Three new metal-organic framework structures containing EuIII and the little explored methanetriacetate (C7H7O63-, mta3-) ligand have been synthesized. Gel synthesis yields a two-dimensional framework with the formula [Eu(mta)(H2O)3]n·2nH2O, (I), while two polymorphs of the three-dimensional framework material [Eu(mta)(H2O)]n·nH2O, (II) and (III), are obtained through hydrothermal synthesis at either 423 or 443 K. Compounds (I) and (II) are isomorphous with previously reported GdIII compounds, but compound (III) constitutes a new phase. Compound (I) can be described in terms of dinuclear [Eu2(H2O)4]6+ units bonded through mta3- ligands to form a two-dimensional framework with topology corresponding to a (6,3)-connected binodal (43)(466683)-kgd net, where the dinuclear [Eu2(H2O)4]6+ units are considered as a single node. Compounds (II) and (III) have distinct three-dimensional topologies, namely a (41263)(4966)-nia net for (II) and a (41065)(41164)-K2O2; 36641 net for (III). The crystal density of (III) is greater than that of (II), consistent with the increase of temperature, and thereby autogeneous pressure, in the hydrothermal synthesis.
Supporting information
CCDC references: 978533; 978534; 978535
Data collection: COLLECT (Nonius, 1998) for (I), (III); Collect (Nonius, 1998) for (II). Cell refinement: EVALCCD for (I); HKL-2000 for (II), (III). Data reduction: EVALCCD (Duisenberg et al., 2003) for (I); HKL-2000 (Otwinowski & Minor, 1997) for (II), (III). For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008). Molecular graphics: DIAMOND (Brandenburg, 1999) for (I), (III); ORTEP-3 for Windows (Farrugia, 1997) for (II). Software used to prepare material for publication: WinGX (Farrugia, 1999), PARST95 (Nardelli, 1995) and PLATON (Spek, 2009) for (I), (III); WinGX (Farrugia, 1999) for (II).
Crystal data top
C7H13EuO9·2(H2O) | Z = 2 |
Mr = 429.17 | F(000) = 420 |
Triclinic, P1 | Dx = 2.216 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.0917 (13) Å | Cell parameters from 2943 reflections |
b = 8.8680 (12) Å | θ = 4.0–27.5° |
c = 10.115 (2) Å | µ = 4.93 mm−1 |
α = 86.994 (17)° | T = 293 K |
β = 73.002 (16)° | Needle, colourless |
γ = 68.172 (15)° | 0.80 × 0.40 × 0.20 mm |
V = 643.06 (19) Å3 | |
Data collection top
Nonius KappaCCD diffractometer | 2943 independent reflections |
Radiation source: fine-focus sealed tube | 2743 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
Detector resolution: 9 pixels mm-1 | θmax = 27.5°, θmin = 4.0° |
thick–slice ω– and φ–scans | h = −10→10 |
Absorption correction: for a sphere Dwiggins (1975) | k = −11→11 |
Tmin = 0.110, Tmax = 0.439 | l = −13→13 |
10427 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.024 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.059 | H-atom parameters constrained |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0304P)2 + 0.1604P] where P = (Fo2 + 2Fc2)/3 |
2943 reflections | (Δ/σ)max < 0.001 |
172 parameters | Δρmax = 1.28 e Å−3 |
0 restraints | Δρmin = −0.56 e Å−3 |
Crystal data top
C7H13EuO9·2(H2O) | γ = 68.172 (15)° |
Mr = 429.17 | V = 643.06 (19) Å3 |
Triclinic, P1 | Z = 2 |
a = 8.0917 (13) Å | Mo Kα radiation |
b = 8.8680 (12) Å | µ = 4.93 mm−1 |
c = 10.115 (2) Å | T = 293 K |
α = 86.994 (17)° | 0.80 × 0.40 × 0.20 mm |
β = 73.002 (16)° | |
Data collection top
Nonius KappaCCD diffractometer | 2943 independent reflections |
Absorption correction: for a sphere Dwiggins (1975) | 2743 reflections with I > 2σ(I) |
Tmin = 0.110, Tmax = 0.439 | Rint = 0.042 |
10427 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.024 | 0 restraints |
wR(F2) = 0.059 | H-atom parameters constrained |
S = 1.10 | Δρmax = 1.28 e Å−3 |
2943 reflections | Δρmin = −0.56 e Å−3 |
172 parameters | |
Special details top
Experimental. Interpolation using International Tables Vol. C (1992) p. 523, Table 6.3.3.3 for
values of muR in the range 0–2.5, and International Tables Vol. II (1959) p.
302, Table 5.3.6B for muR in the range 2.6–10.0. The interpolation procedure
of C. W. Dwiggins Jr [Acta Cryst. (1975) A31, 146–148] is used with some
modification. |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Eu1 | −0.064805 (19) | 0.706924 (17) | −0.100355 (16) | 0.02372 (7) | |
O1 | 0.0672 (3) | 0.5617 (3) | 0.0934 (2) | 0.0308 (5) | |
O1W | −0.2527 (3) | 0.9760 (3) | 0.0417 (3) | 0.0340 (5) | |
H1W | −0.2045 | 1.0478 | 0.0218 | 0.051* | |
H2W | −0.2884 | 0.9796 | 0.1310 | 0.051* | |
O2 | 0.1297 (3) | 0.7759 (3) | 0.0245 (3) | 0.0329 (5) | |
O2W | −0.3580 (3) | 0.8204 (4) | −0.1609 (3) | 0.0454 (7) | |
H3W | −0.4485 | 0.8885 | −0.1004 | 0.068* | |
H4W | −0.4055 | 0.8026 | −0.2201 | 0.068* | |
O3 | −0.0179 (3) | 1.0930 (3) | 0.2256 (3) | 0.0357 (5) | |
O3W | −0.0128 (4) | 0.6244 (3) | −0.3411 (3) | 0.0388 (6) | |
H5W | −0.0830 | 0.6593 | −0.3932 | 0.058* | |
H6W | 0.0674 | 0.5331 | −0.3795 | 0.058* | |
O4 | −0.1733 (3) | 0.9380 (3) | 0.3183 (3) | 0.0403 (6) | |
O5 | 0.6901 (3) | 0.7005 (3) | 0.1023 (3) | 0.0409 (6) | |
O6 | 0.7402 (3) | 0.4677 (3) | 0.2081 (2) | 0.0299 (5) | |
C1 | 0.1506 (4) | 0.6562 (4) | 0.0977 (3) | 0.0266 (6) | |
C2 | 0.2733 (5) | 0.6205 (4) | 0.1897 (4) | 0.0335 (8) | |
H2A | 0.3949 | 0.5429 | 0.1394 | 0.040* | |
H2B | 0.2228 | 0.5674 | 0.2687 | 0.040* | |
C3 | 0.3011 (4) | 0.7636 (4) | 0.2442 (3) | 0.0272 (6) | |
H3 | 0.3344 | 0.8273 | 0.1659 | 0.033* | |
C4 | −0.0324 (4) | 0.9747 (4) | 0.2945 (3) | 0.0275 (6) | |
C5 | 0.1274 (5) | 0.8759 (4) | 0.3513 (4) | 0.0346 (8) | |
H5A | 0.0840 | 0.8106 | 0.4228 | 0.042* | |
H5B | 0.1614 | 0.9504 | 0.3946 | 0.042* | |
C6 | 0.6463 (4) | 0.6155 (4) | 0.1980 (4) | 0.0272 (6) | |
C7 | 0.4628 (4) | 0.6990 (4) | 0.3075 (4) | 0.0295 (7) | |
H7A | 0.4692 | 0.7886 | 0.3542 | 0.035* | |
H7B | 0.4405 | 0.6225 | 0.3760 | 0.035* | |
O4W | 0.5470 (3) | 0.2555 (3) | 0.3264 (3) | 0.0406 (6) | |
H7W | 0.6102 | 0.3154 | 0.3002 | 0.061* | |
H8W | 0.6271 | 0.1597 | 0.3228 | 0.061* | |
O5W | −0.2117 (3) | 0.6850 (3) | 0.4707 (3) | 0.0385 (6) | |
H9W | −0.2100 | 0.7716 | 0.4312 | 0.058* | |
H10W | −0.3230 | 0.7093 | 0.5224 | 0.058* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Eu1 | 0.02339 (9) | 0.02241 (10) | 0.02717 (10) | −0.00904 (7) | −0.00950 (7) | 0.00192 (6) |
O1 | 0.0371 (12) | 0.0301 (12) | 0.0345 (13) | −0.0176 (10) | −0.0179 (11) | 0.0041 (10) |
O1W | 0.0353 (12) | 0.0310 (12) | 0.0365 (14) | −0.0160 (10) | −0.0064 (11) | −0.0005 (10) |
O2 | 0.0437 (13) | 0.0294 (12) | 0.0361 (14) | −0.0191 (10) | −0.0207 (12) | 0.0064 (10) |
O2W | 0.0305 (13) | 0.0550 (17) | 0.0465 (16) | −0.0042 (12) | −0.0181 (12) | −0.0120 (13) |
O3 | 0.0378 (13) | 0.0296 (12) | 0.0404 (15) | −0.0145 (10) | −0.0109 (11) | 0.0078 (11) |
O3W | 0.0429 (14) | 0.0368 (14) | 0.0331 (14) | −0.0050 (11) | −0.0187 (12) | −0.0006 (11) |
O4 | 0.0329 (13) | 0.0430 (14) | 0.0492 (16) | −0.0188 (11) | −0.0141 (12) | 0.0141 (12) |
O5 | 0.0323 (13) | 0.0335 (13) | 0.0466 (16) | −0.0087 (11) | −0.0023 (12) | 0.0090 (12) |
O6 | 0.0256 (11) | 0.0276 (12) | 0.0331 (13) | −0.0070 (9) | −0.0069 (10) | −0.0007 (10) |
C1 | 0.0254 (14) | 0.0232 (15) | 0.0315 (17) | −0.0091 (12) | −0.0077 (13) | −0.0032 (13) |
C2 | 0.0359 (18) | 0.0262 (16) | 0.046 (2) | −0.0119 (14) | −0.0233 (16) | 0.0044 (15) |
C3 | 0.0285 (15) | 0.0283 (16) | 0.0261 (16) | −0.0110 (13) | −0.0091 (13) | 0.0003 (13) |
C4 | 0.0280 (15) | 0.0232 (15) | 0.0267 (16) | −0.0052 (12) | −0.0066 (13) | −0.0005 (12) |
C5 | 0.0315 (17) | 0.0333 (18) | 0.0351 (19) | −0.0048 (14) | −0.0134 (15) | 0.0002 (14) |
C6 | 0.0239 (14) | 0.0281 (16) | 0.0327 (17) | −0.0104 (12) | −0.0114 (13) | −0.0015 (13) |
C7 | 0.0247 (15) | 0.0356 (18) | 0.0276 (16) | −0.0082 (13) | −0.0101 (13) | −0.0035 (13) |
O4W | 0.0296 (12) | 0.0400 (14) | 0.0491 (16) | −0.0116 (11) | −0.0091 (12) | 0.0038 (12) |
O5W | 0.0365 (13) | 0.0382 (14) | 0.0398 (14) | −0.0126 (11) | −0.0126 (11) | 0.0069 (11) |
Geometric parameters (Å, º) top
Eu1—O3i | 2.314 (2) | O5—C6 | 1.245 (4) |
Eu1—O1ii | 2.386 (2) | O5—Eu1v | 2.415 (2) |
Eu1—O5iii | 2.415 (2) | O6—C6 | 1.264 (4) |
Eu1—O6iv | 2.442 (2) | O6—Eu1iv | 2.442 (2) |
Eu1—O3W | 2.450 (3) | C1—C2 | 1.492 (5) |
Eu1—O2W | 2.455 (3) | C2—C3 | 1.524 (5) |
Eu1—O2 | 2.530 (2) | C2—H2A | 0.9700 |
Eu1—O1W | 2.541 (2) | C2—H2B | 0.9700 |
Eu1—O1 | 2.565 (2) | C3—C5 | 1.524 (5) |
Eu1—Eu1ii | 4.0363 (8) | C3—C7 | 1.531 (4) |
O1—C1 | 1.266 (4) | C3—H3 | 0.9800 |
O1—Eu1ii | 2.386 (2) | C4—C5 | 1.520 (5) |
O1W—H1W | 0.85 | C5—H5A | 0.9700 |
O1W—H2W | 0.86 | C5—H5B | 0.9700 |
O2—C1 | 1.249 (4) | C6—C7 | 1.512 (5) |
O2W—H3W | 0.85 | C7—H7A | 0.9700 |
O2W—H4W | 0.85 | C7—H7B | 0.9700 |
O3—C4 | 1.251 (4) | O4W—H7W | 0.85 |
O3—Eu1i | 2.314 (2) | O4W—H8W | 0.85 |
O3W—H5W | 0.85 | O5W—H9W | 0.85 |
O3W—H6W | 0.85 | O5W—H10W | 0.85 |
O4—C4 | 1.253 (4) | | |
| | | |
O3i—Eu1—O1ii | 149.31 (9) | Eu1—O1W—H2W | 121.1 |
O3i—Eu1—O5iii | 135.97 (9) | H1W—O1W—H2W | 104.9 |
O1ii—Eu1—O5iii | 72.17 (9) | C1—O2—Eu1 | 95.95 (19) |
O3i—Eu1—O6iv | 84.38 (8) | Eu1—O2W—H3W | 115.0 |
O1ii—Eu1—O6iv | 75.71 (8) | Eu1—O2W—H4W | 139.0 |
O5iii—Eu1—O6iv | 135.75 (8) | H3W—O2W—H4W | 105.1 |
O3i—Eu1—O3W | 76.20 (9) | C4—O3—Eu1i | 169.4 (2) |
O1ii—Eu1—O3W | 74.92 (9) | Eu1—O3W—H5W | 130.1 |
O5iii—Eu1—O3W | 128.23 (10) | Eu1—O3W—H6W | 122.4 |
O6iv—Eu1—O3W | 68.73 (8) | H5W—O3W—H6W | 105.1 |
O3i—Eu1—O2W | 87.04 (10) | C6—O5—Eu1v | 144.1 (2) |
O1ii—Eu1—O2W | 92.60 (9) | C6—O6—Eu1iv | 132.9 (2) |
O5iii—Eu1—O2W | 72.90 (9) | O2—C1—O1 | 119.5 (3) |
O6iv—Eu1—O2W | 138.60 (9) | O2—C1—C2 | 121.7 (3) |
O3W—Eu1—O2W | 69.89 (9) | O1—C1—C2 | 118.8 (3) |
O3i—Eu1—O2 | 75.45 (8) | O2—C1—Eu1 | 59.01 (17) |
O1ii—Eu1—O2 | 118.99 (8) | O1—C1—Eu1 | 60.64 (17) |
O5iii—Eu1—O2 | 97.31 (9) | C2—C1—Eu1 | 175.3 (2) |
O6iv—Eu1—O2 | 72.76 (8) | C1—C2—C3 | 117.5 (3) |
O3W—Eu1—O2 | 133.73 (9) | C1—C2—H2A | 107.9 |
O2W—Eu1—O2 | 142.86 (9) | C3—C2—H2A | 107.9 |
O3i—Eu1—O1W | 72.10 (9) | C1—C2—H2B | 107.9 |
O1ii—Eu1—O1W | 137.01 (8) | C3—C2—H2B | 107.9 |
O5iii—Eu1—O1W | 64.87 (8) | H2A—C2—H2B | 107.2 |
O6iv—Eu1—O1W | 139.45 (8) | C5—C3—C2 | 113.1 (3) |
O3W—Eu1—O1W | 132.42 (8) | C5—C3—C7 | 109.5 (3) |
O2W—Eu1—O1W | 73.89 (9) | C2—C3—C7 | 109.2 (3) |
O2—Eu1—O1W | 69.65 (8) | C5—C3—H3 | 108.3 |
O3i—Eu1—O1 | 125.13 (8) | C2—C3—H3 | 108.3 |
O1ii—Eu1—O1 | 70.82 (9) | C7—C3—H3 | 108.3 |
O5iii—Eu1—O1 | 68.59 (8) | O3—C4—O4 | 122.2 (3) |
O6iv—Eu1—O1 | 72.63 (8) | O3—C4—C5 | 117.6 (3) |
O3W—Eu1—O1 | 133.22 (8) | O4—C4—C5 | 120.2 (3) |
O2W—Eu1—O1 | 141.10 (9) | C4—C5—C3 | 115.0 (3) |
O2—Eu1—O1 | 50.48 (7) | C4—C5—H5A | 108.5 |
O1W—Eu1—O1 | 94.23 (8) | C3—C5—H5A | 108.5 |
O3i—Eu1—Eu1ii | 150.93 (6) | C4—C5—H5B | 108.5 |
O1ii—Eu1—Eu1ii | 36.88 (6) | C3—C5—H5B | 108.5 |
O5iii—Eu1—Eu1ii | 65.61 (6) | H5A—C5—H5B | 107.5 |
O6iv—Eu1—Eu1ii | 70.39 (6) | O5—C6—O6 | 125.4 (3) |
O3W—Eu1—Eu1ii | 106.34 (6) | O5—C6—C7 | 115.8 (3) |
O2W—Eu1—Eu1ii | 121.42 (7) | O6—C6—C7 | 118.9 (3) |
O2—Eu1—Eu1ii | 83.23 (5) | C6—C7—C3 | 111.4 (3) |
O1W—Eu1—Eu1ii | 118.64 (6) | C6—C7—H7A | 109.4 |
O1—Eu1—Eu1ii | 33.94 (5) | C3—C7—H7A | 109.4 |
C1—Eu1—Eu1ii | 58.41 (6) | C6—C7—H7B | 109.4 |
C1—O1—Eu1ii | 149.4 (2) | C3—C7—H7B | 109.4 |
C1—O1—Eu1 | 93.87 (19) | H7A—C7—H7B | 108.0 |
Eu1ii—O1—Eu1 | 109.18 (9) | H7W—O4W—H8W | 105.1 |
Eu1—O1W—H1W | 114.6 | H9W—O5W—H10W | 105.1 |
| | | |
O3i—Eu1—O1—C1 | 9.2 (2) | Eu1ii—Eu1—O2—C1 | −7.16 (19) |
O1ii—Eu1—O1—C1 | 159.5 (2) | Eu1—O2—C1—O1 | −4.9 (3) |
O5iii—Eu1—O1—C1 | −122.7 (2) | Eu1—O2—C1—C2 | 174.5 (3) |
O6iv—Eu1—O1—C1 | 79.00 (19) | Eu1ii—O1—C1—O2 | 144.3 (3) |
O3W—Eu1—O1—C1 | 114.3 (2) | Eu1—O1—C1—O2 | 4.8 (3) |
O2W—Eu1—O1—C1 | −131.3 (2) | Eu1ii—O1—C1—C2 | −35.1 (6) |
O2—Eu1—O1—C1 | −2.69 (18) | Eu1—O1—C1—C2 | −174.6 (3) |
O1W—Eu1—O1—C1 | −61.83 (19) | O2—C1—C2—C3 | 27.4 (5) |
Eu1ii—Eu1—O1—C1 | 159.5 (2) | O1—C1—C2—C3 | −153.1 (3) |
O3i—Eu1—O1—Eu1ii | −150.29 (9) | C1—C2—C3—C5 | 70.5 (4) |
O1ii—Eu1—O1—Eu1ii | 0.0 | C1—C2—C3—C7 | −167.2 (3) |
O5iii—Eu1—O1—Eu1ii | 77.77 (10) | Eu1i—O3—C4—O4 | −171.9 (11) |
O6iv—Eu1—O1—Eu1ii | −80.50 (10) | Eu1i—O3—C4—C5 | 8.9 (15) |
O3W—Eu1—O1—Eu1ii | −45.17 (15) | O3—C4—C5—C3 | −74.6 (4) |
O2W—Eu1—O1—Eu1ii | 69.24 (16) | O4—C4—C5—C3 | 106.2 (4) |
O2—Eu1—O1—Eu1ii | −162.19 (15) | C2—C3—C5—C4 | −69.6 (4) |
O1W—Eu1—O1—Eu1ii | 138.67 (9) | C7—C3—C5—C4 | 168.4 (3) |
C1—Eu1—O1—Eu1ii | −159.5 (2) | Eu1v—O5—C6—O6 | −7.8 (6) |
O3i—Eu1—O2—C1 | −167.2 (2) | Eu1v—O5—C6—C7 | 173.6 (3) |
O1ii—Eu1—O2—C1 | −16.5 (2) | Eu1iv—O6—C6—O5 | 18.0 (5) |
O5iii—Eu1—O2—C1 | 57.1 (2) | Eu1iv—O6—C6—C7 | −163.4 (2) |
O6iv—Eu1—O2—C1 | −78.7 (2) | O5—C6—C7—C3 | 58.0 (4) |
O3W—Eu1—O2—C1 | −113.3 (2) | O6—C6—C7—C3 | −120.7 (3) |
O2W—Eu1—O2—C1 | 128.3 (2) | C5—C3—C7—C6 | −168.4 (3) |
O1W—Eu1—O2—C1 | 116.8 (2) | C2—C3—C7—C6 | 67.3 (4) |
O1—Eu1—O2—C1 | 2.74 (18) | | |
Symmetry codes: (i) −x, −y+2, −z; (ii) −x, −y+1, −z; (iii) x−1, y, z; (iv) −x+1, −y+1, −z; (v) x+1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O2i | 0.85 | 1.87 | 2.714 (4) | 172 |
O1W—H2W···O4 | 0.86 | 2.30 | 3.024 (4) | 141 |
O2W—H3W···O1Wvi | 0.85 | 2.17 | 2.901 (4) | 144 |
O2W—H4W···O4Wii | 0.85 | 1.99 | 2.824 (4) | 168 |
O3W—H5W···O5Wvii | 0.85 | 1.91 | 2.747 (4) | 166 |
O3W—H6W···O5Wii | 0.85 | 1.96 | 2.797 (4) | 169 |
O4W—H7W···O6 | 0.85 | 2.04 | 2.877 (4) | 169 |
O4W—H8W···O4viii | 0.85 | 2.02 | 2.869 (4) | 177 |
O5W—H9W···O4 | 0.85 | 1.88 | 2.717 (4) | 170 |
O5W—H10W···O4Wix | 0.85 | 1.93 | 2.765 (4) | 166 |
Symmetry codes: (i) −x, −y+2, −z; (ii) −x, −y+1, −z; (vi) −x−1, −y+2, −z; (vii) x, y, z−1; (viii) x+1, y−1, z; (ix) −x, −y+1, −z+1. |
Crystal data top
C7H9EuO7·H2O | Z = 8 |
Mr = 375.12 | F(000) = 1440 |
Orthorhombic, Pca21 | Dx = 2.441 Mg m−3 |
Hall symbol: P 2c -2ac | Mo Kα radiation, λ = 0.71070 Å |
a = 17.4543 (19) Å | µ = 6.17 mm−1 |
b = 7.8087 (6) Å | T = 293 K |
c = 14.9761 (18) Å | Prism, yellow |
V = 2041.2 (4) Å3 | 0.70 × 0.26 × 0.24 mm |
Data collection top
KappaCCD diffractometer | 3215 independent reflections |
Radiation source: fine-focus sealed tube | 3040 reflections with I > 2σ(I) |
Horizonally mounted graphite crystal monochromator | Rint = 0.076 |
Detector resolution: 9 pixels mm-1 | θmax = 28.3°, θmin = 3.5° |
CCD rotation images, thick slices scans | h = −22→23 |
Absorption correction: for a cylinder mounted on the φ axis Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification. | k = −10→8 |
Tmin = 0.370, Tmax = 0.383 | l = −15→19 |
8250 measured reflections | |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.063 | w = 1/[σ2(Fo2) + (0.0878P)2 + 3.3954P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.167 | (Δ/σ)max < 0.001 |
S = 1.14 | Δρmax = 1.39 e Å−3 |
3215 reflections | Δρmin = −1.82 e Å−3 |
291 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
1 restraint | Extinction coefficient: 0.054 (5) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Refined as an inversion twin. |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.38 (3) |
Crystal data top
C7H9EuO7·H2O | V = 2041.2 (4) Å3 |
Mr = 375.12 | Z = 8 |
Orthorhombic, Pca21 | Mo Kα radiation |
a = 17.4543 (19) Å | µ = 6.17 mm−1 |
b = 7.8087 (6) Å | T = 293 K |
c = 14.9761 (18) Å | 0.70 × 0.26 × 0.24 mm |
Data collection top
KappaCCD diffractometer | 3215 independent reflections |
Absorption correction: for a cylinder mounted on the φ axis Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification. | 3040 reflections with I > 2σ(I) |
Tmin = 0.370, Tmax = 0.383 | Rint = 0.076 |
8250 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.063 | H-atom parameters constrained |
wR(F2) = 0.167 | Δρmax = 1.39 e Å−3 |
S = 1.14 | Δρmin = −1.82 e Å−3 |
3215 reflections | Absolute structure: Refined as an inversion twin. |
291 parameters | Absolute structure parameter: 0.38 (3) |
1 restraint | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Eu1 | 0.15041 (3) | 0.24606 (3) | 0.00438 (4) | 0.0166 (2) | |
Eu2 | 0.09236 (3) | −0.25409 (3) | 0.04429 (4) | 0.0166 (2) | |
O1 | 0.1453 (3) | 0.0136 (9) | 0.1122 (5) | 0.0269 (14) | |
O1W | 0.2535 (4) | 0.4328 (8) | −0.0629 (6) | 0.0399 (19) | |
H1W | 0.2432 | 0.5374 | −0.0528 | 0.060* | |
H2W | 0.2967 | 0.4338 | −0.0893 | 0.060* | |
O2 | 0.1227 (4) | −0.2038 (8) | 0.2015 (5) | 0.0310 (12) | |
O2W | −0.0119 (4) | −0.0698 (9) | 0.1055 (6) | 0.0350 (17) | |
H3W | −0.0013 | 0.0348 | 0.0959 | 0.052* | |
H4W | −0.0532 | −0.0697 | 0.1357 | 0.052* | |
O3 | 0.2621 (4) | 0.0543 (8) | 0.4466 (6) | 0.0360 (17) | |
O4 | 0.2857 (5) | −0.2199 (8) | 0.4674 (9) | 0.0393 (19) | |
O5 | −0.0731 (3) | −0.0067 (9) | 0.4502 (5) | 0.0241 (12) | |
O6 | 0.0020 (3) | 0.2085 (8) | 0.4227 (6) | 0.0325 (13) | |
O7 | 0.2521 (3) | 0.2951 (7) | 0.1172 (5) | 0.0322 (13) | |
O8 | 0.1719 (3) | 0.5069 (7) | 0.1002 (4) | 0.0203 (11) | |
O9 | 0.5026 (3) | 0.4459 (7) | 0.0994 (5) | 0.0267 (14) | |
O10 | 0.5231 (4) | 0.7253 (7) | 0.0736 (8) | 0.0314 (18) | |
O11 | 0.3813 (3) | 0.3078 (8) | 0.3433 (4) | 0.0320 (12) | |
O12 | 0.4024 (3) | 0.5117 (9) | 0.4363 (5) | 0.0235 (13) | |
C1 | 0.1393 (4) | −0.0486 (9) | 0.1911 (5) | 0.0228 (13) | |
C2 | 0.1496 (5) | 0.0668 (11) | 0.2714 (6) | 0.0351 (19) | |
H2A | 0.2036 | 0.0944 | 0.2767 | 0.042* | |
H2B | 0.1225 | 0.1730 | 0.2602 | 0.042* | |
C3 | 0.1230 (3) | −0.0031 (9) | 0.3587 (6) | 0.0215 (14) | |
H3 | 0.1268 | 0.0906 | 0.4020 | 0.026* | |
C4 | 0.1721 (4) | −0.1490 (9) | 0.3947 (6) | 0.0345 (17) | |
H4A | 0.1415 | −0.2142 | 0.4367 | 0.041* | |
H4B | 0.1846 | −0.2246 | 0.3454 | 0.041* | |
C5 | 0.2451 (4) | −0.0989 (8) | 0.4400 (5) | 0.0239 (14) | |
C6 | 0.0376 (3) | −0.0602 (11) | 0.3577 (7) | 0.040 (2) | |
H6A | 0.0194 | −0.0605 | 0.2966 | 0.047* | |
H6B | 0.0342 | −0.1764 | 0.3802 | 0.047* | |
C7 | −0.0134 (3) | 0.0536 (9) | 0.4128 (5) | 0.0216 (13) | |
C8 | 0.2326 (3) | 0.4457 (9) | 0.1349 (5) | 0.0206 (13) | |
C9 | 0.2780 (3) | 0.5496 (9) | 0.2005 (5) | 0.0216 (13) | |
H9A | 0.2624 | 0.5179 | 0.2604 | 0.026* | |
H9B | 0.2655 | 0.6696 | 0.1922 | 0.026* | |
C10 | 0.3652 (3) | 0.5287 (9) | 0.1932 (5) | 0.0164 (12) | |
H10 | 0.3770 | 0.4077 | 0.1824 | 0.020* | |
C11 | 0.3967 (3) | 0.6353 (8) | 0.1152 (5) | 0.0195 (12) | |
H11A | 0.3913 | 0.7558 | 0.1295 | 0.023* | |
H11B | 0.3661 | 0.6125 | 0.0625 | 0.023* | |
C12 | 0.4813 (3) | 0.5982 (8) | 0.0934 (5) | 0.0199 (12) | |
C13 | 0.4041 (3) | 0.5848 (9) | 0.2806 (5) | 0.0203 (13) | |
H13A | 0.4584 | 0.6008 | 0.2694 | 0.024* | |
H13B | 0.3831 | 0.6946 | 0.2985 | 0.024* | |
C14 | 0.3947 (3) | 0.4599 (10) | 0.3571 (6) | 0.0213 (13) | |
O3W | −0.1033 (5) | −0.4584 (12) | −0.1368 (10) | 0.087 (4) | |
H5W | −0.0728 | −0.3810 | −0.1187 | 0.131* | |
H6W | −0.0757 | −0.5271 | −0.1669 | 0.131* | |
O4W | 0.8544 (3) | 0.9340 (8) | 0.2025 (5) | 0.0402 (15) | |
H7W | 0.8239 | 0.8868 | 0.1657 | 0.060* | |
H8W | 0.8662 | 0.8555 | 0.2394 | 0.060* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Eu1 | 0.0108 (3) | 0.0131 (3) | 0.0260 (4) | 0.00012 (8) | 0.00183 (18) | −0.00039 (17) |
Eu2 | 0.0100 (3) | 0.0124 (3) | 0.0273 (4) | 0.00033 (7) | 0.0017 (2) | −0.00025 (17) |
O1 | 0.023 (3) | 0.034 (3) | 0.025 (3) | −0.005 (2) | 0.001 (2) | 0.004 (2) |
O1W | 0.023 (3) | 0.031 (3) | 0.066 (5) | −0.002 (3) | 0.016 (3) | 0.003 (3) |
O2 | 0.045 (4) | 0.017 (2) | 0.030 (3) | −0.002 (3) | −0.004 (3) | −0.006 (2) |
O2W | 0.023 (3) | 0.027 (3) | 0.055 (5) | 0.001 (2) | 0.016 (3) | 0.000 (3) |
O3 | 0.022 (3) | 0.027 (3) | 0.059 (5) | −0.010 (2) | −0.017 (3) | −0.004 (3) |
O4 | 0.035 (4) | 0.030 (3) | 0.053 (5) | 0.008 (3) | −0.017 (3) | 0.011 (4) |
O5 | 0.009 (2) | 0.026 (3) | 0.037 (3) | −0.003 (2) | 0.005 (2) | 0.000 (2) |
O6 | 0.023 (3) | 0.018 (2) | 0.057 (4) | −0.001 (3) | 0.015 (3) | 0.001 (3) |
O7 | 0.024 (2) | 0.018 (2) | 0.054 (4) | 0.002 (3) | −0.018 (2) | −0.002 (3) |
O8 | 0.017 (2) | 0.018 (2) | 0.026 (3) | −0.0002 (19) | −0.006 (2) | −0.005 (2) |
O9 | 0.018 (3) | 0.025 (3) | 0.037 (4) | 0.003 (2) | 0.005 (2) | 0.003 (3) |
O10 | 0.015 (3) | 0.015 (2) | 0.064 (5) | −0.003 (2) | 0.014 (3) | 0.003 (3) |
O11 | 0.047 (3) | 0.018 (3) | 0.031 (3) | 0.001 (2) | 0.000 (2) | −0.002 (2) |
O12 | 0.024 (3) | 0.023 (3) | 0.023 (3) | −0.005 (2) | 0.0017 (19) | 0.003 (2) |
C1 | 0.021 (3) | 0.019 (3) | 0.028 (3) | 0.008 (3) | 0.001 (2) | 0.000 (3) |
C2 | 0.046 (5) | 0.024 (4) | 0.035 (4) | −0.007 (3) | −0.007 (3) | −0.003 (3) |
C3 | 0.007 (3) | 0.013 (3) | 0.045 (4) | 0.003 (2) | 0.000 (3) | −0.002 (3) |
C4 | 0.036 (4) | 0.020 (3) | 0.048 (4) | −0.006 (3) | −0.017 (3) | 0.007 (3) |
C5 | 0.017 (3) | 0.022 (3) | 0.033 (4) | 0.002 (2) | −0.004 (3) | −0.003 (3) |
C6 | 0.010 (3) | 0.047 (5) | 0.061 (5) | 0.001 (3) | 0.013 (3) | −0.028 (4) |
C7 | 0.009 (3) | 0.028 (3) | 0.028 (3) | 0.006 (2) | 0.002 (2) | 0.006 (3) |
C8 | 0.012 (3) | 0.025 (3) | 0.025 (3) | −0.003 (2) | 0.001 (2) | 0.003 (3) |
C9 | 0.009 (2) | 0.022 (3) | 0.034 (4) | 0.000 (2) | 0.001 (2) | −0.002 (3) |
C10 | 0.009 (2) | 0.025 (3) | 0.015 (3) | 0.003 (2) | −0.003 (2) | −0.004 (2) |
C11 | 0.012 (2) | 0.022 (3) | 0.024 (3) | 0.002 (2) | 0.001 (2) | 0.006 (2) |
C12 | 0.018 (3) | 0.023 (3) | 0.019 (3) | 0.000 (2) | 0.003 (2) | 0.001 (2) |
C13 | 0.017 (3) | 0.023 (3) | 0.021 (3) | −0.006 (2) | −0.005 (2) | 0.002 (3) |
C14 | 0.010 (2) | 0.031 (4) | 0.023 (3) | −0.004 (2) | 0.002 (2) | 0.000 (3) |
O3W | 0.047 (5) | 0.064 (7) | 0.151 (10) | −0.021 (4) | 0.033 (6) | −0.020 (6) |
O4W | 0.025 (3) | 0.044 (4) | 0.052 (4) | −0.011 (2) | 0.001 (2) | 0.013 (3) |
Geometric parameters (Å, º) top
Eu1—O3i | 2.307 (6) | O9—C12 | 1.249 (8) |
Eu1—O1 | 2.431 (7) | O9—Eu2x | 2.319 (6) |
Eu1—O5ii | 2.445 (6) | O10—C12 | 1.267 (9) |
Eu1—O10iii | 2.462 (8) | O10—Eu1xi | 2.462 (8) |
Eu1—O7 | 2.480 (6) | O11—C14 | 1.228 (9) |
Eu1—O12i | 2.488 (6) | O11—Eu1viii | 2.521 (7) |
Eu1—O8 | 2.520 (6) | O12—C14 | 1.261 (10) |
Eu1—O11i | 2.521 (7) | O12—Eu2xii | 2.443 (7) |
Eu1—O1W | 2.526 (7) | O12—Eu1viii | 2.488 (6) |
Eu1—C14i | 2.876 (8) | C1—C2 | 1.514 (10) |
Eu1—C8 | 2.883 (7) | C2—C3 | 1.491 (13) |
Eu1—Eu2iv | 4.0767 (5) | C2—H2A | 0.9700 |
Eu2—O9v | 2.319 (6) | C2—H2B | 0.9700 |
Eu2—O4i | 2.435 (9) | C3—C4 | 1.525 (10) |
Eu2—O12vi | 2.443 (7) | C3—C6 | 1.555 (9) |
Eu2—O2 | 2.445 (7) | C3—H3 | 0.9800 |
Eu2—O8vii | 2.472 (6) | C4—C5 | 1.496 (9) |
Eu2—O6ii | 2.480 (7) | C4—H4A | 0.9700 |
Eu2—O2W | 2.495 (7) | C4—H4B | 0.9700 |
Eu2—O5ii | 2.499 (7) | C6—C7 | 1.505 (9) |
Eu2—O1 | 2.502 (7) | C6—H6A | 0.9700 |
Eu2—C1 | 2.842 (8) | C6—H6B | 0.9700 |
Eu2—C7ii | 2.868 (7) | C7—Eu2ix | 2.868 (7) |
Eu2—Eu1vii | 4.0767 (5) | C8—C9 | 1.501 (9) |
O1—C1 | 1.281 (9) | C9—C10 | 1.535 (8) |
O1W—H1W | 0.8500 | C9—H9A | 0.9700 |
O1W—H2W | 0.8501 | C9—H9B | 0.9700 |
O2—C1 | 1.255 (9) | C10—C11 | 1.536 (9) |
O2W—H3W | 0.8500 | C10—C13 | 1.538 (9) |
O2W—H4W | 0.8499 | C10—H10 | 0.9800 |
O3—C5 | 1.236 (8) | C11—C12 | 1.539 (8) |
O3—Eu1viii | 2.307 (6) | C11—H11A | 0.9700 |
O4—C5 | 1.250 (9) | C11—H11B | 0.9700 |
O4—Eu2viii | 2.435 (9) | C13—C14 | 1.513 (10) |
O5—C7 | 1.272 (8) | C13—H13A | 0.9700 |
O5—Eu1ix | 2.445 (6) | C13—H13B | 0.9700 |
O5—Eu2ix | 2.499 (7) | C14—Eu1viii | 2.876 (8) |
O6—C7 | 1.248 (9) | O3W—H5W | 0.8499 |
O6—Eu2ix | 2.480 (7) | O3W—H6W | 0.8499 |
O7—C8 | 1.252 (9) | O4W—H7W | 0.8499 |
O8—C8 | 1.274 (8) | O4W—H8W | 0.8500 |
O8—Eu2iv | 2.472 (6) | | |
| | | |
O3i—Eu1—O1 | 77.8 (2) | O1—Eu2—C7ii | 90.0 (2) |
O3i—Eu1—O5ii | 75.2 (2) | C1—Eu2—C7ii | 111.17 (19) |
O1—Eu1—O5ii | 68.3 (2) | O9v—Eu2—Eu1vii | 66.54 (14) |
O3i—Eu1—O10iii | 144.5 (2) | O4i—Eu2—Eu1vii | 79.53 (16) |
O1—Eu1—O10iii | 75.8 (2) | O12vi—Eu2—Eu1vii | 34.59 (15) |
O5ii—Eu1—O10iii | 73.2 (2) | O2—Eu2—Eu1vii | 103.95 (15) |
O3i—Eu1—O7 | 83.2 (3) | O8vii—Eu2—Eu1vii | 35.64 (13) |
O1—Eu1—O7 | 71.9 (2) | O6ii—Eu2—Eu1vii | 101.24 (15) |
O5ii—Eu1—O7 | 137.7 (2) | O2W—Eu2—Eu1vii | 141.95 (15) |
O10iii—Eu1—O7 | 110.2 (3) | O5ii—Eu2—Eu1vii | 136.96 (16) |
O3i—Eu1—O12i | 129.3 (3) | O1—Eu2—Eu1vii | 140.16 (14) |
O1—Eu1—O12i | 151.7 (2) | C1—Eu2—Eu1vii | 125.62 (14) |
O5ii—Eu1—O12i | 107.3 (2) | C7ii—Eu2—Eu1vii | 122.78 (14) |
O10iii—Eu1—O12i | 76.3 (2) | C1—O1—Eu1 | 154.0 (5) |
O7—Eu1—O12i | 114.5 (2) | C1—O1—Eu2 | 91.6 (5) |
O3i—Eu1—O8 | 129.8 (2) | Eu1—O1—Eu2 | 111.5 (3) |
O1—Eu1—O8 | 103.3 (3) | Eu1—O1W—H1W | 109.4 |
O5ii—Eu1—O8 | 152.8 (2) | Eu1—O1W—H2W | 145.2 |
O10iii—Eu1—O8 | 79.7 (2) | H1W—O1W—H2W | 105.1 |
O7—Eu1—O8 | 51.74 (19) | C1—O2—Eu2 | 94.9 (5) |
O12i—Eu1—O8 | 67.3 (2) | Eu2—O2W—H3W | 109.4 |
O3i—Eu1—O11i | 84.9 (3) | Eu2—O2W—H4W | 144.5 |
O1—Eu1—O11i | 140.4 (2) | H3W—O2W—H4W | 105.9 |
O5ii—Eu1—O11i | 73.0 (2) | C5—O3—Eu1viii | 144.8 (6) |
O10iii—Eu1—O11i | 100.8 (3) | C5—O4—Eu2viii | 137.1 (6) |
O7—Eu1—O11i | 141.2 (2) | C7—O5—Eu1ix | 151.7 (5) |
O12i—Eu1—O11i | 50.8 (2) | C7—O5—Eu2ix | 93.3 (5) |
O8—Eu1—O11i | 115.03 (19) | Eu1ix—O5—Eu2ix | 111.2 (2) |
O3i—Eu1—O1W | 75.7 (3) | C7—O6—Eu2ix | 94.8 (4) |
O1—Eu1—O1W | 136.2 (2) | C8—O7—Eu1 | 95.5 (4) |
O5ii—Eu1—O1W | 134.6 (3) | C8—O8—Eu2iv | 152.7 (5) |
O10iii—Eu1—O1W | 139.3 (2) | C8—O8—Eu1 | 93.0 (4) |
O7—Eu1—O1W | 70.9 (3) | Eu2iv—O8—Eu1 | 109.5 (2) |
O12i—Eu1—O1W | 67.6 (2) | C12—O9—Eu2x | 142.2 (5) |
O8—Eu1—O1W | 69.8 (2) | C12—O10—Eu1xi | 133.6 (5) |
O11i—Eu1—O1W | 70.4 (3) | C14—O11—Eu1viii | 93.8 (5) |
O3i—Eu1—C14i | 105.7 (3) | C14—O12—Eu2xii | 150.1 (5) |
O1—Eu1—C14i | 158.86 (19) | C14—O12—Eu1viii | 94.5 (5) |
O5ii—Eu1—C14i | 92.2 (2) | Eu2xii—O12—Eu1viii | 111.5 (3) |
O10iii—Eu1—C14i | 91.3 (3) | O2—C1—O1 | 120.0 (7) |
O7—Eu1—C14i | 129.0 (2) | O2—C1—C2 | 120.2 (7) |
O12i—Eu1—C14i | 25.9 (2) | O1—C1—C2 | 119.8 (7) |
O8—Eu1—C14i | 90.5 (2) | O2—C1—Eu2 | 59.0 (4) |
O11i—Eu1—C14i | 25.2 (2) | O1—C1—Eu2 | 61.6 (4) |
O1W—Eu1—C14i | 63.5 (2) | C2—C1—Eu2 | 170.1 (5) |
O3i—Eu1—C8 | 106.0 (2) | C3—C2—C1 | 116.2 (7) |
O1—Eu1—C8 | 88.4 (2) | C3—C2—H2A | 108.2 |
O5ii—Eu1—C8 | 156.0 (2) | C1—C2—H2A | 108.2 |
O10iii—Eu1—C8 | 96.6 (3) | C3—C2—H2B | 108.2 |
O7—Eu1—C8 | 25.62 (18) | C1—C2—H2B | 108.2 |
O12i—Eu1—C8 | 90.7 (2) | H2A—C2—H2B | 107.4 |
O8—Eu1—C8 | 26.18 (17) | C2—C3—C4 | 114.1 (6) |
O11i—Eu1—C8 | 130.89 (19) | C2—C3—C6 | 113.3 (7) |
O1W—Eu1—C8 | 66.7 (2) | C4—C3—C6 | 109.1 (6) |
C14i—Eu1—C8 | 110.0 (2) | C2—C3—H3 | 106.6 |
O3i—Eu1—Eu2iv | 147.25 (16) | C4—C3—H3 | 106.6 |
O1—Eu1—Eu2iv | 127.46 (17) | C6—C3—H3 | 106.6 |
O5ii—Eu1—Eu2iv | 130.06 (13) | C5—C4—C3 | 116.4 (6) |
O10iii—Eu1—Eu2iv | 68.10 (13) | C5—C4—H4A | 108.2 |
O7—Eu1—Eu2iv | 85.99 (13) | C3—C4—H4A | 108.2 |
O12i—Eu1—Eu2iv | 33.88 (16) | C5—C4—H4B | 108.2 |
O8—Eu1—Eu2iv | 34.86 (13) | C3—C4—H4B | 108.2 |
O11i—Eu1—Eu2iv | 84.42 (13) | H4A—C4—H4B | 107.4 |
O1W—Eu1—Eu2iv | 71.51 (15) | O3—C5—O4 | 124.7 (8) |
C14i—Eu1—Eu2iv | 59.24 (16) | O3—C5—C4 | 119.6 (7) |
C8—Eu1—Eu2iv | 60.43 (13) | O4—C5—C4 | 115.7 (7) |
O9v—Eu2—O4i | 146.1 (2) | C7—C6—C3 | 113.1 (6) |
O9v—Eu2—O12vi | 77.1 (2) | C7—C6—H6A | 109.0 |
O4i—Eu2—O12vi | 74.7 (3) | C3—C6—H6A | 109.0 |
O9v—Eu2—O2 | 84.7 (2) | C7—C6—H6B | 109.0 |
O4i—Eu2—O2 | 104.4 (3) | C3—C6—H6B | 109.0 |
O12vi—Eu2—O2 | 138.5 (2) | H6A—C6—H6B | 107.8 |
O9v—Eu2—O8vii | 76.8 (2) | O6—C7—O5 | 118.8 (7) |
O4i—Eu2—O8vii | 75.7 (2) | O6—C7—C6 | 120.7 (6) |
O12vi—Eu2—O8vii | 68.78 (19) | O5—C7—C6 | 120.5 (7) |
O2—Eu2—O8vii | 70.9 (2) | O6—C7—Eu2ix | 59.5 (4) |
O9v—Eu2—O6ii | 84.6 (2) | O5—C7—Eu2ix | 60.5 (4) |
O4i—Eu2—O6ii | 102.6 (4) | C6—C7—Eu2ix | 169.5 (5) |
O12vi—Eu2—O6ii | 69.3 (2) | O7—C8—O8 | 119.5 (6) |
O2—Eu2—O6ii | 145.9 (2) | O7—C8—C9 | 120.2 (6) |
O8vii—Eu2—O6ii | 136.9 (2) | O8—C8—C9 | 120.2 (6) |
O9v—Eu2—O2W | 75.4 (2) | O7—C8—Eu1 | 58.9 (4) |
O4i—Eu2—O2W | 138.5 (2) | O8—C8—Eu1 | 60.8 (4) |
O12vi—Eu2—O2W | 134.6 (2) | C9—C8—Eu1 | 177.8 (4) |
O2—Eu2—O2W | 73.2 (3) | C8—C9—C10 | 114.8 (5) |
O8vii—Eu2—O2W | 136.1 (2) | C8—C9—H9A | 108.6 |
O6ii—Eu2—O2W | 72.7 (3) | C10—C9—H9A | 108.6 |
O9v—Eu2—O5ii | 129.5 (2) | C8—C9—H9B | 108.6 |
O4i—Eu2—O5ii | 76.2 (2) | C10—C9—H9B | 108.6 |
O12vi—Eu2—O5ii | 104.0 (3) | H9A—C9—H9B | 107.5 |
O2—Eu2—O5ii | 116.2 (2) | C9—C10—C11 | 110.6 (5) |
O8vii—Eu2—O5ii | 151.9 (2) | C9—C10—C13 | 110.3 (5) |
O6ii—Eu2—O5ii | 51.65 (19) | C11—C10—C13 | 109.6 (5) |
O2W—Eu2—O5ii | 68.8 (2) | C9—C10—H10 | 108.8 |
O9v—Eu2—O1 | 130.1 (2) | C11—C10—H10 | 108.8 |
O4i—Eu2—O1 | 77.2 (3) | C13—C10—H10 | 108.8 |
O12vi—Eu2—O1 | 151.8 (2) | C10—C11—C12 | 113.7 (5) |
O2—Eu2—O1 | 52.7 (2) | C10—C11—H11A | 108.8 |
O8vii—Eu2—O1 | 106.6 (2) | C12—C11—H11A | 108.8 |
O6ii—Eu2—O1 | 115.1 (2) | C10—C11—H11B | 108.8 |
O2W—Eu2—O1 | 68.8 (2) | C12—C11—H11B | 108.8 |
O5ii—Eu2—O1 | 66.3 (2) | H11A—C11—H11B | 107.7 |
O9v—Eu2—C1 | 106.5 (3) | O9—C12—O10 | 126.2 (7) |
O4i—Eu2—C1 | 93.0 (3) | O9—C12—C11 | 116.7 (6) |
O12vi—Eu2—C1 | 157.49 (19) | O10—C12—C11 | 117.0 (6) |
O2—Eu2—C1 | 26.1 (2) | C14—C13—C10 | 114.4 (5) |
O8vii—Eu2—C1 | 90.1 (2) | C14—C13—H13A | 108.7 |
O6ii—Eu2—C1 | 132.7 (2) | C10—C13—H13A | 108.7 |
O2W—Eu2—C1 | 66.4 (2) | C14—C13—H13B | 108.7 |
O5ii—Eu2—C1 | 90.9 (2) | C10—C13—H13B | 108.7 |
O1—Eu2—C1 | 26.8 (2) | H13A—C13—H13B | 107.6 |
O9v—Eu2—C7ii | 105.8 (2) | O11—C14—O12 | 119.2 (7) |
O4i—Eu2—C7ii | 92.0 (3) | O11—C14—C13 | 121.1 (7) |
O12vi—Eu2—C7ii | 88.4 (2) | O12—C14—C13 | 119.6 (7) |
O2—Eu2—C7ii | 132.6 (2) | O11—C14—Eu1viii | 61.0 (4) |
O8vii—Eu2—C7ii | 156.1 (2) | O12—C14—Eu1viii | 59.6 (4) |
O6ii—Eu2—C7ii | 25.7 (2) | C13—C14—Eu1viii | 169.8 (4) |
O2W—Eu2—C7ii | 65.6 (2) | H5W—O3W—H6W | 105.2 |
O5ii—Eu2—C7ii | 26.29 (18) | H7W—O4W—H8W | 105.1 |
| | | |
O3i—Eu1—O1—C1 | 143.1 (12) | O6ii—Eu2—C1—O1 | −56.8 (5) |
O5ii—Eu1—O1—C1 | −138.1 (12) | O2W—Eu2—C1—O1 | −89.3 (4) |
O10iii—Eu1—O1—C1 | −60.9 (11) | O5ii—Eu2—C1—O1 | −22.9 (4) |
O7—Eu1—O1—C1 | 56.3 (11) | C7ii—Eu2—C1—O1 | −40.0 (5) |
O12i—Eu1—O1—C1 | −52.0 (13) | Eu1vii—Eu2—C1—O1 | 132.6 (4) |
O8—Eu1—O1—C1 | 14.7 (11) | O9v—Eu2—C1—C2 | −54 (3) |
O11i—Eu1—O1—C1 | −150.7 (11) | O4i—Eu2—C1—C2 | 154 (3) |
O1W—Eu1—O1—C1 | 89.3 (12) | O12vi—Eu2—C1—C2 | −150 (3) |
C14i—Eu1—O1—C1 | −114.8 (12) | O2—Eu2—C1—C2 | −88 (3) |
C8—Eu1—O1—C1 | 36.3 (11) | O8vii—Eu2—C1—C2 | −130 (3) |
Eu2iv—Eu1—O1—C1 | −13.6 (12) | O6ii—Eu2—C1—C2 | 44 (3) |
O3i—Eu1—O1—Eu2 | −65.8 (3) | O2W—Eu2—C1—C2 | 12 (3) |
O5ii—Eu1—O1—Eu2 | 13.0 (2) | O5ii—Eu2—C1—C2 | 78 (3) |
O10iii—Eu1—O1—Eu2 | 90.3 (3) | O1—Eu2—C1—C2 | 101 (3) |
O7—Eu1—O1—Eu2 | −152.6 (3) | C7ii—Eu2—C1—C2 | 61 (3) |
O12i—Eu1—O1—Eu2 | 99.1 (5) | Eu1vii—Eu2—C1—C2 | −126 (3) |
O8—Eu1—O1—Eu2 | 165.8 (2) | O2—C1—C2—C3 | −12.7 (11) |
O11i—Eu1—O1—Eu2 | 0.4 (4) | O1—C1—C2—C3 | 165.3 (7) |
O1W—Eu1—O1—Eu2 | −119.6 (3) | Eu2—C1—C2—C3 | 70 (3) |
C14i—Eu1—O1—Eu2 | 36.3 (7) | C1—C2—C3—C4 | 70.2 (9) |
C8—Eu1—O1—Eu2 | −172.5 (2) | C1—C2—C3—C6 | −55.5 (9) |
Eu2iv—Eu1—O1—Eu2 | 137.53 (16) | C2—C3—C4—C5 | 79.8 (9) |
O9v—Eu2—O1—C1 | 32.3 (5) | C6—C3—C4—C5 | −152.4 (7) |
O4i—Eu2—O1—C1 | −124.7 (5) | Eu1viii—O3—C5—O4 | −5.3 (19) |
O12vi—Eu2—O1—C1 | −130.1 (5) | Eu1viii—O3—C5—C4 | 176.0 (9) |
O2—Eu2—O1—C1 | −5.1 (4) | Eu2viii—O4—C5—O3 | 1.0 (19) |
O8vii—Eu2—O1—C1 | −54.2 (4) | Eu2viii—O4—C5—C4 | 179.8 (9) |
O6ii—Eu2—O1—C1 | 137.2 (4) | C3—C4—C5—O3 | 0.3 (12) |
O2W—Eu2—O1—C1 | 79.5 (4) | C3—C4—C5—O4 | −178.5 (9) |
O5ii—Eu2—O1—C1 | 154.9 (5) | C2—C3—C6—C7 | −110.4 (8) |
C7ii—Eu2—O1—C1 | 143.2 (4) | C4—C3—C6—C7 | 121.3 (8) |
Eu1vii—Eu2—O1—C1 | −69.0 (5) | Eu2ix—O6—C7—O5 | 12.2 (7) |
O9v—Eu2—O1—Eu1 | −135.4 (3) | Eu2ix—O6—C7—C6 | −167.8 (6) |
O4i—Eu2—O1—Eu1 | 67.5 (3) | Eu1ix—O5—C7—O6 | −162.6 (8) |
O12vi—Eu2—O1—Eu1 | 62.2 (5) | Eu2ix—O5—C7—O6 | −12.0 (7) |
O2—Eu2—O1—Eu1 | −172.9 (3) | Eu1ix—O5—C7—C6 | 17.4 (15) |
O8vii—Eu2—O1—Eu1 | 138.1 (2) | Eu2ix—O5—C7—C6 | 167.9 (6) |
O6ii—Eu2—O1—Eu1 | −30.5 (3) | Eu1ix—O5—C7—Eu2ix | −150.5 (11) |
O2W—Eu2—O1—Eu1 | −88.2 (3) | C3—C6—C7—O6 | 29.9 (11) |
O5ii—Eu2—O1—Eu1 | −12.9 (2) | C3—C6—C7—O5 | −150.0 (7) |
C1—Eu2—O1—Eu1 | −167.7 (6) | C3—C6—C7—Eu2ix | −58 (3) |
C7ii—Eu2—O1—Eu1 | −24.6 (3) | Eu1—O7—C8—O8 | 5.8 (7) |
Eu1vii—Eu2—O1—Eu1 | 123.20 (19) | Eu1—O7—C8—C9 | −177.6 (5) |
O9v—Eu2—O2—C1 | −146.9 (5) | Eu2iv—O8—C8—O7 | −151.9 (8) |
O4i—Eu2—O2—C1 | 66.4 (5) | Eu1—O8—C8—O7 | −5.7 (7) |
O12vi—Eu2—O2—C1 | 149.4 (4) | Eu2iv—O8—C8—C9 | 31.5 (14) |
O8vii—Eu2—O2—C1 | 135.3 (5) | Eu1—O8—C8—C9 | 177.7 (5) |
O6ii—Eu2—O2—C1 | −74.7 (6) | Eu2iv—O8—C8—Eu1 | −146.2 (11) |
O2W—Eu2—O2—C1 | −70.5 (5) | O3i—Eu1—C8—O7 | −28.1 (5) |
O5ii—Eu2—O2—C1 | −15.1 (5) | O1—Eu1—C8—O7 | 48.7 (5) |
O1—Eu2—O2—C1 | 5.3 (4) | O5ii—Eu1—C8—O7 | 61.4 (7) |
C7ii—Eu2—O2—C1 | −40.2 (6) | O10iii—Eu1—C8—O7 | 124.2 (5) |
Eu1vii—Eu2—O2—C1 | 148.9 (4) | O12i—Eu1—C8—O7 | −159.5 (5) |
O3i—Eu1—O7—C8 | 152.9 (5) | O8—Eu1—C8—O7 | 174.2 (7) |
O1—Eu1—O7—C8 | −127.8 (5) | O11i—Eu1—C8—O7 | −125.3 (5) |
O5ii—Eu1—O7—C8 | −148.0 (4) | O1W—Eu1—C8—O7 | −94.3 (5) |
O10iii—Eu1—O7—C8 | −61.0 (5) | C14i—Eu1—C8—O7 | −141.9 (5) |
O12i—Eu1—O7—C8 | 22.6 (5) | Eu2iv—Eu1—C8—O7 | −175.6 (5) |
O8—Eu1—O7—C8 | −3.3 (4) | O3i—Eu1—C8—O8 | 157.7 (4) |
O11i—Eu1—O7—C8 | 79.8 (6) | O1—Eu1—C8—O8 | −125.5 (4) |
O1W—Eu1—O7—C8 | 75.7 (5) | O5ii—Eu1—C8—O8 | −112.8 (6) |
C14i—Eu1—O7—C8 | 48.1 (6) | O10iii—Eu1—C8—O8 | −50.0 (4) |
Eu2iv—Eu1—O7—C8 | 3.9 (4) | O7—Eu1—C8—O8 | −174.2 (7) |
O3i—Eu1—O8—C8 | −28.3 (6) | O12i—Eu1—C8—O8 | 26.3 (4) |
O1—Eu1—O8—C8 | 56.8 (4) | O11i—Eu1—C8—O8 | 60.5 (5) |
O5ii—Eu1—O8—C8 | 124.9 (5) | O1W—Eu1—C8—O8 | 91.5 (4) |
O10iii—Eu1—O8—C8 | 129.4 (5) | C14i—Eu1—C8—O8 | 43.9 (4) |
O7—Eu1—O8—C8 | 3.2 (4) | Eu2iv—Eu1—C8—O8 | 10.2 (4) |
O12i—Eu1—O8—C8 | −151.3 (5) | O3i—Eu1—C8—C9 | 39 (12) |
O11i—Eu1—O8—C8 | −133.4 (4) | O1—Eu1—C8—C9 | 116 (12) |
O1W—Eu1—O8—C8 | −77.9 (4) | O5ii—Eu1—C8—C9 | 129 (12) |
C14i—Eu1—O8—C8 | −139.4 (4) | O10iii—Eu1—C8—C9 | −169 (12) |
Eu2iv—Eu1—O8—C8 | −164.3 (5) | O7—Eu1—C8—C9 | 67 (12) |
O3i—Eu1—O8—Eu2iv | 136.0 (3) | O12i—Eu1—C8—C9 | −92 (12) |
O1—Eu1—O8—Eu2iv | −138.9 (2) | O8—Eu1—C8—C9 | −119 (12) |
O5ii—Eu1—O8—Eu2iv | −70.8 (6) | O11i—Eu1—C8—C9 | −58 (12) |
O10iii—Eu1—O8—Eu2iv | −66.3 (3) | O1W—Eu1—C8—C9 | −27 (12) |
O7—Eu1—O8—Eu2iv | 167.5 (3) | C14i—Eu1—C8—C9 | −75 (12) |
O12i—Eu1—O8—Eu2iv | 13.0 (2) | Eu2iv—Eu1—C8—C9 | −108 (12) |
O11i—Eu1—O8—Eu2iv | 30.9 (3) | O7—C8—C9—C10 | 40.6 (9) |
O1W—Eu1—O8—Eu2iv | 86.4 (3) | O8—C8—C9—C10 | −142.9 (6) |
C14i—Eu1—O8—Eu2iv | 24.9 (2) | Eu1—C8—C9—C10 | −25 (12) |
C8—Eu1—O8—Eu2iv | 164.3 (5) | C8—C9—C10—C11 | 78.9 (7) |
Eu2—O2—C1—O1 | −9.5 (7) | C8—C9—C10—C13 | −159.7 (6) |
Eu2—O2—C1—C2 | 168.5 (6) | C9—C10—C11—C12 | −170.3 (5) |
Eu1—O1—C1—O2 | 162.5 (8) | C13—C10—C11—C12 | 67.9 (7) |
Eu2—O1—C1—O2 | 9.2 (7) | Eu2x—O9—C12—O10 | −28.6 (15) |
Eu1—O1—C1—C2 | −15.5 (16) | Eu2x—O9—C12—C11 | 153.5 (6) |
Eu2—O1—C1—C2 | −168.8 (6) | Eu1xi—O10—C12—O9 | 16.7 (17) |
Eu1—O1—C1—Eu2 | 153.3 (12) | Eu1xi—O10—C12—C11 | −165.3 (7) |
O9v—Eu2—C1—O2 | 34.6 (5) | C10—C11—C12—O9 | 38.1 (9) |
O4i—Eu2—C1—O2 | −117.3 (5) | C10—C11—C12—O10 | −140.1 (9) |
O12vi—Eu2—C1—O2 | −61.6 (8) | C9—C10—C13—C14 | 74.0 (7) |
O8vii—Eu2—C1—O2 | −41.6 (5) | C11—C10—C13—C14 | −164.1 (5) |
O6ii—Eu2—C1—O2 | 132.6 (5) | Eu1viii—O11—C14—O12 | 13.0 (6) |
O2W—Eu2—C1—O2 | 100.1 (5) | Eu1viii—O11—C14—C13 | −168.4 (5) |
O5ii—Eu2—C1—O2 | 166.5 (4) | Eu2xii—O12—C14—O11 | −164.4 (6) |
O1—Eu2—C1—O2 | −170.7 (7) | Eu1viii—O12—C14—O11 | −13.2 (6) |
C7ii—Eu2—C1—O2 | 149.4 (4) | Eu2xii—O12—C14—C13 | 17.1 (12) |
Eu1vii—Eu2—C1—O2 | −38.0 (5) | Eu1viii—O12—C14—C13 | 168.2 (5) |
O9v—Eu2—C1—O1 | −154.7 (4) | Eu2xii—O12—C14—Eu1viii | −151.2 (9) |
O4i—Eu2—C1—O1 | 53.4 (5) | C10—C13—C14—O11 | 23.3 (9) |
O12vi—Eu2—C1—O1 | 109.0 (7) | C10—C13—C14—O12 | −158.2 (6) |
O2—Eu2—C1—O1 | 170.7 (7) | C10—C13—C14—Eu1viii | −76 (3) |
O8vii—Eu2—C1—O1 | 129.0 (4) | | |
Symmetry codes: (i) −x+1/2, y, z−1/2; (ii) −x, −y, z−1/2; (iii) x−1/2, −y+1, z; (iv) x, y+1, z; (v) x−1/2, −y, z; (vi) −x+1/2, y−1, z−1/2; (vii) x, y−1, z; (viii) −x+1/2, y, z+1/2; (ix) −x, −y, z+1/2; (x) x+1/2, −y, z; (xi) x+1/2, −y+1, z; (xii) −x+1/2, y+1, z+1/2. |
Crystal data top
C7H9EuO7·H2O | Z = 8 |
Mr = 375.12 | F(000) = 1440 |
Orthorhombic, Pbcn | Dx = 2.520 Mg m−3 |
Hall symbol: -P 2n 2ab | Mo Kα radiation, λ = 0.71073 Å |
a = 14.1085 (3) Å | µ = 6.37 mm−1 |
b = 7.7825 (2) Å | T = 293 K |
c = 18.0083 (4) Å | Prism, yellow |
V = 1977.30 (8) Å3 | 0.32 × 0.30 × 0.24 mm |
Data collection top
Nonius KappaCCD diffractometer | 3133 independent reflections |
Radiation source: fine-focus sealed tube | 2860 reflections with I > 2σ(I) |
Horizonally mounted graphite crystal monochromator | Rint = 0.041 |
Detector resolution: 9 pixels mm-1 | θmax = 31.1°, θmin = 3.7° |
thick–slice ω– and φ–scans | h = −19→20 |
Absorption correction: for a sphere Dwiggins (1975) | k = −11→9 |
Tmin = 0.235, Tmax = 0.310 | l = −25→22 |
15892 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.074 | H-atom parameters constrained |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0279P)2 + 4.6261P] where P = (Fo2 + 2Fc2)/3 |
3133 reflections | (Δ/σ)max < 0.001 |
145 parameters | Δρmax = 0.96 e Å−3 |
0 restraints | Δρmin = −1.16 e Å−3 |
Crystal data top
C7H9EuO7·H2O | V = 1977.30 (8) Å3 |
Mr = 375.12 | Z = 8 |
Orthorhombic, Pbcn | Mo Kα radiation |
a = 14.1085 (3) Å | µ = 6.37 mm−1 |
b = 7.7825 (2) Å | T = 293 K |
c = 18.0083 (4) Å | 0.32 × 0.30 × 0.24 mm |
Data collection top
Nonius KappaCCD diffractometer | 3133 independent reflections |
Absorption correction: for a sphere Dwiggins (1975) | 2860 reflections with I > 2σ(I) |
Tmin = 0.235, Tmax = 0.310 | Rint = 0.041 |
15892 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.029 | 0 restraints |
wR(F2) = 0.074 | H-atom parameters constrained |
S = 1.13 | Δρmax = 0.96 e Å−3 |
3133 reflections | Δρmin = −1.16 e Å−3 |
145 parameters | |
Special details top
Experimental. Interpolation using International Tables Vol. C (1992) p. 523, Table 6.3.3.3 for
values of muR in the range 0–2.5, and International Tables Vol. II (1959) p.
302, Table 5.3.6B for muR in the range 2.6–10.0. The interpolation procedure
of C. W. Dwiggins Jr [Acta Cryst. (1975) A31, 146–148] is used with some
modification. |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Eu1 | 0.705403 (11) | 0.491484 (17) | −0.346199 (8) | 0.02112 (6) | |
O1 | 0.75706 (16) | 0.7403 (3) | −0.26618 (13) | 0.0291 (5) | |
O1W | 0.56042 (18) | 0.3178 (3) | −0.32334 (15) | 0.0386 (6) | |
H1W | 0.5792 | 0.2147 | −0.3285 | 0.058* | |
H2W | 0.5122 | 0.3268 | −0.3514 | 0.058* | |
O2 | 0.6496 (2) | 0.5665 (3) | −0.22157 (14) | 0.0365 (5) | |
O3 | 0.3755 (2) | 0.9645 (4) | −0.15833 (16) | 0.0374 (6) | |
O4 | 0.41657 (17) | 0.6967 (3) | −0.13148 (15) | 0.0337 (5) | |
O5 | 0.72517 (18) | 0.7822 (3) | 0.08010 (13) | 0.0291 (4) | |
O6 | 0.6495 (2) | 0.5735 (3) | 0.02627 (14) | 0.0390 (6) | |
C1 | 0.7023 (2) | 0.6938 (4) | −0.21331 (17) | 0.0261 (6) | |
C2 | 0.7052 (2) | 0.7861 (5) | −0.13973 (17) | 0.0274 (6) | |
H2A | 0.7268 | 0.9030 | −0.1477 | 0.033* | |
H2B | 0.7507 | 0.7295 | −0.1076 | 0.033* | |
C3 | 0.6088 (2) | 0.7904 (4) | −0.10094 (14) | 0.0220 (5) | |
H3 | 0.5832 | 0.6735 | −0.0991 | 0.026* | |
C4 | 0.5394 (2) | 0.9053 (4) | −0.14418 (16) | 0.0251 (5) | |
H4A | 0.5432 | 1.0206 | −0.1240 | 0.030* | |
H4B | 0.5603 | 0.9107 | −0.1954 | 0.030* | |
C5 | 0.4362 (2) | 0.8496 (4) | −0.14335 (16) | 0.0240 (5) | |
C6 | 0.6210 (2) | 0.8568 (4) | −0.02113 (16) | 0.0278 (6) | |
H6A | 0.6580 | 0.9618 | −0.0223 | 0.033* | |
H6B | 0.5591 | 0.8846 | −0.0010 | 0.033* | |
C7 | 0.6688 (2) | 0.7302 (4) | 0.02954 (15) | 0.0242 (5) | |
O2W | 0.4212 (4) | 0.3136 (8) | −0.4347 (4) | 0.130 (2) | |
H3W | 0.3998 | 0.3925 | −0.4627 | 0.196* | |
H4W | 0.4042 | 0.3735 | −0.3975 | 0.196* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Eu1 | 0.02385 (9) | 0.01739 (9) | 0.02210 (9) | 0.00021 (4) | 0.00005 (5) | −0.00193 (4) |
O1 | 0.0318 (12) | 0.0309 (12) | 0.0246 (10) | −0.0005 (10) | 0.0029 (8) | −0.0014 (8) |
O1W | 0.0356 (13) | 0.0336 (13) | 0.0466 (14) | −0.0070 (10) | −0.0023 (11) | −0.0011 (11) |
O2 | 0.0497 (15) | 0.0286 (12) | 0.0311 (11) | −0.0092 (11) | 0.0112 (11) | −0.0072 (9) |
O3 | 0.0274 (12) | 0.0290 (11) | 0.0558 (17) | 0.0031 (10) | −0.0043 (11) | 0.0007 (11) |
O4 | 0.0269 (11) | 0.0254 (11) | 0.0488 (14) | −0.0038 (9) | −0.0037 (10) | 0.0026 (10) |
O5 | 0.0350 (11) | 0.0276 (11) | 0.0248 (10) | −0.0035 (9) | −0.0057 (9) | 0.0020 (9) |
O6 | 0.0625 (17) | 0.0226 (11) | 0.0318 (12) | −0.0045 (11) | −0.0178 (11) | 0.0027 (9) |
C1 | 0.0300 (14) | 0.0243 (14) | 0.0240 (13) | 0.0044 (11) | 0.0008 (11) | −0.0001 (10) |
C2 | 0.0268 (14) | 0.0320 (16) | 0.0233 (13) | 0.0009 (11) | 0.0006 (10) | −0.0033 (11) |
C3 | 0.0246 (13) | 0.0226 (12) | 0.0187 (11) | 0.0014 (11) | −0.0010 (9) | 0.0007 (9) |
C4 | 0.0237 (13) | 0.0263 (13) | 0.0253 (13) | −0.0007 (11) | −0.0028 (10) | 0.0040 (10) |
C5 | 0.0248 (13) | 0.0252 (13) | 0.0220 (12) | 0.0005 (11) | −0.0006 (10) | −0.0020 (10) |
C6 | 0.0373 (16) | 0.0242 (13) | 0.0217 (12) | 0.0056 (12) | −0.0018 (11) | −0.0013 (10) |
C7 | 0.0296 (14) | 0.0228 (13) | 0.0202 (12) | −0.0001 (11) | −0.0003 (10) | 0.0002 (10) |
O2W | 0.081 (3) | 0.111 (4) | 0.199 (6) | 0.002 (3) | −0.030 (4) | 0.089 (4) |
Geometric parameters (Å, º) top
Eu1—O4i | 2.382 (2) | O5—C7 | 1.275 (4) |
Eu1—O3ii | 2.411 (3) | O5—Eu1viii | 2.413 (2) |
Eu1—O5iii | 2.413 (2) | O5—Eu1ix | 2.525 (2) |
Eu1—O2 | 2.449 (2) | O6—C7 | 1.251 (4) |
Eu1—O6iv | 2.480 (2) | O6—Eu1ix | 2.480 (2) |
Eu1—O1v | 2.485 (2) | C1—C2 | 1.508 (4) |
Eu1—O1W | 2.486 (3) | C2—C3 | 1.529 (4) |
Eu1—O1 | 2.521 (2) | C2—H2A | 0.9700 |
Eu1—O5iv | 2.525 (2) | C2—H2B | 0.9700 |
Eu1—Eu1vi | 4.0897 (1) | C3—C6 | 1.537 (4) |
Eu1—H1W | 2.8133 | C3—C4 | 1.537 (4) |
O1—C1 | 1.279 (4) | C3—H3 | 0.9800 |
O1—Eu1vi | 2.485 (2) | C4—C5 | 1.520 (4) |
O1W—H1W | 0.8500 | C4—H4A | 0.9700 |
O1W—H2W | 0.8500 | C4—H4B | 0.9700 |
O2—C1 | 1.248 (4) | C6—C7 | 1.502 (4) |
O3—C5 | 1.267 (4) | C6—H6A | 0.9700 |
O3—Eu1vii | 2.411 (3) | C6—H6B | 0.9700 |
O4—C5 | 1.240 (4) | O2W—H3W | 0.85 |
O4—Eu1i | 2.382 (2) | O2W—H4W | 0.85 |
| | | |
O4i—Eu1—O3ii | 141.58 (9) | C1—O2—Eu1 | 96.13 (19) |
O4i—Eu1—O5iii | 73.21 (9) | C5—O3—Eu1vii | 136.6 (2) |
O3ii—Eu1—O5iii | 71.22 (9) | C5—O4—Eu1i | 140.8 (2) |
O4i—Eu1—O2 | 76.26 (10) | C7—O5—Eu1viii | 151.4 (2) |
O3ii—Eu1—O2 | 108.06 (10) | C7—O5—Eu1ix | 92.21 (18) |
O5iii—Eu1—O2 | 117.43 (8) | Eu1viii—O5—Eu1ix | 111.80 (9) |
O4i—Eu1—O6iv | 75.57 (9) | C7—O6—Eu1ix | 94.95 (18) |
O3ii—Eu1—O6iv | 109.27 (10) | O2—C1—O1 | 119.8 (3) |
O5iii—Eu1—O6iv | 76.62 (9) | O2—C1—C2 | 119.9 (3) |
O2—Eu1—O6iv | 142.65 (10) | O1—C1—C2 | 120.2 (3) |
O4i—Eu1—O1v | 141.18 (8) | C1—C2—C3 | 112.8 (3) |
O3ii—Eu1—O1v | 72.52 (9) | C1—C2—H2A | 109.0 |
O5iii—Eu1—O1v | 143.74 (8) | C3—C2—H2A | 109.0 |
O2—Eu1—O1v | 74.02 (8) | C1—C2—H2B | 109.0 |
O6iv—Eu1—O1v | 116.37 (8) | C3—C2—H2B | 109.0 |
O4i—Eu1—O1W | 78.36 (9) | H2A—C2—H2B | 107.8 |
O3ii—Eu1—O1W | 140.01 (9) | C2—C3—C6 | 109.6 (2) |
O5iii—Eu1—O1W | 145.28 (9) | C2—C3—C4 | 110.4 (2) |
O2—Eu1—O1W | 73.34 (9) | C6—C3—C4 | 110.5 (2) |
O6iv—Eu1—O1W | 77.34 (10) | C2—C3—H3 | 108.8 |
O1v—Eu1—O1W | 69.61 (8) | C6—C3—H3 | 108.8 |
O4i—Eu1—O1 | 77.89 (8) | C4—C3—H3 | 108.8 |
O3ii—Eu1—O1 | 76.11 (8) | C5—C4—C3 | 116.1 (3) |
O5iii—Eu1—O1 | 68.68 (8) | C5—C4—H4A | 108.3 |
O2—Eu1—O1 | 52.14 (8) | C3—C4—H4A | 108.3 |
O6iv—Eu1—O1 | 141.05 (8) | C5—C4—H4B | 108.3 |
O1v—Eu1—O1 | 102.19 (8) | C3—C4—H4B | 108.3 |
O1W—Eu1—O1 | 124.11 (8) | H4A—C4—H4B | 107.4 |
O4i—Eu1—O5iv | 123.83 (8) | O4—C5—O3 | 124.3 (3) |
O3ii—Eu1—O5iv | 80.46 (9) | O4—C5—C4 | 119.3 (3) |
O5iii—Eu1—O5iv | 106.36 (8) | O3—C5—C4 | 116.4 (3) |
O2—Eu1—O5iv | 135.90 (8) | C7—C6—C3 | 113.4 (2) |
O6iv—Eu1—O5iv | 51.42 (8) | C7—C6—H6A | 108.9 |
O1v—Eu1—O5iv | 67.53 (8) | C3—C6—H6A | 108.9 |
O1W—Eu1—O5iv | 73.69 (9) | C7—C6—H6B | 108.9 |
O1—Eu1—O5iv | 156.39 (7) | C3—C6—H6B | 108.9 |
C1—O1—Eu1vi | 141.6 (2) | H6A—C6—H6B | 107.7 |
C1—O1—Eu1 | 91.91 (18) | O6—C7—O5 | 118.6 (3) |
Eu1vi—O1—Eu1 | 109.53 (9) | O6—C7—C6 | 120.9 (3) |
Eu1—O1W—H1W | 103.8 | O5—C7—C6 | 120.4 (3) |
Eu1—O1W—H2W | 121.0 | H3W—O2W—H4W | 88.4 |
H1W—O1W—H2W | 105.2 | | |
| | | |
O4i—Eu1—O1—C1 | 83.30 (18) | Eu1—O2—C1—O1 | 2.6 (3) |
O3ii—Eu1—O1—C1 | −125.24 (19) | Eu1—O2—C1—C2 | −174.0 (2) |
O5iii—Eu1—O1—C1 | 159.80 (19) | Eu1vi—O1—C1—O2 | 123.0 (3) |
O2—Eu1—O1—C1 | 1.40 (17) | Eu1—O1—C1—O2 | −2.5 (3) |
O6iv—Eu1—O1—C1 | 131.2 (2) | Eu1vi—O1—C1—C2 | −60.4 (4) |
O1v—Eu1—O1—C1 | −56.95 (15) | Eu1—O1—C1—C2 | 174.1 (3) |
O1W—Eu1—O1—C1 | 16.5 (2) | O2—C1—C2—C3 | −35.3 (4) |
O5iv—Eu1—O1—C1 | −118.1 (2) | O1—C1—C2—C3 | 148.1 (3) |
C7iv—Eu1—O1—C1 | 160.9 (3) | C1—C2—C3—C6 | 169.9 (3) |
Eu1vi—Eu1—O1—C1 | 147.5 (2) | C1—C2—C3—C4 | −68.2 (3) |
O4i—Eu1—O1—Eu1vi | −64.20 (10) | C2—C3—C4—C5 | 145.9 (3) |
O3ii—Eu1—O1—Eu1vi | 87.26 (10) | C6—C3—C4—C5 | −92.7 (3) |
O5iii—Eu1—O1—Eu1vi | 12.30 (9) | Eu1i—O4—C5—O3 | 20.9 (6) |
O2—Eu1—O1—Eu1vi | −146.10 (14) | Eu1i—O4—C5—C4 | −155.9 (2) |
O6iv—Eu1—O1—Eu1vi | −16.32 (18) | Eu1vii—O3—C5—O4 | 12.6 (5) |
O1v—Eu1—O1—Eu1vi | 155.55 (11) | Eu1vii—O3—C5—C4 | −170.5 (2) |
O1W—Eu1—O1—Eu1vi | −130.96 (10) | C3—C4—C5—O4 | −23.6 (4) |
O5iv—Eu1—O1—Eu1vi | 94.38 (19) | C3—C4—C5—O3 | 159.4 (3) |
C1—Eu1—O1—Eu1vi | −147.5 (2) | C2—C3—C6—C7 | −71.8 (3) |
C7iv—Eu1—O1—Eu1vi | 13.4 (3) | C4—C3—C6—C7 | 166.4 (3) |
O4i—Eu1—O2—C1 | −86.7 (2) | Eu1ix—O6—C7—O5 | 17.1 (3) |
O3ii—Eu1—O2—C1 | 53.6 (2) | Eu1ix—O6—C7—C6 | −158.3 (3) |
O5iii—Eu1—O2—C1 | −24.2 (2) | Eu1viii—O5—C7—O6 | −164.6 (3) |
O6iv—Eu1—O2—C1 | −128.7 (2) | Eu1ix—O5—C7—O6 | −16.8 (3) |
O1v—Eu1—O2—C1 | 118.6 (2) | Eu1viii—O5—C7—C6 | 10.9 (6) |
O1W—Eu1—O2—C1 | −168.4 (2) | Eu1ix—O5—C7—C6 | 158.7 (3) |
O1—Eu1—O2—C1 | −1.44 (18) | C3—C6—C7—O6 | −40.3 (4) |
O5iv—Eu1—O2—C1 | 148.50 (18) | C3—C6—C7—O5 | 144.3 (3) |
C7iv—Eu1—O2—C1 | −171.89 (18) | | |
Symmetry codes: (i) −x+1, y, −z−1/2; (ii) x+1/2, y−1/2, −z−1/2; (iii) −x+3/2, −y+3/2, z−1/2; (iv) x, −y+1, z−1/2; (v) −x+3/2, y−1/2, z; (vi) −x+3/2, y+1/2, z; (vii) x−1/2, y+1/2, −z−1/2; (viii) −x+3/2, −y+3/2, z+1/2; (ix) x, −y+1, z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O3x | 0.85 | 2.06 | 2.913 (4) | 180 |
O1W—H2W···O2W | 0.85 | 1.98 | 2.807 (7) | 165 |
O2W—H3W···O6i | 0.85 | 1.94 | 2.794 (7) | 180 |
Symmetry codes: (i) −x+1, y, −z−1/2; (x) −x+1, y−1, −z−1/2. |
Experimental details
| (I) | (II) | (III) |
Crystal data |
Chemical formula | C7H13EuO9·2(H2O) | C7H9EuO7·H2O | C7H9EuO7·H2O |
Mr | 429.17 | 375.12 | 375.12 |
Crystal system, space group | Triclinic, P1 | Orthorhombic, Pca21 | Orthorhombic, Pbcn |
Temperature (K) | 293 | 293 | 293 |
a, b, c (Å) | 8.0917 (13), 8.8680 (12), 10.115 (2) | 17.4543 (19), 7.8087 (6), 14.9761 (18) | 14.1085 (3), 7.7825 (2), 18.0083 (4) |
α, β, γ (°) | 86.994 (17), 73.002 (16), 68.172 (15) | 90, 90, 90 | 90, 90, 90 |
V (Å3) | 643.06 (19) | 2041.2 (4) | 1977.30 (8) |
Z | 2 | 8 | 8 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 4.93 | 6.17 | 6.37 |
Crystal size (mm) | 0.80 × 0.40 × 0.20 | 0.70 × 0.26 × 0.24 | 0.32 × 0.30 × 0.24 |
|
Data collection |
Diffractometer | Nonius KappaCCD diffractometer | KappaCCD diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | For a sphere Dwiggins (1975) | For a cylinder mounted on the φ axis Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification. | For a sphere Dwiggins (1975) |
Tmin, Tmax | 0.110, 0.439 | 0.370, 0.383 | 0.235, 0.310 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10427, 2943, 2743 | 8250, 3215, 3040 | 15892, 3133, 2860 |
Rint | 0.042 | 0.076 | 0.041 |
(sin θ/λ)max (Å−1) | 0.649 | 0.667 | 0.726 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.059, 1.10 | 0.063, 0.167, 1.14 | 0.029, 0.074, 1.13 |
No. of reflections | 2943 | 3215 | 3133 |
No. of parameters | 172 | 291 | 145 |
No. of restraints | 0 | 1 | 0 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.28, −0.56 | 1.39, −1.82 | 0.96, −1.16 |
Absolute structure | ? | Refined as an inversion twin. | ? |
Absolute structure parameter | ? | 0.38 (3) | ? |
Hydrogen-bond geometry (Å, º) for (I) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O2i | 0.85 | 1.87 | 2.714 (4) | 172 |
O1W—H2W···O4 | 0.86 | 2.30 | 3.024 (4) | 141 |
O2W—H3W···O1Wii | 0.85 | 2.17 | 2.901 (4) | 144 |
O2W—H4W···O4Wiii | 0.85 | 1.99 | 2.824 (4) | 168 |
O3W—H5W···O5Wiv | 0.85 | 1.91 | 2.747 (4) | 166 |
O3W—H6W···O5Wiii | 0.85 | 1.96 | 2.797 (4) | 169 |
O4W—H7W···O6 | 0.85 | 2.04 | 2.877 (4) | 169 |
O4W—H8W···O4v | 0.85 | 2.02 | 2.869 (4) | 177 |
O5W—H9W···O4 | 0.85 | 1.88 | 2.717 (4) | 170 |
O5W—H10W···O4Wvi | 0.85 | 1.93 | 2.765 (4) | 166 |
Symmetry codes: (i) −x, −y+2, −z; (ii) −x−1, −y+2, −z; (iii) −x, −y+1, −z; (iv) x, y, z−1; (v) x+1, y−1, z; (vi) −x, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) for (III) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O3i | 0.85 | 2.06 | 2.913 (4) | 180 |
O1W—H2W···O2W | 0.85 | 1.98 | 2.807 (7) | 165 |
O2W—H3W···O6ii | 0.85 | 1.94 | 2.794 (7) | 180 |
Symmetry codes: (i) −x+1, y−1, −z−1/2; (ii) −x+1, y, −z−1/2. |