Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270104005773/av1173sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270104005773/av1173Isup2.hkl |
CCDC reference: 237918
The title compound was synthesized using the hydrothermal method, from a mixture of 2,3-pyrazinedicarboxylic acid (1 mmol, 0.17 g), Eu(NO3)3·6H2O (1 mmol, 0.45 g), 1,10-phenanthroline (3 mmol, 0.54 g) and water (20 ml) in a 30 ml Teflon-lined stainless steel reactor. The solution was heated at 432 K for 5 d. After the reaction system was cooled slowly to room temperature, colorless prismatic crystals were collected and washed with distilled water.
H atoms of water molecules were placed at idealized positions but were not refined; their Uiso(H) values were set at 1.2Ueq(O). Atom O2W is disordered over two sites, the occupancies of which were fixed at 0.5. A l l other H atoms were positioned geometrically and allowed to ride on their parent atoms at distances of 0.93 Å, with Uiso(H) values of 1.2Ueq(parent atom). The final difference Fourier map had a large peak near atom Eu1.
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Bruker, 2002); software used to prepare material for publication: SHELXL97.
[Eu(C6H2O4)(NO3)(C12H8N2)(H2O)]·H2O | F(000) = 1168 |
Mr = 596.30 | Dx = 1.981 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 4140 reflections |
a = 12.3427 (3) Å | θ = 2.4–27.1° |
b = 10.4806 (3) Å | µ = 3.20 mm−1 |
c = 15.7966 (4) Å | T = 298 K |
β = 101.947 (1)° | Prism, colorless |
V = 1999.17 (9) Å3 | 0.28 × 0.18 × 0.17 mm |
Z = 4 |
Bruker SMART APEX area-detector diffractometer | 4497 independent reflections |
Radiation source: fine-focus sealed tube | 3676 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
ϕ and ω scan | θmax = 27.5°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −14→15 |
Tmin = 0.468, Tmax = 0.612 | k = −13→11 |
11996 measured reflections | l = −14→20 |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.095 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0545P)2] where P = (Fo2 + 2Fc2)/3 |
4497 reflections | (Δ/σ)max = 0.001 |
301 parameters | Δρmax = 1.65 e Å−3 |
0 restraints | Δρmin = −0.82 e Å−3 |
[Eu(C6H2O4)(NO3)(C12H8N2)(H2O)]·H2O | V = 1999.17 (9) Å3 |
Mr = 596.30 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 12.3427 (3) Å | µ = 3.20 mm−1 |
b = 10.4806 (3) Å | T = 298 K |
c = 15.7966 (4) Å | 0.28 × 0.18 × 0.17 mm |
β = 101.947 (1)° |
Bruker SMART APEX area-detector diffractometer | 4497 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | 3676 reflections with I > 2σ(I) |
Tmin = 0.468, Tmax = 0.612 | Rint = 0.035 |
11996 measured reflections |
R[F2 > 2σ(F2)] = 0.038 | 0 restraints |
wR(F2) = 0.095 | H-atom parameters constrained |
S = 1.04 | Δρmax = 1.65 e Å−3 |
4497 reflections | Δρmin = −0.82 e Å−3 |
301 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Eu1 | 0.667050 (18) | 0.577623 (19) | 0.633356 (13) | 0.02142 (9) | |
O1 | 0.6656 (3) | 0.7790 (3) | 0.6956 (2) | 0.0338 (8) | |
O2 | 0.6387 (3) | 0.9166 (3) | 0.7976 (2) | 0.0399 (9) | |
O3 | 0.4351 (3) | 0.8816 (3) | 0.8781 (2) | 0.0316 (7) | |
O4 | 0.5777 (3) | 0.8828 (4) | 0.9898 (2) | 0.0450 (10) | |
O5 | 0.8561 (3) | 0.5801 (3) | 0.7304 (2) | 0.0381 (9) | |
O6 | 0.7747 (3) | 0.3975 (3) | 0.7223 (2) | 0.0351 (8) | |
O7 | 0.9392 (3) | 0.4190 (3) | 0.8027 (3) | 0.0514 (11) | |
O1W | 0.4650 (3) | 0.6294 (4) | 0.6255 (3) | 0.0532 (11) | |
H1W1 | 0.4591 | 0.7068 | 0.6569 | 0.064* | |
H1W2 | 0.4306 | 0.5609 | 0.6508 | 0.064* | |
O2W | 0.3504 (9) | 0.6612 (9) | 0.7435 (6) | 0.077 (2) | 0.50 |
H2W1 | 0.3204 | 0.6358 | 0.7933 | 0.093* | 0.50 |
H2W2 | 0.3832 | 0.7300 | 0.7661 | 0.093* | 0.50 |
O2W' | 0.2642 (10) | 0.6030 (9) | 0.8223 (6) | 0.077 (2) | 0.50 |
H2W' | 0.3204 | 0.6358 | 0.7933 | 0.093* | 0.50 |
H2W" | 0.2507 | 0.5242 | 0.8065 | 0.093* | 0.50 |
N1 | 0.7733 (3) | 0.4522 (4) | 0.5357 (3) | 0.0298 (9) | |
N2 | 0.7978 (3) | 0.7092 (4) | 0.5604 (2) | 0.0314 (9) | |
N3 | 0.6249 (3) | 0.5815 (3) | 0.7877 (2) | 0.0253 (8) | |
N4 | 0.5386 (4) | 0.6093 (4) | 0.9354 (3) | 0.0374 (11) | |
N5 | 0.8594 (4) | 0.4646 (4) | 0.7530 (3) | 0.0312 (9) | |
C1 | 0.7664 (5) | 0.3262 (5) | 0.5249 (4) | 0.0405 (13) | |
H1 | 0.7320 | 0.2793 | 0.5618 | 0.049* | |
C2 | 0.8072 (5) | 0.2607 (5) | 0.4622 (4) | 0.0486 (15) | |
H2 | 0.7997 | 0.1725 | 0.4570 | 0.058* | |
C3 | 0.8584 (5) | 0.3275 (7) | 0.4084 (4) | 0.0546 (17) | |
H3 | 0.8861 | 0.2849 | 0.3657 | 0.065* | |
C4 | 0.8699 (4) | 0.4602 (6) | 0.4163 (4) | 0.0429 (14) | |
C5 | 0.9218 (5) | 0.5364 (7) | 0.3612 (4) | 0.0578 (17) | |
H5 | 0.9505 | 0.4975 | 0.3178 | 0.069* | |
C6 | 0.9296 (5) | 0.6625 (7) | 0.3712 (4) | 0.0548 (17) | |
H6 | 0.9621 | 0.7100 | 0.3334 | 0.066* | |
C7 | 0.8893 (4) | 0.7271 (6) | 0.4387 (3) | 0.0443 (14) | |
C8 | 0.9024 (5) | 0.8576 (6) | 0.4539 (4) | 0.0487 (15) | |
H8 | 0.9368 | 0.9080 | 0.4188 | 0.058* | |
C9 | 0.8645 (5) | 0.9100 (5) | 0.5206 (5) | 0.0512 (16) | |
H9 | 0.8726 | 0.9970 | 0.5315 | 0.061* | |
C10 | 0.8136 (5) | 0.8336 (5) | 0.5725 (4) | 0.0415 (13) | |
H10 | 0.7891 | 0.8718 | 0.6183 | 0.050* | |
C11 | 0.8262 (4) | 0.5184 (5) | 0.4823 (3) | 0.0305 (11) | |
C12 | 0.8379 (4) | 0.6540 (5) | 0.4943 (3) | 0.0326 (11) | |
C13 | 0.6398 (4) | 0.8080 (4) | 0.7672 (3) | 0.0261 (10) | |
C14 | 0.6072 (4) | 0.6974 (4) | 0.8169 (3) | 0.0219 (9) | |
C15 | 0.5601 (4) | 0.7107 (4) | 0.8902 (3) | 0.0263 (10) | |
C16 | 0.5598 (5) | 0.4954 (5) | 0.9060 (3) | 0.0412 (14) | |
H16 | 0.5466 | 0.4232 | 0.9365 | 0.049* | |
C17 | 0.6008 (4) | 0.4805 (5) | 0.8320 (3) | 0.0329 (11) | |
H17 | 0.6118 | 0.3988 | 0.8124 | 0.039* | |
C18 | 0.5229 (4) | 0.8369 (4) | 0.9212 (3) | 0.0265 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Eu1 | 0.02926 (14) | 0.02140 (14) | 0.01505 (13) | −0.00164 (9) | 0.00792 (9) | −0.00057 (9) |
O1 | 0.056 (2) | 0.0250 (17) | 0.0262 (18) | −0.0036 (15) | 0.0210 (16) | −0.0012 (14) |
O2 | 0.065 (3) | 0.0237 (19) | 0.039 (2) | −0.0030 (15) | 0.0270 (19) | −0.0077 (14) |
O3 | 0.0324 (19) | 0.0320 (17) | 0.0296 (19) | 0.0052 (15) | 0.0045 (15) | −0.0030 (15) |
O4 | 0.052 (2) | 0.053 (2) | 0.0238 (19) | 0.0167 (19) | −0.0082 (17) | −0.0221 (17) |
O5 | 0.040 (2) | 0.038 (2) | 0.034 (2) | −0.0041 (15) | 0.0031 (17) | 0.0049 (15) |
O6 | 0.040 (2) | 0.0292 (18) | 0.036 (2) | −0.0014 (15) | 0.0064 (16) | 0.0015 (15) |
O7 | 0.039 (2) | 0.064 (3) | 0.045 (3) | 0.0093 (18) | −0.0036 (19) | 0.0162 (19) |
O1W | 0.041 (2) | 0.046 (2) | 0.070 (3) | 0.0055 (19) | 0.005 (2) | −0.018 (2) |
O2W | 0.104 (6) | 0.068 (4) | 0.063 (5) | −0.013 (4) | 0.024 (4) | −0.017 (4) |
O2W' | 0.104 (6) | 0.068 (4) | 0.063 (5) | −0.013 (4) | 0.024 (4) | −0.017 (4) |
N1 | 0.033 (2) | 0.031 (2) | 0.026 (2) | 0.0023 (17) | 0.0075 (18) | 0.0025 (17) |
N2 | 0.035 (2) | 0.033 (2) | 0.028 (2) | −0.0072 (18) | 0.0084 (18) | 0.0020 (17) |
N3 | 0.031 (2) | 0.027 (2) | 0.0192 (19) | 0.0016 (16) | 0.0085 (16) | −0.0019 (15) |
N4 | 0.057 (3) | 0.035 (2) | 0.027 (2) | 0.007 (2) | 0.024 (2) | 0.0068 (18) |
N5 | 0.034 (2) | 0.040 (2) | 0.022 (2) | 0.0041 (19) | 0.0100 (18) | 0.0010 (18) |
C1 | 0.044 (3) | 0.036 (3) | 0.041 (3) | 0.003 (2) | 0.007 (2) | 0.001 (2) |
C2 | 0.057 (4) | 0.037 (3) | 0.051 (4) | 0.011 (3) | 0.008 (3) | −0.011 (3) |
C3 | 0.050 (4) | 0.069 (4) | 0.042 (3) | 0.021 (3) | 0.005 (3) | −0.019 (3) |
C4 | 0.034 (3) | 0.064 (4) | 0.032 (3) | 0.011 (3) | 0.009 (2) | −0.006 (3) |
C5 | 0.048 (4) | 0.100 (5) | 0.034 (3) | 0.005 (4) | 0.027 (3) | −0.003 (3) |
C6 | 0.039 (3) | 0.092 (5) | 0.036 (3) | −0.006 (3) | 0.015 (3) | 0.014 (3) |
C7 | 0.035 (3) | 0.069 (4) | 0.029 (3) | −0.005 (3) | 0.007 (2) | 0.015 (3) |
C8 | 0.040 (3) | 0.058 (4) | 0.046 (4) | −0.018 (3) | 0.004 (3) | 0.026 (3) |
C9 | 0.050 (4) | 0.038 (3) | 0.061 (4) | −0.018 (3) | 0.002 (3) | 0.012 (3) |
C10 | 0.049 (3) | 0.036 (3) | 0.040 (3) | −0.016 (2) | 0.011 (3) | −0.002 (2) |
C11 | 0.027 (3) | 0.045 (3) | 0.021 (2) | 0.004 (2) | 0.0063 (19) | 0.001 (2) |
C12 | 0.028 (3) | 0.044 (3) | 0.024 (2) | −0.004 (2) | 0.003 (2) | 0.007 (2) |
C13 | 0.033 (3) | 0.026 (2) | 0.021 (2) | 0.0001 (19) | 0.007 (2) | −0.0027 (18) |
C14 | 0.027 (2) | 0.021 (2) | 0.016 (2) | 0.0038 (17) | 0.0030 (18) | −0.0007 (17) |
C15 | 0.030 (3) | 0.034 (3) | 0.015 (2) | 0.004 (2) | 0.0070 (18) | −0.0001 (19) |
C16 | 0.072 (4) | 0.028 (3) | 0.032 (3) | 0.007 (3) | 0.028 (3) | 0.008 (2) |
C17 | 0.054 (3) | 0.021 (2) | 0.028 (3) | 0.006 (2) | 0.019 (2) | 0.002 (2) |
C18 | 0.032 (3) | 0.029 (2) | 0.021 (2) | 0.0038 (19) | 0.012 (2) | −0.0005 (19) |
Eu1—O1 | 2.331 (3) | N3—C17 | 1.335 (6) |
Eu1—O4i | 2.344 (3) | N4—C16 | 1.326 (6) |
Eu1—O3ii | 2.398 (3) | N4—C15 | 1.337 (6) |
Eu1—O5 | 2.513 (4) | C1—C2 | 1.383 (7) |
Eu1—O1W | 2.530 (4) | C1—H1 | 0.9300 |
Eu1—O6 | 2.555 (3) | C2—C3 | 1.354 (8) |
Eu1—N2 | 2.570 (4) | C2—H2 | 0.9300 |
Eu1—N1 | 2.582 (4) | C3—C4 | 1.401 (9) |
Eu1—N3 | 2.597 (4) | C3—H3 | 0.9300 |
O1—C13 | 1.272 (5) | C4—C11 | 1.408 (7) |
O2—C13 | 1.238 (5) | C4—C5 | 1.426 (8) |
O3—C18 | 1.246 (5) | C5—C6 | 1.331 (10) |
O3—Eu1iii | 2.398 (3) | C5—H5 | 0.9300 |
O4—C18 | 1.250 (6) | C6—C7 | 1.437 (8) |
O4—Eu1iv | 2.344 (3) | C6—H6 | 0.9300 |
O5—N5 | 1.260 (5) | C7—C8 | 1.392 (8) |
O6—N5 | 1.270 (5) | C7—C12 | 1.411 (6) |
O7—N5 | 1.223 (6) | C8—C9 | 1.354 (9) |
O1W—H1W1 | 0.96 | C8—H8 | 0.9300 |
O1W—H1W2 | 0.96 | C9—C10 | 1.386 (7) |
O2W—H2W1 | 0.97 | C9—H9 | 0.9300 |
O2W—H2W2 | 0.867 | C10—H10 | 0.9300 |
O2W'—H2W' | 0.97 | C11—C12 | 1.437 (8) |
O2W'—H2W" | 0.87 | C13—C14 | 1.501 (6) |
N1—C1 | 1.332 (6) | C14—C15 | 1.406 (6) |
N1—C11 | 1.360 (6) | C15—C18 | 1.514 (6) |
N2—C10 | 1.327 (6) | C16—C17 | 1.376 (6) |
N2—C12 | 1.372 (6) | C16—H16 | 0.9300 |
N3—C14 | 1.334 (5) | C17—H17 | 0.9300 |
O1—Eu1—O4i | 101.81 (13) | O7—N5—O6 | 121.2 (4) |
O1—Eu1—O3ii | 139.30 (11) | O5—N5—O6 | 116.6 (4) |
O4i—Eu1—O3ii | 86.81 (12) | N1—C1—C2 | 124.1 (5) |
O1—Eu1—O5 | 79.64 (12) | N1—C1—H1 | 117.9 |
O4i—Eu1—O5 | 141.25 (13) | C2—C1—H1 | 117.9 |
O3ii—Eu1—O5 | 117.52 (11) | C3—C2—C1 | 118.6 (6) |
O1—Eu1—O1W | 74.50 (12) | C3—C2—H2 | 120.7 |
O4i—Eu1—O1W | 69.71 (14) | C1—C2—H2 | 120.7 |
O3ii—Eu1—O1W | 71.50 (12) | C2—C3—C4 | 120.6 (5) |
O5—Eu1—O1W | 143.97 (13) | C2—C3—H3 | 119.7 |
O1—Eu1—O6 | 119.06 (11) | C4—C3—H3 | 119.7 |
O4i—Eu1—O6 | 138.55 (13) | C3—C4—C11 | 116.7 (5) |
O3ii—Eu1—O6 | 67.28 (11) | C3—C4—C5 | 123.5 (5) |
O5—Eu1—O6 | 50.27 (11) | C11—C4—C5 | 119.8 (6) |
O1W—Eu1—O6 | 125.49 (13) | C6—C5—C4 | 121.0 (5) |
O1—Eu1—N2 | 76.32 (12) | C6—C5—H5 | 119.5 |
O4i—Eu1—N2 | 71.62 (12) | C4—C5—H5 | 119.5 |
O3ii—Eu1—N2 | 142.69 (12) | C5—C6—C7 | 121.8 (5) |
O5—Eu1—N2 | 71.21 (12) | C5—C6—H6 | 119.1 |
O1W—Eu1—N2 | 124.56 (14) | C7—C6—H6 | 119.1 |
O6—Eu1—N2 | 109.83 (12) | C8—C7—C12 | 118.5 (5) |
O1—Eu1—N1 | 139.69 (12) | C8—C7—C6 | 123.0 (5) |
O4i—Eu1—N1 | 73.01 (14) | C12—C7—C6 | 118.4 (6) |
O3ii—Eu1—N1 | 80.96 (12) | C9—C8—C7 | 119.1 (5) |
O5—Eu1—N1 | 81.23 (13) | C9—C8—H8 | 120.5 |
O1W—Eu1—N1 | 134.25 (13) | C7—C8—H8 | 120.5 |
O6—Eu1—N1 | 71.42 (12) | C8—C9—C10 | 119.9 (5) |
N2—Eu1—N1 | 63.99 (13) | C8—C9—H9 | 120.1 |
O1—Eu1—N3 | 64.48 (11) | C10—C9—H9 | 120.1 |
O4i—Eu1—N3 | 139.47 (14) | N2—C10—C9 | 123.6 (5) |
O3ii—Eu1—N3 | 83.08 (11) | N2—C10—H10 | 118.2 |
O5—Eu1—N3 | 76.57 (12) | C9—C10—H10 | 118.2 |
O1W—Eu1—N3 | 69.85 (13) | N1—C11—C4 | 123.0 (5) |
O6—Eu1—N3 | 71.20 (11) | N1—C11—C12 | 118.1 (4) |
N2—Eu1—N3 | 132.77 (12) | C4—C11—C12 | 118.9 (5) |
N1—Eu1—N3 | 142.57 (12) | N2—C12—C7 | 121.6 (5) |
C13—O1—Eu1 | 128.0 (3) | N2—C12—C11 | 118.4 (4) |
C18—O3—Eu1iii | 138.4 (3) | C7—C12—C11 | 120.0 (5) |
C18—O4—Eu1iv | 165.8 (4) | O2—C13—O1 | 126.1 (4) |
N5—O5—Eu1 | 97.7 (3) | O2—C13—C14 | 118.7 (4) |
N5—O6—Eu1 | 95.4 (3) | O1—C13—C14 | 115.1 (4) |
Eu1—O1W—H1W1 | 109.6 | N3—C14—C15 | 120.0 (4) |
Eu1—O1W—H1W2 | 109.5 | N3—C14—C13 | 116.2 (4) |
H1W1—O1W—H1W2 | 109.3 | C15—C14—C13 | 123.8 (4) |
H2W1—O2W—H2W2 | 96.8 | N4—C15—C14 | 121.5 (4) |
H2W'—O2W'—H2W" | 108.3 | N4—C15—C18 | 114.5 (4) |
C1—N1—C11 | 116.9 (4) | C14—C15—C18 | 123.9 (4) |
C1—N1—Eu1 | 123.7 (3) | N4—C16—C17 | 122.2 (4) |
C11—N1—Eu1 | 118.7 (3) | N4—C16—H16 | 118.9 |
C10—N2—C12 | 117.3 (4) | C17—C16—H16 | 118.9 |
C10—N2—Eu1 | 123.4 (3) | N3—C17—C16 | 121.1 (4) |
C12—N2—Eu1 | 118.3 (3) | N3—C17—H17 | 119.5 |
C14—N3—C17 | 118.1 (4) | C16—C17—H17 | 119.5 |
C14—N3—Eu1 | 114.7 (3) | O3—C18—O4 | 125.7 (4) |
C17—N3—Eu1 | 126.1 (3) | O3—C18—C15 | 116.0 (4) |
C16—N4—C15 | 117.0 (4) | O4—C18—C15 | 118.1 (4) |
O7—N5—O5 | 122.1 (4) |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) −x+1, y−1/2, −z+3/2; (iii) −x+1, y+1/2, −z+3/2; (iv) x, −y+3/2, z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Eu(C6H2O4)(NO3)(C12H8N2)(H2O)]·H2O |
Mr | 596.30 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 298 |
a, b, c (Å) | 12.3427 (3), 10.4806 (3), 15.7966 (4) |
β (°) | 101.947 (1) |
V (Å3) | 1999.17 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 3.20 |
Crystal size (mm) | 0.28 × 0.18 × 0.17 |
Data collection | |
Diffractometer | Bruker SMART APEX area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2002) |
Tmin, Tmax | 0.468, 0.612 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11996, 4497, 3676 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.095, 1.04 |
No. of reflections | 4497 |
No. of parameters | 301 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.65, −0.82 |
Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XP (Bruker, 2002), SHELXL97.
Eu1—O1 | 2.331 (3) | Eu1—O6 | 2.555 (3) |
Eu1—O4i | 2.344 (3) | Eu1—N2 | 2.570 (4) |
Eu1—O3ii | 2.398 (3) | Eu1—N1 | 2.582 (4) |
Eu1—O5 | 2.513 (4) | Eu1—N3 | 2.597 (4) |
Eu1—O1W | 2.530 (4) | ||
O1—Eu1—O4i | 101.81 (13) | O5—Eu1—N2 | 71.21 (12) |
O1—Eu1—O3ii | 139.30 (11) | O1W—Eu1—N2 | 124.56 (14) |
O4i—Eu1—O3ii | 86.81 (12) | O6—Eu1—N2 | 109.83 (12) |
O1—Eu1—O5 | 79.64 (12) | O1—Eu1—N1 | 139.69 (12) |
O4i—Eu1—O5 | 141.25 (13) | O4i—Eu1—N1 | 73.01 (14) |
O3ii—Eu1—O5 | 117.52 (11) | O3ii—Eu1—N1 | 80.96 (12) |
O1—Eu1—O1W | 74.50 (12) | O5—Eu1—N1 | 81.23 (13) |
O4i—Eu1—O1W | 69.71 (14) | O1W—Eu1—N1 | 134.25 (13) |
O3ii—Eu1—O1W | 71.50 (12) | O6—Eu1—N1 | 71.42 (12) |
O5—Eu1—O1W | 143.97 (13) | N2—Eu1—N1 | 63.99 (13) |
O1—Eu1—O6 | 119.06 (11) | O1—Eu1—N3 | 64.48 (11) |
O4i—Eu1—O6 | 138.55 (13) | O4i—Eu1—N3 | 139.47 (14) |
O3ii—Eu1—O6 | 67.28 (11) | O3ii—Eu1—N3 | 83.08 (11) |
O5—Eu1—O6 | 50.27 (11) | O5—Eu1—N3 | 76.57 (12) |
O1W—Eu1—O6 | 125.49 (13) | O1W—Eu1—N3 | 69.85 (13) |
O1—Eu1—N2 | 76.32 (12) | O6—Eu1—N3 | 71.20 (11) |
O4i—Eu1—N2 | 71.62 (12) | N2—Eu1—N3 | 132.77 (12) |
O3ii—Eu1—N2 | 142.69 (12) | N1—Eu1—N3 | 142.57 (12) |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) −x+1, y−1/2, −z+3/2. |
Subscribe to Acta Crystallographica Section C: Structural Chemistry
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- Purchase subscription
- Reduced-price subscriptions
- If you have already subscribed, you may need to register
In recent years, more and more attention has been focused on coordination polymers with multifunctional ligands, as the presence of different functional groups allows incorporation of interesting properties into the resulting coordination networks (Ayyappan, et al., 2001). Among the various organic ligands, 2,3-pyrazinedicarboxylic acid is a commonly used multifunctional ligand. Its complexes with d-block transition metals have been well studied; compounds that have been structurally documented include polymeric [Cu(pzdc)·HCl]x, [Cu(pzdc)(H2O)2]x.2xH2O, [Fe(pzdc)(H2O)2]x.2xH2O and [Mn(pzdc)(H2O)2]x.2xH2O (O'Connor et al., 1982; Mao et al., 1996a; Gao et al., 1999; Mao et al., 1996b). However, the lanthanide complexes of this ligand are almost structurally unexplored. In light of the fact that lanthanide and d-block transition metal ions differ in their coordination number, pzdc may coordinate with them in a different manner, so we selected the europium–pzdc–phen system in order to extend this research. In the title compound, [(pzdc)(NO3)(phen)(H2O)Eu]·H2O, (I), the europium(III) ion is linked to four different ligands.
In (I), each europium(III) ion coordinates to three O atoms from three carboxylate groups of three pzdc anions, with a typical Eu—O(carboxylate) distance range [2.331 (3)–2.398 (3) Å; Li et al., 2002), one water molecule, with a longer Eu—O distance [2.530 (4) Å], one heterocycle N atom, with an Eu—N distance of 2.597 (4) Å, and two N atoms of phen in a chelating fashion, with Eu—N distances of 2.570 (4) and 2.582 (4) Å, resulting in a distorted monocap square- antiprismatic coordination polyhedron (Fig. 1). The square plane formed by atoms O5, O6, N1 and N2, with a mean deviation of 0.2280 Å, is significantly distorted, but the mean deviation of the other square plane, containing atoms O1, N3, O3i and O4ii [symmetry codes: (i) −x + 1, y − 1/2, −z + 3/2; (ii) x, −y + 3/2, z − 1/2], is only 0.0849 Å, comparable with the deviations found in the Eu–phen analogue [Eu2(p-BDC)3(phen)2(H2O)2]n (p-BDC is 1,4-benzenedicarboxylate; Wang, et al., 2003). To complete the coordination environment of the europium(III) center, atom O1W is located on the cap. Obviously, the pzdc anion acts as a tetradentate ligand, bridging three europium(III) ions, and adopts only one bridging mode. Four pzdc anions bridge four europium(III) ions into a parallelogram unit with approximate dimensions of 10.293 and 13.176 Å, the four vertices of which are occupied by the four pzdc anions. Moreover, each parallelogram unit links six other adjacent parallelogram units, forming a two-dimensional network (Fig. 2). The pzdc anion displays three types of bridging; bridging by the anion is also found in [Eu2(pzdc)3(H2O)]x.2xH2O, which adopts a microporous three-dimensinal network structure (Zheng, et al., 2002). Limited studies of this anion suggest that the different binding modes arise from the manner in which the carboxy group is oriented with respect to the aromatic ring. However, functioning as a chelate, the phen ligand prevents the oligomeric compounds from adopting high dimensionality (Plater et al., 1999). This is noted in the present compound, which has a two-dimensional structure.