 | 1.255 (5) | C61—C64 | 1.488 (6) |
O18—C72 | 1.285 (5) | C62—C63 | 1.378 (7) |
O18—Eu1ii | 2.407 (3) | C65—C66 | 1.509 (7) |
C1—C2 | 1.512 (6) | C66—C67 | 1.366 (7) |
C2—C3 | 1.368 (7) | C66—C71 | 1.392 (7) |
C2—C7 | 1.377 (7) | C67—C68 | 1.392 (7) |
C3—C4 | 1.390 (6) | C68—C69 | 1.374 (6) |
C4—C5 | 1.374 (6) | C69—C70 | 1.370 (6) |
C5—C6 | 1.387 (6) | C69—C72 | 1.486 (6) |
C5—C8 | 1.478 (6) | C70—C71 | 1.371 (7) |
C6—C7 | 1.393 (6) | ||
O7—Eu1—O16i | 87.07 (14) | O10—Eu3—C64 | 84.60 (12) |
O7—Eu1—O18i | 83.99 (12) | O12—Eu3—C64 | 95.35 (12) |
O16i—Eu1—O18i | 73.26 (11) | O17—Eu3—C64 | 97.15 (13) |
O7—Eu1—O3 | 81.16 (12) | O14—Eu3—C64 | 156.99 (13) |
O16i—Eu1—O3 | 76.57 (11) | O18—Eu3—C64 | 77.09 (11) |
O18i—Eu1—O3 | 146.90 (11) | O13—Eu3—C64 | 151.55 (11) |
O7—Eu1—O2 | 153.53 (12) | O16—Eu3—C64 | 25.58 (11) |
O16i—Eu1—O2 | 93.59 (11) | C72—Eu3—C64 | 89.60 (13) |
O18i—Eu1—O2 | 121.55 (10) | C56—Eu3—C64 | 173.18 (13) |
O3—Eu1—O2 | 73.30 (11) | C8—O1—Eu3i | 161.7 (3) |
O7—Eu1—O5 | 121.96 (13) | C8—O1—Eu1 | 90.8 (3) |
O16i—Eu1—O5 | 139.71 (12) | Eu3i—O1—Eu1 | 100.27 (10) |
O18i—Eu1—O5 | 82.11 (11) | C8—O2—Eu1 | 96.6 (3) |
O3—Eu1—O5 | 130.67 (12) | C16—O3—Eu1 | 99.3 (3) |
O2—Eu1—O5 | 72.62 (12) | C16—O4—Eu2 | 142.8 (3) |
O7—Eu1—O6 | 70.56 (12) | C16—O4—Eu1 | 89.5 (3) |
O16i—Eu1—O6 | 149.65 (10) | Eu2—O4—Eu1 | 99.81 (11) |
O18i—Eu1—O6 | 83.94 (10) | C24—O5—Eu1 | 97.1 (3) |
O3—Eu1—O6 | 118.03 (10) | C24—O6—Eu2 | 140.8 (3) |
O2—Eu1—O6 | 115.64 (10) | C24—O6—Eu1 | 91.9 (3) |
O5—Eu1—O6 | 52.10 (10) | Eu2—O6—Eu1 | 103.34 (10) |
O7—Eu1—O1 | 148.46 (12) | C32—O7—Eu1 | 152.9 (3) |
O16i—Eu1—O1 | 68.03 (11) | C32—O7—Eu2 | 80.6 (4) |
O18i—Eu1—O1 | 70.82 (10) | Eu1—O7—Eu2 | 91.46 (12) |
O3—Eu1—O1 | 109.83 (11) | C32—O8—Eu2 | 109.8 (4) |
O2—Eu1—O1 | 51.98 (10) | C40—O9—Eu2 | 98.9 (3) |
O5—Eu1—O1 | 74.03 (10) | C40—O10—Eu3 | 168.5 (3) |
O6—Eu1—O1 | 123.15 (10) | C40—O10—Eu2 | 90.7 (3) |
O7—Eu1—O4 | 72.62 (12) | Eu3—O10—Eu2 | 98.29 (11) |
O16i—Eu1—O4 | 125.88 (11) | C48—O11—Eu2 | 98.7 (3) |
O18i—Eu1—O4 | 147.67 (10) | C48—O12—Eu3 | 138.0 (3) |
O3—Eu1—O4 | 51.46 (10) | C48—O12—Eu2 | 89.8 (3) |
O2—Eu1—O4 | 85.84 (10) | Eu3—O12—Eu2 | 97.99 (10) |
O5—Eu1—O4 | 91.49 (11) | C56—O13—Eu2 | 171.2 (3) |
O6—Eu1—O4 | 67.58 (10) | C56—O13—Eu3 | 90.5 (3) |
O1—Eu1—O4 | 137.64 (10) | Eu2—O13—Eu3 | 97.88 (11) |
O7—Eu1—C8 | 168.76 (14) | C56—O14—Eu3 | 99.7 (3) |
O16i—Eu1—C8 | 82.24 (12) | C64—O15—Eu3 | 104.0 (3) |
O18i—Eu1—C8 | 96.16 (12) | C64—O16—Eu1ii | 150.4 (3) |
O3—Eu1—C8 | 92.95 (12) | C64—O16—Eu3 | 85.9 (3) |
O2—Eu1—C8 | 25.64 (11) | Eu1ii—O16—Eu3 | 94.22 (11) |
O5—Eu1—C8 | 69.07 (12) | C72—O17—Eu3 | 96.2 (3) |
O6—Eu1—C8 | 120.67 (10) | C72—O18—Eu1ii | 170.8 (3) |
O1—Eu1—C8 | 26.53 (11) | C72—O18—Eu3 | 89.7 (3) |
O4—Eu1—C8 | 111.12 (12) | Eu1ii—O18—Eu3 | 99.19 (11) |
O7—Eu1—C24 | 96.76 (14) | C3—C2—C7 | 118.4 (5) |
O16i—Eu1—C24 | 153.12 (12) | C3—C2—C1 | 121.4 (5) |
O18i—Eu1—C24 | 80.67 (12) | C7—C2—C1 | 120.3 (5) |
O3—Eu1—C24 | 130.30 (12) | C2—C3—C4 | 120.7 (5) |
O2—Eu1—C24 | 94.50 (12) | C5—C4—C3 | 121.3 (5) |
O5—Eu1—C24 | 25.35 (11) | C4—C5—C6 | 118.4 (4) |
O6—Eu1—C24 | 26.83 (11) | C4—C5—C8 | 121.5 (4) |
O1—Eu1—C24 | 97.50 (12) | C6—C5—C8 | 119.9 (4) |
O4—Eu1—C24 | 80.29 (12) | C5—C6—C7 | 119.8 (5) |
C8—Eu1—C24 | 94.35 (13) | C2—C7—C6 | 121.5 (5) |
O7—Eu1—C16 | 77.26 (13) | O2—C8—O1 | 119.7 (4) |
O16i—Eu1—C16 | 101.41 (13) | O2—C8—C5 | 120.8 (4) |
O18i—Eu1—C16 | 160.80 (11) | O1—C8—C5 | 119.4 (4) |
O3—Eu1—C16 | 25.37 (11) | O2—C8—Eu1 | 57.7 (2) |
O2—Eu1—C16 | 76.67 (12) | O1—C8—Eu1 | 62.6 (2) |
O5—Eu1—C16 | 111.31 (13) | C5—C8—Eu1 | 170.7 (3) |
O6—Eu1—C16 | 93.56 (12) | C15—C10—C11 | 117.8 (5) |
O1—Eu1—C16 | 125.08 (12) | C15—C10—C9 | 121.7 (6) |
O4—Eu1—C16 | 26.20 (11) | C11—C10—C9 | 120.4 (6) |
C8—Eu1—C16 | 101.43 (13) | C10—C11—C12 | 120.6 (5) |
C24—Eu1—C16 | 105.40 (14) | C13—C12—C11 | 120.5 (5) |
O13—Eu2—O6 | 154.11 (11) | C14—C13—C12 | 118.4 (5) |
O13—Eu2—O8 | 82.23 (13) | C14—C13—C16 | 119.9 (5) |
O6—Eu2—O8 | 88.10 (12) | C12—C13—C16 | 121.7 (5) |
O13—Eu2—O4 | 86.85 (11) | C15—C14—C13 | 121.0 (6) |
O6—Eu2—O4 | 74.04 (10) | C14—C15—C10 | 121.7 (6) |
O8—Eu2—O4 | 110.27 (13) | O3—C16—O4 | 119.3 (4) |
O13—Eu2—O11 | 120.00 (11) | O3—C16—C13 | 119.6 (5) |
O6—Eu2—O11 | 77.12 (10) | O4—C16—C13 | 121.1 (4) |
O8—Eu2—O11 | 153.24 (13) | O3—C16—Eu1 | 55.3 (2) |
O4—Eu2—O11 | 87.20 (11) | O4—C16—Eu1 | 64.3 (2) |
O13—Eu2—O9 | 115.73 (11) | C13—C16—Eu1 | 171.6 (3) |
O6—Eu2—O9 | 83.77 (11) | C23—C18—C19 | 117.7 (5) |
O8—Eu2—O9 | 72.97 (14) | C23—C18—C17 | 121.5 (5) |
O4—Eu2—O9 | 157.32 (11) | C19—C18—C17 | 120.7 (6) |
O11—Eu2—O9 | 83.23 (11) | C20—C19—C18 | 121.4 (6) |
O13—Eu2—O12 | 68.01 (10) | C19—C20—C21 | 120.6 (5) |
O6—Eu2—O12 | 124.90 (9) | C20—C21—C22 | 119.1 (5) |
O8—Eu2—O12 | 146.99 (12) | C20—C21—C24 | 121.3 (4) |
O4—Eu2—O12 | 82.87 (10) | C22—C21—C24 | 119.6 (5) |
O11—Eu2—O12 | 52.01 (10) | C21—C22—C23 | 119.1 (5) |
O9—Eu2—O12 | 106.76 (10) | C18—C23—C22 | 122.0 (5) |
O13—Eu2—O10 | 71.03 (11) | O5—C24—O6 | 118.6 (4) |
O6—Eu2—O10 | 133.31 (10) | O5—C24—C21 | 122.5 (4) |
O8—Eu2—O10 | 90.55 (13) | O6—C24—C21 | 118.9 (4) |
O4—Eu2—O10 | 147.47 (10) | O5—C24—Eu1 | 57.6 (2) |
O11—Eu2—O10 | 83.89 (10) | O6—C24—Eu1 | 61.3 (2) |
O9—Eu2—O10 | 51.59 (10) | C21—C24—Eu1 | 172.2 (3) |
O12—Eu2—O10 | 67.04 (9) | C31—C26—C27 | 118.9 (5) |
O13—Eu2—C48 | 94.83 (13) | C31—C26—C25 | 121.3 (5) |
O6—Eu2—C48 | 99.97 (12) | C27—C26—C25 | 119.8 (5) |
O8—Eu2—C48 | 165.86 (14) | C28—C27—C26 | 120.7 (5) |
O4—Eu2—C48 | 83.26 (11) | C27—C28—C29 | 120.0 (5) |
O11—Eu2—C48 | 25.23 (11) | C30—C29—C28 | 118.9 (5) |
O9—Eu2—C48 | 96.22 (12) | C30—C29—C32 | 122.3 (5) |
O12—Eu2—C48 | 26.84 (11) | C28—C29—C32 | 118.8 (5) |
O10—Eu2—C48 | 75.45 (11) | C29—C30—C31 | 121.6 (5) |
O13—Eu2—C40 | 93.89 (13) | C26—C31—C30 | 119.8 (5) |
O6—Eu2—C40 | 108.25 (12) | O8—C32—O7 | 122.4 (5) |
O8—Eu2—C40 | 80.81 (14) | O8—C32—C29 | 120.2 (5) |
O4—Eu2—C40 | 168.87 (12) | O7—C32—C29 | 117.3 (6) |
O11—Eu2—C40 | 82.81 (12) | O8—C32—Eu2 | 47.8 (3) |
O9—Eu2—C40 | 25.33 (12) | O7—C32—Eu2 | 75.0 (3) |
O12—Eu2—C40 | 87.10 (12) | C29—C32—Eu2 | 165.5 (4) |
O10—Eu2—C40 | 26.26 (11) | C39—C34—C35 | 118.6 (6) |
C48—Eu2—C40 | 85.61 (12) | C39—C34—C33 | 120.9 (7) |
O13—Eu2—O7 | 93.59 (11) | C35—C34—C33 | 120.5 (7) |
O6—Eu2—O7 | 62.87 (9) | C34—C35—C36 | 120.7 (6) |
O8—Eu2—O7 | 46.84 (12) | C35—C36—C37 | 120.8 (6) |
O4—Eu2—O7 | 65.72 (10) | C38—C37—C36 | 118.1 (5) |
O11—Eu2—O7 | 136.04 (10) | C38—C37—C40 | 121.6 (5) |
O9—Eu2—O7 | 108.34 (11) | C36—C37—C40 | 120.3 (5) |
O12—Eu2—O7 | 144.75 (10) | C37—C38—C39 | 120.5 (5) |
O10—Eu2—O7 | 136.95 (10) | C34—C39—C38 | 121.3 (6) |
C48—Eu2—O7 | 147.30 (11) | O9—C40—O10 | 118.8 (4) |
C40—Eu2—O7 | 125.24 (12) | O9—C40—C37 | 119.8 (5) |
O13—Eu2—C32 | 88.81 (12) | O10—C40—C37 | 121.4 (4) |
O6—Eu2—C32 | 73.95 (12) | O9—C40—Eu2 | 55.7 (2) |
O8—Eu2—C32 | 22.46 (14) | O10—C40—Eu2 | 63.1 (2) |
O4—Eu2—C32 | 89.35 (14) | C37—C40—Eu2 | 175.5 (4) |
O11—Eu2—C32 | 150.69 (13) | C43—C42—C47 | 118.3 (5) |
O9—Eu2—C32 | 89.03 (14) | C43—C42—C41 | 121.4 (6) |
O12—Eu2—C32 | 155.83 (12) | C47—C42—C41 | 120.2 (6) |
O10—Eu2—C32 | 112.97 (14) | C42—C43—C44 | 121.3 (5) |
C48—Eu2—C32 | 171.55 (15) | C45—C44—C43 | 120.0 (5) |
C40—Eu2—C32 | 101.77 (15) | C44—C45—C46 | 119.2 (5) |
O7—Eu2—C32 | 24.46 (12) | C44—C45—C48 | 119.3 (5) |
O1ii—Eu3—O15 | 114.49 (12) | C46—C45—C48 | 121.5 (4) |
O1ii—Eu3—O10 | 81.50 (11) | C45—C46—C47 | 120.0 (5) |
O15—Eu3—O10 | 88.27 (12) | C42—C47—C46 | 121.0 (6) |
O1ii—Eu3—O12 | 153.33 (11) | O11—C48—O12 | 119.2 (4) |
O15—Eu3—O12 | 73.47 (11) | O11—C48—C45 | 121.0 (4) |
O10—Eu3—O12 | 73.14 (10) | O12—C48—C45 | 119.8 (4) |
O1ii—Eu3—O17 | 120.62 (11) | O11—C48—Eu2 | 56.0 (2) |
O15—Eu3—O17 | 84.76 (13) | O12—C48—Eu2 | 63.4 (2) |
O10—Eu3—O17 | 157.71 (11) | C45—C48—Eu2 | 173.5 (3) |
O12—Eu3—O17 | 84.58 (10) | C51—C50—C55 | 118.0 (6) |
O1ii—Eu3—O14 | 76.19 (12) | C51—C50—C49 | 120.7 (6) |
O15—Eu3—O14 | 159.60 (14) | C55—C50—C49 | 121.4 (7) |
O10—Eu3—O14 | 111.07 (12) | C50—C51—C52 | 121.3 (6) |
O12—Eu3—O14 | 105.13 (11) | C53—C52—C51 | 119.8 (6) |
O17—Eu3—O14 | 74.88 (12) | C54—C53—C52 | 118.8 (5) |
O1ii—Eu3—O18 | 72.18 (10) | C54—C53—C56 | 122.3 (5) |
O15—Eu3—O18 | 85.83 (11) | C52—C53—C56 | 118.9 (5) |
O10—Eu3—O18 | 147.59 (10) | C53—C54—C55 | 121.1 (5) |
O12—Eu3—O18 | 134.48 (10) | C50—C55—C54 | 121.1 (6) |
O17—Eu3—O18 | 52.90 (10) | O14—C56—O13 | 118.8 (5) |
O14—Eu3—O18 | 81.05 (11) | O14—C56—C53 | 121.7 (5) |
O1ii—Eu3—O13 | 97.47 (10) | O13—C56—C53 | 119.5 (5) |
O15—Eu3—O13 | 138.10 (11) | O14—C56—Eu3 | 55.5 (3) |
O10—Eu3—O13 | 69.67 (10) | O13—C56—Eu3 | 63.7 (3) |
O12—Eu3—O13 | 66.31 (10) | C53—C56—Eu3 | 172.4 (4) |
O17—Eu3—O13 | 102.21 (11) | C63—C58—C59 | 118.1 (5) |
O14—Eu3—O13 | 50.58 (11) | C63—C58—C57 | 121.3 (6) |
O18—Eu3—O13 | 131.33 (10) | C59—C58—C57 | 120.6 (7) |
O1ii—Eu3—O16 | 65.26 (10) | C60—C59—C58 | 121.0 (6) |
O15—Eu3—O16 | 49.58 (10) | C61—C60—C59 | 120.0 (5) |
O10—Eu3—O16 | 86.61 (10) | C60—C61—C62 | 119.3 (5) |
O12—Eu3—O16 | 120.07 (10) | C60—C61—C64 | 121.5 (4) |
O17—Eu3—O16 | 104.55 (11) | C62—C61—C64 | 119.1 (5) |
O14—Eu3—O16 | 134.67 (11) | C63—C62—C61 | 119.6 (6) |
O18—Eu3—O16 | 65.54 (10) | C58—C63—C62 | 122.0 (5) |
O13—Eu3—O16 | 152.94 (10) | O15—C64—O16 | 119.4 (5) |
O1ii—Eu3—C72 | 95.81 (12) | O15—C64—C61 | 120.1 (4) |
O15—Eu3—C72 | 87.55 (13) | O16—C64—C61 | 120.4 (5) |
O10—Eu3—C72 | 173.58 (12) | O15—C64—Eu3 | 51.8 (2) |
O12—Eu3—C72 | 110.24 (12) | O16—C64—Eu3 | 68.5 (3) |
O17—Eu3—C72 | 26.16 (11) | C61—C64—Eu3 | 164.6 (3) |
O14—Eu3—C72 | 73.70 (13) | C67—C66—C71 | 118.0 (5) |
O18—Eu3—C72 | 27.02 (11) | C67—C66—C65 | 121.2 (6) |
O13—Eu3—C72 | 116.58 (12) | C71—C66—C65 | 120.7 (6) |
O16—Eu3—C72 | 86.97 (12) | C66—C67—C68 | 121.0 (5) |
O1ii—Eu3—C56 | 84.92 (12) | C69—C68—C67 | 121.0 (5) |
O15—Eu3—C56 | 159.97 (13) | C70—C69—C68 | 117.5 (5) |
O10—Eu3—C56 | 89.93 (13) | C70—C69—C72 | 120.7 (5) |
O12—Eu3—C56 | 86.92 (12) | C68—C69—C72 | 121.7 (5) |
O17—Eu3—C56 | 89.46 (13) | C69—C70—C71 | 122.1 (5) |
O14—Eu3—C56 | 24.82 (12) | C70—C71—C66 | 120.3 (5) |
O18—Eu3—C56 | 105.85 (13) | O17—C72—O18 | 119.9 (4) |
O13—Eu3—C56 | 25.85 (11) | O17—C72—C69 | 120.1 (4) |
O16—Eu3—C56 | 150.16 (12) | O18—C72—C69 | 119.9 (4) |
C72—Eu3—C56 | 95.66 (14) | O17—C72—Eu3 | 57.6 (2) |
O1ii—Eu3—C64 | 90.24 (12) | O18—C72—Eu3 | 63.3 (2) |
O15—Eu3—C64 | 24.26 (12) | C69—C72—Eu3 | 167.5 (3) |
Symmetry codes: (i) −x−3/2, y−1/2, −z+1/2; (ii) −x−3/2, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Eu3(C8H7O2)9] |
Mr | 1672.10 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 298 |
a, b, c (Å) | 12.988 (1), 21.823 (2), 23.542 (4) |
β (°) | 90.84 (1) |
V (Å3) | 6672.0 (14) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.86 |
Crystal size (mm) | 0.32 × 0.20 × 0.18 |
Data collection | |
Diffractometer | Siemens P4 diffractometer |
Absorption correction | Empirical (using intensity measurements) (Kopfman & Huber, 1968) |
Tmin, Tmax | 0.571, 0.629 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13082, 11743, 8293 |
Rint | 0.020 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.060, 0.90 |
No. of reflections | 11743 |
No. of parameters | 848 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.81, −0.55 |
Computer programs: XSCANS (Fait, 1991), XSCANS, SHELXTL (Sheldrick, 1997a), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997b), SHELXTL.
Eu2—O13 | 2.343 (3) | Eu2—O9 | 2.422 (3) |
Eu2—O6 | 2.353 (3) | Eu2—O12 | 2.573 (3) |
Eu2—O8 | 2.382 (4) | Eu2—O10 | 2.581 (3) |
Eu2—O4 | 2.393 (3) | Eu2—O7 | 2.963 (5) |
Eu2—O11 | 2.415 (3) | Eu2—C32 | 3.027 (6) |
O5—Eu1—O6 | 52.10 (10) | Eu2—O6—Eu1 | 103.34 (10) |
O15—Eu3—O14 | 159.60 (14) | O5—C24—O6 | 118.6 (4) |
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Rare earth carboxylate complexes have many special structures and interesting luminescent properties. The carboxylate groups may be coordinated simultaneously to metal ions in three modes, viz. bridging, chelating and bridging–chelating. The europium luminescent probe has been widely used in the local structure determination of crystalline materials. Our interest has focused on the crystal structures of europium complexes and their high-resolution laser-exited excitation and emission spectra. We report here a new europium complex, [Eu(C8H7O2)3]3n, (I) (Fig. 1).
In (I), each Eu atom is coordinated by nine O atoms from six different carboxylate groups, and all the carboxylate groups are coordinated in bridging–chelating modes, with two O atoms chelating one Eu3+ ion to form a tridentate bridge. Three Eu3+ ions, linked by three carboxylate groups, form a trimeric unit. Theses trimeric units are then linked to one another along the b axis by three bridging–chelating carboxylates to form an infinite one-dimensional polymer chain.
Most of the Eu—O bond lengths [range 2.343 (3)–2.963 (5) Å] agree with those in the similar compound Eu2(p-CH3C6H4COO)6(2,2'-bipy), (II) (Wang et al., 1995), but the Eu2—O7 bond length is significantly larger than the Eu—O bond in (II). The difference may be due to their different chelating modes.
From the Eu1—C8, Eu1—C24, Eu1—C16, Eu2—C48, Eu2—C40 and Eu3—C72 distances [range 2.830 (5)–2.895 (5) Å], we can see that the bond between the Eu and C atoms is very weak, and no chemical bond exists between Eu3 and C56 (or C64) or between Eu2 and C32. The Eu···Eu distance, when the atoms are bridged by four bidentate carboxylate groups, is longer than when they are bridged by three carboxylate groups, as in the present case.
The O—Eu—O angles in (I) vary from 49.58 (10) to 159.60 (14)°, in agreement with those in (II).
In most complexes containing MBA or MOBA (MBA is methylbenzonic acid and MOBA is methoxybenzonic acid), the Eu atoms are eight-coordinated by bidentate carboxylate ligands, as in (II), [Eu2(p-MBA)6(phen)2] [(III); Jin et al., 1994; phen is phenanthroline], [Eu(m-MOBA)3(2,2'-bipy)] [(IV); Li, Zheng et al., 2000; 2,2'-bipy is 2,2'-bipyridine], [Eu(m-MOBA)3(H2O)2].0.5(4,4'-bipy) [(V); Li, Bian et al., 2000; 4,4'-bipy is 4,4'-bipyridine] and [Eu(m-MBA)3(H2O)2], (VI). Complex (I) may be a unique complex of this type where Eu is nine-coordinated.
It should also be noted that there are no hydrogen bonds in (I), while many Eu complexes, such as (V) and (VI), contain hydrogen bonds which can stabilize the complexes.
Complexes (I) and (II) show that the coordinating ability of phen, 2,2'-bipy, p-MBA and p-MOBA is stronger than that of H2O; (V) and (VI) show that m-MOBA, m-MBA and H2O may have similar coordinating ability; and (I) and (IV) show that 4,4'-bipy is a very weak ligand because it cannot form a five-membered chelate ring.