Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801001271/cf6039sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801001271/cf6039Isup2.hkl |
At 373 K, 0.352 g (1 mmol) Eu2O3 (99.99%; Across) was dissolved in 10 ml 1.0 mol l-1 HNO3. From the light yellow solution, crystals appeared at room temperature within 5 d.
All H atoms were located by difference Fourier synthesis and refined isotropically applying a restraint of 0.84 (1) Å to the O—H distances.
Data collection: SMART (Siemens, 1995); cell refinement: SMART; data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97.
Fig. 1. A perspective view of the title compound with the atom-numbering scheme. Displacement ellipsoids are at the 50% probability level. |
[Eu(NO3)3(H2O)4]·2H2O | Z = 2 |
Mr = 446.09 | F(000) = 432 |
Triclinic, P1 | Dx = 2.383 Mg m−3 |
a = 6.705 (1) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.140 (1) Å | Cell parameters from 5718 reflections |
c = 11.647 (1) Å | θ = 1–25° |
α = 69.71 (1)° | µ = 5.13 mm−1 |
β = 88.94 (1)° | T = 173 K |
γ = 69.29 (1)° | Block, colourless |
V = 621.79 (13) Å3 | 0.41 × 0.39 × 0.28 mm |
Siemens CCD three-circle diffractometer | 3448 independent reflections |
Radiation source: fine-focus sealed tube | 3284 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
ω scans | θmax = 30.9°, θmin = 1.9° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −9→9 |
Tmin = 0.148, Tmax = 0.238 | k = −11→13 |
12544 measured reflections | l = −15→15 |
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)] = 0.016 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.039 | w = 1/[σ2(Fo2) + (0.0218P)2 + 0.063P] where P = (Fo2 + 2Fc2)/3 |
S = 1.13 | (Δ/σ)max = 0.002 |
3448 reflections | Δρmax = 1.42 e Å−3 |
221 parameters | Δρmin = −0.66 e Å−3 |
12 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0410 (9) |
[Eu(NO3)3(H2O)4]·2H2O | γ = 69.29 (1)° |
Mr = 446.09 | V = 621.79 (13) Å3 |
Triclinic, P1 | Z = 2 |
a = 6.705 (1) Å | Mo Kα radiation |
b = 9.140 (1) Å | µ = 5.13 mm−1 |
c = 11.647 (1) Å | T = 173 K |
α = 69.71 (1)° | 0.41 × 0.39 × 0.28 mm |
β = 88.94 (1)° |
Siemens CCD three-circle diffractometer | 3448 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 3284 reflections with I > 2σ(I) |
Tmin = 0.148, Tmax = 0.238 | Rint = 0.022 |
12544 measured reflections |
R[F2 > 2σ(F2)] = 0.016 | 12 restraints |
wR(F2) = 0.039 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.13 | Δρmax = 1.42 e Å−3 |
3448 reflections | Δρmin = −0.66 e Å−3 |
221 parameters |
Experimental. ; |
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 | 0.196332 (13) | 0.405156 (11) | 0.274408 (8) | 0.01200 (5) | |
O1 | 0.3018 (2) | 0.4421 (2) | 0.07027 (14) | 0.0193 (3) | |
H1A | 0.403 (4) | 0.365 (3) | 0.058 (3) | 0.037 (9)* | |
H1B | 0.233 (4) | 0.506 (3) | 0.0013 (15) | 0.033 (8)* | |
O2 | 0.5736 (2) | 0.2364 (2) | 0.32478 (17) | 0.0234 (3) | |
H2A | 0.664 (6) | 0.281 (6) | 0.309 (4) | 0.082 (15)* | |
H2B | 0.631 (5) | 0.1361 (17) | 0.371 (2) | 0.031 (8)* | |
O3 | 0.3683 (3) | 0.6031 (2) | 0.22168 (14) | 0.0237 (3) | |
H3A | 0.364 (6) | 0.671 (4) | 0.1514 (16) | 0.052 (11)* | |
H3B | 0.384 (5) | 0.657 (3) | 0.263 (2) | 0.031 (8)* | |
O4 | 0.2798 (3) | 0.4476 (2) | 0.45732 (14) | 0.0197 (3) | |
H4A | 0.361 (4) | 0.370 (3) | 0.518 (2) | 0.034 (8)* | |
H4B | 0.198 (4) | 0.514 (3) | 0.487 (3) | 0.036 (8)* | |
O5 | 0.6242 (3) | 0.2030 (2) | 0.01593 (16) | 0.0227 (3) | |
H5A | 0.743 (3) | 0.159 (5) | 0.059 (3) | 0.048 (11)* | |
H5B | 0.582 (7) | 0.127 (4) | 0.020 (4) | 0.071 (14)* | |
O6 | 0.4091 (3) | 0.7789 (2) | 0.36185 (15) | 0.0206 (3) | |
H6A | 0.294 (3) | 0.825 (4) | 0.387 (3) | 0.036 (9)* | |
H6B | 0.435 (5) | 0.860 (3) | 0.313 (3) | 0.043 (10)* | |
N1 | 0.0829 (3) | 0.1757 (2) | 0.17886 (17) | 0.0200 (3) | |
O11 | −0.0578 (2) | 0.3183 (2) | 0.17037 (15) | 0.0236 (3) | |
O12 | 0.2653 (3) | 0.1373 (2) | 0.23306 (16) | 0.0271 (3) | |
O13 | 0.0423 (3) | 0.0819 (2) | 0.13757 (17) | 0.0285 (4) | |
N2 | 0.0793 (3) | 0.1669 (2) | 0.50115 (17) | 0.0186 (3) | |
O21 | 0.2703 (3) | 0.1216 (2) | 0.47951 (18) | 0.0292 (4) | |
O22 | −0.0522 (2) | 0.3068 (2) | 0.42717 (14) | 0.0218 (3) | |
O23 | 0.0183 (3) | 0.0802 (2) | 0.59053 (16) | 0.0284 (4) | |
N3 | −0.1772 (3) | 0.7254 (2) | 0.18588 (17) | 0.0182 (3) | |
O31 | −0.1021 (3) | 0.6489 (2) | 0.29835 (14) | 0.0255 (3) | |
O32 | −0.0834 (3) | 0.6566 (2) | 0.11240 (15) | 0.0262 (3) | |
O33 | −0.3340 (3) | 0.8580 (2) | 0.15067 (16) | 0.0270 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Eu1 | 0.01176 (6) | 0.01208 (6) | 0.01045 (6) | −0.00380 (4) | 0.00094 (3) | −0.00270 (4) |
O1 | 0.0219 (7) | 0.0204 (7) | 0.0131 (7) | −0.0051 (6) | 0.0030 (6) | −0.0062 (6) |
O2 | 0.0140 (7) | 0.0174 (8) | 0.0323 (9) | −0.0033 (6) | −0.0021 (6) | −0.0040 (7) |
O3 | 0.0396 (9) | 0.0263 (8) | 0.0146 (7) | −0.0228 (7) | 0.0062 (6) | −0.0077 (7) |
O4 | 0.0229 (7) | 0.0196 (8) | 0.0118 (7) | −0.0033 (6) | −0.0015 (5) | −0.0047 (6) |
O5 | 0.0278 (8) | 0.0189 (8) | 0.0211 (8) | −0.0106 (6) | 0.0033 (6) | −0.0050 (6) |
O6 | 0.0234 (7) | 0.0175 (7) | 0.0189 (7) | −0.0069 (6) | 0.0005 (6) | −0.0046 (6) |
N1 | 0.0259 (9) | 0.0177 (8) | 0.0155 (8) | −0.0103 (7) | −0.0010 (7) | −0.0025 (7) |
O11 | 0.0197 (7) | 0.0240 (8) | 0.0271 (8) | −0.0065 (6) | −0.0006 (6) | −0.0109 (7) |
O12 | 0.0245 (8) | 0.0170 (7) | 0.0348 (9) | −0.0060 (6) | −0.0097 (7) | −0.0049 (7) |
O13 | 0.0377 (9) | 0.0229 (8) | 0.0285 (9) | −0.0147 (7) | −0.0033 (7) | −0.0097 (7) |
N2 | 0.0204 (8) | 0.0160 (8) | 0.0194 (9) | −0.0061 (7) | 0.0048 (7) | −0.0070 (7) |
O21 | 0.0179 (7) | 0.0238 (8) | 0.0419 (10) | −0.0044 (6) | 0.0093 (7) | −0.0108 (8) |
O22 | 0.0190 (7) | 0.0192 (7) | 0.0197 (7) | −0.0052 (6) | 0.0010 (6) | −0.0004 (6) |
O23 | 0.0351 (9) | 0.0210 (8) | 0.0219 (8) | −0.0098 (7) | 0.0110 (7) | −0.0002 (7) |
N3 | 0.0158 (7) | 0.0130 (8) | 0.0221 (9) | −0.0048 (6) | 0.0023 (6) | −0.0026 (7) |
O31 | 0.0271 (8) | 0.0224 (8) | 0.0148 (7) | 0.0006 (6) | 0.0028 (6) | −0.0024 (6) |
O32 | 0.0275 (8) | 0.0247 (8) | 0.0181 (7) | 0.0004 (6) | −0.0015 (6) | −0.0082 (6) |
O33 | 0.0212 (7) | 0.0144 (7) | 0.0321 (9) | 0.0003 (6) | 0.0018 (6) | 0.0000 (7) |
Eu1—O3 | 2.3787 (16) | O3—H3B | 0.829 (10) |
Eu1—O4 | 2.4029 (15) | O4—H4A | 0.837 (10) |
Eu1—O2 | 2.4063 (16) | O4—H4B | 0.836 (10) |
Eu1—O1 | 2.4118 (15) | O5—H5A | 0.837 (10) |
Eu1—O31 | 2.5105 (16) | O5—H5B | 0.827 (10) |
Eu1—O32 | 2.5364 (17) | O6—H6A | 0.842 (10) |
Eu1—O12 | 2.5396 (18) | O6—H6B | 0.835 (10) |
Eu1—O22 | 2.5671 (16) | N1—O13 | 1.223 (2) |
Eu1—O11 | 2.5891 (16) | N1—O12 | 1.260 (2) |
Eu1—O21 | 2.7407 (19) | N1—O11 | 1.282 (2) |
Eu1—N3 | 2.9531 (18) | N2—O23 | 1.233 (2) |
Eu1—N1 | 2.9988 (18) | N2—O21 | 1.249 (2) |
O1—H1A | 0.837 (10) | N2—O22 | 1.274 (2) |
O1—H1B | 0.835 (10) | N3—O33 | 1.229 (2) |
O2—H2A | 0.833 (10) | N3—O32 | 1.264 (2) |
O2—H2B | 0.834 (10) | N3—O31 | 1.264 (2) |
O3—H3A | 0.831 (10) | ||
O3—Eu1—O4 | 71.13 (5) | O22—Eu1—N3 | 83.52 (5) |
O3—Eu1—O2 | 75.47 (6) | O11—Eu1—N3 | 80.41 (5) |
O4—Eu1—O2 | 78.48 (6) | O21—Eu1—N3 | 130.45 (5) |
O3—Eu1—O1 | 71.16 (5) | O3—Eu1—N1 | 141.67 (5) |
O4—Eu1—O1 | 140.04 (6) | O4—Eu1—N1 | 144.56 (5) |
O2—Eu1—O1 | 79.82 (6) | O2—Eu1—N1 | 95.53 (5) |
O3—Eu1—O31 | 81.24 (6) | O1—Eu1—N1 | 70.59 (5) |
O4—Eu1—O31 | 69.50 (5) | O31—Eu1—N1 | 118.58 (6) |
O2—Eu1—O31 | 145.10 (6) | O32—Eu1—N1 | 89.77 (5) |
O1—Eu1—O31 | 116.70 (5) | O12—Eu1—N1 | 24.56 (5) |
O3—Eu1—O32 | 78.54 (6) | O22—Eu1—N1 | 77.16 (5) |
O4—Eu1—O32 | 115.56 (5) | O11—Eu1—N1 | 25.17 (5) |
O2—Eu1—O32 | 144.17 (6) | O21—Eu1—N1 | 76.28 (5) |
O1—Eu1—O32 | 68.63 (5) | N3—Eu1—N1 | 105.26 (5) |
O31—Eu1—O32 | 50.31 (5) | Eu1—O1—H1A | 120 (2) |
O3—Eu1—O12 | 132.73 (6) | Eu1—O1—H1B | 130 (2) |
O4—Eu1—O12 | 130.94 (5) | H1A—O1—H1B | 106 (3) |
O2—Eu1—O12 | 71.26 (5) | Eu1—O2—H2A | 120 (3) |
O1—Eu1—O12 | 70.69 (6) | Eu1—O2—H2B | 128 (2) |
O31—Eu1—O12 | 141.74 (6) | H2A—O2—H2B | 111 (4) |
O32—Eu1—O12 | 111.56 (5) | Eu1—O3—H3A | 126 (3) |
O3—Eu1—O22 | 140.43 (5) | Eu1—O3—H3B | 127 (2) |
O4—Eu1—O22 | 74.67 (5) | H3A—O3—H3B | 99 (3) |
O2—Eu1—O22 | 116.43 (6) | Eu1—O4—H4A | 122 (2) |
O1—Eu1—O22 | 145.29 (5) | Eu1—O4—H4B | 127 (2) |
O31—Eu1—O22 | 68.47 (5) | H4A—O4—H4B | 104 (3) |
O32—Eu1—O22 | 99.31 (5) | H5A—O5—H5B | 107 (4) |
O12—Eu1—O22 | 85.27 (6) | H6A—O6—H6B | 104 (3) |
O3—Eu1—O11 | 139.30 (5) | O13—N1—O12 | 122.0 (2) |
O4—Eu1—O11 | 144.49 (5) | O13—N1—O11 | 121.99 (19) |
O2—Eu1—O11 | 120.55 (5) | O12—N1—O11 | 116.05 (18) |
O1—Eu1—O11 | 75.35 (5) | O13—N1—Eu1 | 177.86 (16) |
O31—Eu1—O11 | 94.01 (6) | O12—N1—Eu1 | 56.86 (11) |
O32—Eu1—O11 | 68.05 (6) | O11—N1—Eu1 | 59.23 (10) |
O12—Eu1—O11 | 49.71 (5) | N1—O11—Eu1 | 95.59 (11) |
O22—Eu1—O11 | 69.98 (5) | N1—O12—Eu1 | 98.58 (13) |
O3—Eu1—O21 | 130.44 (6) | O23—N2—O21 | 121.78 (19) |
O4—Eu1—O21 | 68.94 (6) | O23—N2—O22 | 120.60 (18) |
O2—Eu1—O21 | 68.88 (6) | O21—N2—O22 | 117.62 (18) |
O1—Eu1—O21 | 131.34 (5) | O23—N2—Eu1 | 175.47 (14) |
O31—Eu1—O21 | 110.12 (5) | O21—N2—Eu1 | 62.72 (11) |
O32—Eu1—O21 | 146.13 (5) | O22—N2—Eu1 | 54.91 (10) |
O12—Eu1—O21 | 64.53 (6) | N2—O21—Eu1 | 93.40 (12) |
O22—Eu1—O21 | 47.84 (5) | N2—O22—Eu1 | 101.14 (12) |
O11—Eu1—O21 | 89.30 (5) | O33—N3—O32 | 122.17 (18) |
O3—Eu1—N3 | 78.76 (6) | O33—N3—O31 | 121.72 (19) |
O4—Eu1—N3 | 92.52 (5) | O32—N3—O31 | 116.09 (17) |
O2—Eu1—N3 | 154.22 (5) | O33—N3—Eu1 | 179.03 (15) |
O1—Eu1—N3 | 92.71 (5) | O32—N3—Eu1 | 58.64 (10) |
O31—Eu1—N3 | 25.12 (5) | O31—N3—Eu1 | 57.46 (10) |
O32—Eu1—N3 | 25.19 (5) | N3—O31—Eu1 | 97.42 (12) |
O12—Eu1—N3 | 129.61 (5) | N3—O32—Eu1 | 96.18 (11) |
O3—Eu1—N1—O12 | 82.21 (15) | O3—Eu1—O21—N2 | 126.05 (12) |
O4—Eu1—N1—O12 | −69.16 (16) | O4—Eu1—O21—N2 | 87.64 (13) |
O2—Eu1—N1—O12 | 8.71 (13) | O2—Eu1—O21—N2 | 173.01 (14) |
O1—Eu1—N1—O12 | 85.86 (13) | O1—Eu1—O21—N2 | −133.32 (12) |
O31—Eu1—N1—O12 | −163.62 (12) | O31—Eu1—O21—N2 | 30.36 (14) |
O32—Eu1—N1—O12 | 153.22 (13) | O32—Eu1—O21—N2 | −17.20 (18) |
O22—Eu1—N1—O12 | −107.18 (13) | O12—Eu1—O21—N2 | −108.39 (14) |
O11—Eu1—N1—O12 | −177.3 (2) | O22—Eu1—O21—N2 | −0.44 (11) |
O21—Eu1—N1—O12 | −57.95 (13) | O11—Eu1—O21—N2 | −63.66 (13) |
N3—Eu1—N1—O12 | 173.32 (13) | N3—Eu1—O21—N2 | 13.08 (16) |
O3—Eu1—N1—O11 | −100.51 (14) | N1—Eu1—O21—N2 | −85.42 (13) |
O4—Eu1—N1—O11 | 108.12 (13) | O23—N2—O22—Eu1 | 179.29 (17) |
O2—Eu1—N1—O11 | −174.01 (12) | O21—N2—O22—Eu1 | −0.8 (2) |
O1—Eu1—N1—O11 | −96.87 (12) | O3—Eu1—O22—N2 | −105.69 (14) |
O31—Eu1—N1—O11 | 13.66 (13) | O4—Eu1—O22—N2 | −74.82 (12) |
O32—Eu1—N1—O11 | −29.50 (12) | O2—Eu1—O22—N2 | −6.38 (14) |
O12—Eu1—N1—O11 | 177.3 (2) | O1—Eu1—O22—N2 | 105.39 (13) |
O22—Eu1—N1—O11 | 70.10 (12) | O31—Eu1—O22—N2 | −148.43 (13) |
O21—Eu1—N1—O11 | 119.33 (12) | O32—Eu1—O22—N2 | 171.07 (12) |
N3—Eu1—N1—O11 | −9.40 (13) | O12—Eu1—O22—N2 | 59.97 (12) |
O13—N1—O11—Eu1 | −177.95 (18) | O11—Eu1—O22—N2 | 108.64 (13) |
O12—N1—O11—Eu1 | 2.54 (19) | O21—Eu1—O22—N2 | 0.44 (11) |
O3—Eu1—O11—N1 | 110.77 (13) | N3—Eu1—O22—N2 | −169.24 (13) |
O4—Eu1—O11—N1 | −108.40 (13) | N1—Eu1—O22—N2 | 83.45 (12) |
O2—Eu1—O11—N1 | 6.93 (14) | O3—Eu1—N3—O32 | 86.93 (13) |
O1—Eu1—O11—N1 | 75.43 (12) | O4—Eu1—N3—O32 | 157.12 (13) |
O31—Eu1—O11—N1 | −168.00 (12) | O2—Eu1—N3—O32 | 88.74 (18) |
O32—Eu1—O11—N1 | 147.93 (13) | O1—Eu1—N3—O32 | 16.75 (13) |
O12—Eu1—O11—N1 | −1.48 (11) | O31—Eu1—N3—O32 | −179.7 (2) |
O22—Eu1—O11—N1 | −102.66 (12) | O12—Eu1—N3—O32 | −50.26 (15) |
O21—Eu1—O11—N1 | −57.89 (12) | O22—Eu1—N3—O32 | −128.62 (13) |
N3—Eu1—O11—N1 | 170.80 (12) | O11—Eu1—N3—O32 | −57.90 (13) |
O13—N1—O12—Eu1 | 177.88 (18) | O21—Eu1—N3—O32 | −138.67 (12) |
O11—N1—O12—Eu1 | −2.60 (19) | N1—Eu1—N3—O32 | −53.86 (13) |
O3—Eu1—O12—N1 | −123.22 (13) | O3—Eu1—N3—O31 | −93.33 (13) |
O4—Eu1—O12—N1 | 134.16 (12) | O4—Eu1—N3—O31 | −23.14 (13) |
O2—Eu1—O12—N1 | −170.84 (14) | O2—Eu1—N3—O31 | −91.52 (18) |
O1—Eu1—O12—N1 | −85.37 (13) | O1—Eu1—N3—O31 | −163.51 (13) |
O31—Eu1—O12—N1 | 23.58 (17) | O32—Eu1—N3—O31 | 179.7 (2) |
O32—Eu1—O12—N1 | −28.98 (14) | O12—Eu1—N3—O31 | 129.48 (13) |
O22—Eu1—O12—N1 | 69.18 (13) | O22—Eu1—N3—O31 | 51.12 (13) |
O11—Eu1—O12—N1 | 1.52 (11) | O11—Eu1—N3—O31 | 121.84 (13) |
O21—Eu1—O12—N1 | 114.22 (14) | O21—Eu1—N3—O31 | 41.07 (15) |
N3—Eu1—O12—N1 | −8.38 (16) | N1—Eu1—N3—O31 | 125.88 (13) |
O3—Eu1—N2—O21 | −76.58 (15) | O33—N3—O31—Eu1 | 179.38 (17) |
O4—Eu1—N2—O21 | −83.25 (13) | O32—N3—O31—Eu1 | 0.25 (19) |
O2—Eu1—N2—O21 | −6.53 (13) | O3—Eu1—O31—N3 | 82.19 (13) |
O1—Eu1—N2—O21 | 69.57 (16) | O4—Eu1—O31—N3 | 155.22 (14) |
O31—Eu1—N2—O21 | −151.66 (13) | O2—Eu1—O31—N3 | 130.54 (13) |
O32—Eu1—N2—O21 | 168.68 (12) | O1—Eu1—O31—N3 | 18.50 (14) |
O12—Eu1—N2—O21 | 63.11 (13) | O32—Eu1—O31—N3 | −0.14 (11) |
O22—Eu1—N2—O21 | 179.2 (2) | O12—Eu1—O31—N3 | −73.80 (15) |
O11—Eu1—N2—O21 | 114.10 (13) | O22—Eu1—O31—N3 | −123.75 (13) |
N3—Eu1—N2—O21 | −169.62 (12) | O11—Eu1—O31—N3 | −57.11 (13) |
N1—Eu1—N2—O21 | 88.51 (13) | O21—Eu1—O31—N3 | −147.83 (12) |
O3—Eu1—N2—O22 | 104.23 (14) | N1—Eu1—O31—N3 | −62.89 (14) |
O4—Eu1—N2—O22 | 97.56 (13) | O33—N3—O32—Eu1 | −179.37 (17) |
O2—Eu1—N2—O22 | 174.28 (13) | O31—N3—O32—Eu1 | −0.24 (19) |
O1—Eu1—N2—O22 | −109.61 (13) | O3—Eu1—O32—N3 | −87.93 (13) |
O31—Eu1—N2—O22 | 29.15 (12) | O4—Eu1—O32—N3 | −25.50 (14) |
O32—Eu1—N2—O22 | −10.51 (14) | O2—Eu1—O32—N3 | −132.03 (12) |
O12—Eu1—N2—O22 | −116.08 (13) | O1—Eu1—O32—N3 | −161.99 (14) |
O11—Eu1—N2—O22 | −65.09 (12) | O31—Eu1—O32—N3 | 0.14 (11) |
O21—Eu1—N2—O22 | −179.2 (2) | O12—Eu1—O32—N3 | 140.44 (12) |
N3—Eu1—N2—O22 | 11.19 (13) | O22—Eu1—O32—N3 | 51.87 (13) |
N1—Eu1—N2—O22 | −90.68 (13) | O11—Eu1—O32—N3 | 115.77 (13) |
O23—N2—O21—Eu1 | −179.36 (18) | O21—Eu1—O32—N3 | 64.38 (16) |
O22—N2—O21—Eu1 | 0.75 (19) | N1—Eu1—O32—N3 | 128.82 (13) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O5 | 0.84 (1) | 1.89 (1) | 2.723 (2) | 175 (3) |
O1—H1B···O11i | 0.84 (1) | 2.12 (1) | 2.951 (2) | 176 (3) |
O2—H2A···O11ii | 0.83 (1) | 2.48 (3) | 3.180 (2) | 143 (4) |
O2—H2A···O22ii | 0.83 (1) | 2.49 (3) | 3.149 (2) | 137 (4) |
O2—H2B···O21iii | 0.83 (1) | 2.26 (1) | 3.081 (2) | 168 (3) |
O2—H2B···O23iii | 0.83 (1) | 2.40 (2) | 3.058 (2) | 136 (3) |
O3—H3A···O5iv | 0.83 (1) | 1.91 (1) | 2.731 (2) | 171 (4) |
O3—H3B···O6 | 0.83 (1) | 1.90 (1) | 2.733 (2) | 177 (3) |
O4—H4A···O6v | 0.84 (1) | 1.86 (1) | 2.675 (2) | 165 (3) |
O4—H4B···O22vi | 0.84 (1) | 2.14 (1) | 2.962 (2) | 167 (3) |
O5—H5A···O13ii | 0.84 (1) | 1.99 (1) | 2.821 (3) | 170 (4) |
O5—H5B···O33vii | 0.83 (1) | 2.26 (3) | 2.906 (2) | 135 (4) |
O5—H5B···O33i | 0.83 (1) | 2.55 (4) | 3.085 (3) | 124 (4) |
O6—H6A···O23vi | 0.84 (1) | 2.01 (1) | 2.829 (2) | 163 (3) |
O6—H6B···O12viii | 0.84 (1) | 2.23 (3) | 2.885 (2) | 136 (3) |
O6—H6B···O33ii | 0.84 (1) | 2.42 (3) | 3.005 (2) | 128 (3) |
Symmetry codes: (i) −x, −y+1, −z; (ii) x+1, y, z; (iii) −x+1, −y, −z+1; (iv) −x+1, −y+1, −z; (v) −x+1, −y+1, −z+1; (vi) −x, −y+1, −z+1; (vii) x+1, y−1, z; (viii) x, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | [Eu(NO3)3(H2O)4]·2H2O |
Mr | 446.09 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 173 |
a, b, c (Å) | 6.705 (1), 9.140 (1), 11.647 (1) |
α, β, γ (°) | 69.71 (1), 88.94 (1), 69.29 (1) |
V (Å3) | 621.79 (13) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 5.13 |
Crystal size (mm) | 0.41 × 0.39 × 0.28 |
Data collection | |
Diffractometer | Siemens CCD three-circle diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.148, 0.238 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12544, 3448, 3284 |
Rint | 0.022 |
(sin θ/λ)max (Å−1) | 0.723 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.016, 0.039, 1.13 |
No. of reflections | 3448 |
No. of parameters | 221 |
No. of restraints | 12 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.42, −0.66 |
Computer programs: SMART (Siemens, 1995), SMART, SAINT (Siemens, 1995), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP in SHELXTL-Plus (Sheldrick, 1991), SHELXL97.
Eu1—O3 | 2.3787 (16) | Eu1—O32 | 2.5364 (17) |
Eu1—O4 | 2.4029 (15) | Eu1—O12 | 2.5396 (18) |
Eu1—O2 | 2.4063 (16) | Eu1—O22 | 2.5671 (16) |
Eu1—O1 | 2.4118 (15) | Eu1—O11 | 2.5891 (16) |
Eu1—O31 | 2.5105 (16) | Eu1—O21 | 2.7407 (19) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O5 | 0.837 (10) | 1.889 (11) | 2.723 (2) | 175 (3) |
O1—H1B···O11i | 0.835 (10) | 2.117 (11) | 2.951 (2) | 176 (3) |
O2—H2A···O11ii | 0.833 (10) | 2.48 (3) | 3.180 (2) | 143 (4) |
O2—H2A···O22ii | 0.833 (10) | 2.49 (3) | 3.149 (2) | 137 (4) |
O2—H2B···O21iii | 0.834 (10) | 2.260 (12) | 3.081 (2) | 168 (3) |
O2—H2B···O23iii | 0.834 (10) | 2.40 (2) | 3.058 (2) | 136 (3) |
O3—H3A···O5iv | 0.831 (10) | 1.906 (12) | 2.731 (2) | 171 (4) |
O3—H3B···O6 | 0.829 (10) | 1.904 (10) | 2.733 (2) | 177 (3) |
O4—H4A···O6v | 0.837 (10) | 1.857 (13) | 2.675 (2) | 165 (3) |
O4—H4B···O22vi | 0.836 (10) | 2.141 (13) | 2.962 (2) | 167 (3) |
O5—H5A···O13ii | 0.837 (10) | 1.993 (13) | 2.821 (3) | 170 (4) |
O5—H5B···O33vii | 0.827 (10) | 2.26 (3) | 2.906 (2) | 135 (4) |
O5—H5B···O33i | 0.827 (10) | 2.55 (4) | 3.085 (3) | 124 (4) |
O6—H6A···O23vi | 0.842 (10) | 2.013 (14) | 2.829 (2) | 163 (3) |
O6—H6B···O12viii | 0.835 (10) | 2.23 (3) | 2.885 (2) | 136 (3) |
O6—H6B···O33ii | 0.835 (10) | 2.42 (3) | 3.005 (2) | 128 (3) |
Symmetry codes: (i) −x, −y+1, −z; (ii) x+1, y, z; (iii) −x+1, −y, −z+1; (iv) −x+1, −y+1, −z; (v) −x+1, −y+1, −z+1; (vi) −x, −y+1, −z+1; (vii) x+1, y−1, z; (viii) x, y+1, z. |
In the series of tetraaquatrinitratolanthanide dihydrates, the structures from cerbium to terbium with the exception of the Pm and Eu compounds are known. Whereas this fact is not astonishing in the case of promethium, which is radioactive, it is surprising that the europium structure has not been determined yet. In order to fill this gap, we present in this article the structure of [Eu(NO3)3(H2O)4].2H2O.
Three bidentate nitrates and four coordinated water molecules produce a ten-coordinated europium with six different Eu—O bonds between 2.511 (2) and 2.741 (2) Å to the nitrate groups and four slightly shorter bonds to water molecules between 2.379 (2) and 2.412 (2) Å. One nitrate ion is asymmetrically bonded and the Eu—O21 distance is about 0.2 Å longer than the other Eu—O distances. Two further H2O molecules in the second coordination sphere of the europium are included as crystal water. The three nitrate groups are located on the same side of the Eu ion, while the water molecules are located on the other side. The crystal packing is stabilized by a complicated network of hydrogen bonds.
The structure of the title compound is isostructural with the already known [Ln(NO3)3(H2O)4].2H2O structures [Ln = Pr (Fuller & Jacobsen, 1976; Volodina et al., 1961; Rumanova et al., 1964), Nd (Rogers et al., 1983; Shi & Wang, 1991), Sm (Shi & Wang, 1990), Gd (Ma et al., 1991) and Tb (Moret et al., 1990)]. It fits well into and completes this series.