Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (O-N) = 0.003 Å
- R factor = 0.016
- wR factor = 0.039
- Data-to-parameter ratio = 15.6
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
PLATON alerts of the form PLAT_7?? have been detected for an inorganic
structure. These tests are under development for inorganics and
comments are welcomed. It is not necessary to supply a data
validation response form for these alerts at this time.
Alert Level B:
REFLT_03
From the CIF: _diffrn_reflns_theta_max 30.90
From the CIF: _reflns_number_total 3448
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 3932
Completeness (_total/calc) 87.69%
Alert B: < 90% complete (theta max?)
| Author response: The data are over 99% complete to 52 deg. in 2theta.
|
PLAT_731 Alert B Bond Calc 0.83(5), Rep 0.833(10) .... 5.00 s.u-Ratio
O2 -H2A 1.555 1.555
PLAT_735 Alert B D-H Calc 0.83(5), Rep 0.833(10) .... 5.00 s.u-Ratio
O2 -H2A 1.555 1.555
PLAT_735 Alert B D-H Calc 0.83(5), Rep 0.833(10) .... 5.00 s.u-Ratio
O2 -H2A 1.555 1.555
Alert Level C:
PLAT_731 Alert C Bond Calc 0.84(3), Rep 0.837(10) .... 3.00 s.u-Ratio
O1 -H1A 1.555 1.555
PLAT_731 Alert C Bond Calc 0.83(3), Rep 0.829(10) .... 3.00 s.u-Ratio
O3 -H3B 1.555 1.555
PLAT_731 Alert C Bond Calc 0.83(3), Rep 0.836(10) .... 3.00 s.u-Ratio
O4 -H4B 1.555 1.555
PLAT_731 Alert C Bond Calc 0.83(3), Rep 0.837(10) .... 3.00 s.u-Ratio
O5 -H5A 1.555 1.555
PLAT_731 Alert C Bond Calc 0.82(4), Rep 0.827(10) .... 4.00 s.u-Ratio
O5 -H5B 1.555 1.555
PLAT_731 Alert C Bond Calc 0.84(3), Rep 0.842(10) .... 3.00 s.u-Ratio
O6 -H6A 1.555 1.555
PLAT_731 Alert C Bond Calc 0.84(3), Rep 0.835(10) .... 3.00 s.u-Ratio
O6 -H6B 1.555 1.555
PLAT_735 Alert C D-H Calc 0.84(3), Rep 0.837(10) .... 3.00 s.u-Ratio
O1 -H1A 1.555 1.555
PLAT_735 Alert C D-H Calc 0.83(3), Rep 0.829(10) .... 3.00 s.u-Ratio
O3 -H3B 1.555 1.555
PLAT_735 Alert C D-H Calc 0.83(3), Rep 0.836(10) .... 3.00 s.u-Ratio
O4 -H4B 1.555 1.555
PLAT_735 Alert C D-H Calc 0.83(3), Rep 0.837(10) .... 3.00 s.u-Ratio
O5 -H5A 1.555 1.555
PLAT_735 Alert C D-H Calc 0.82(4), Rep 0.827(10) .... 4.00 s.u-Ratio
O5 -H5B 1.555 1.555
PLAT_735 Alert C D-H Calc 0.82(4), Rep 0.827(10) .... 4.00 s.u-Ratio
O5 -H5B 1.555 1.555
PLAT_735 Alert C D-H Calc 0.84(3), Rep 0.842(10) .... 3.00 s.u-Ratio
O6 -H6A 1.555 1.555
PLAT_735 Alert C D-H Calc 0.84(3), Rep 0.835(10) .... 3.00 s.u-Ratio
O6 -H6B 1.555 1.555
PLAT_735 Alert C D-H Calc 0.84(3), Rep 0.835(10) .... 3.00 s.u-Ratio
O6 -H6B 1.555 1.555
PLAT_736 Alert C H...A Calc 1.89(3), Rep 1.889(11) .... 2.73 s.u-Ratio
H1A -O5 1.555 1.555
PLAT_736 Alert C H...A Calc 1.90(3), Rep 1.904(10) .... 3.00 s.u-Ratio
H3B -O6 1.555 1.555
PLAT_736 Alert C H...A Calc 1.86(3), Rep 1.857(13) .... 2.31 s.u-Ratio
H4A -O6 1.555 2.666
PLAT_736 Alert C H...A Calc 2.15(3), Rep 2.141(13) .... 2.31 s.u-Ratio
H4B -O22 1.555 2.566
PLAT_736 Alert C H...A Calc 2.00(3), Rep 1.993(13) .... 2.31 s.u-Ratio
H5A -O13 1.555 1.655
PLAT_736 Alert C H...A Calc 2.01(3), Rep 2.013(14) .... 2.14 s.u-Ratio
H6A -O23 1.555 2.566
0 Alert Level A = Potentially serious problem
4 Alert Level B = Potential problem
22 Alert Level C = Please check
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.
Crystal data top
[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 |
Data collection top
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 top
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) |
Crystal data top
[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)° | |
Data collection top
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 | |
Refinement top
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 | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | 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) | |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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) |
Hydrogen-bond geometry (Å, º) top
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 |
Selected bond lengths (Å) topEu1—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) |
Hydrogen-bond geometry (Å, º) top
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.