metal-organic compounds
Triimidazolium tris(pyridine-2,6-dicarboxylato)dysprosate(III) trihydrate
aSchool of Chemistry & Environmental Resources, Linyi Normal University, Linyi 276005, People's Republic of China
*Correspondence e-mail: menglingzong@lytu.edu.cn
The structure of the title compound, (C3N2H5)3[Dy(C7H3NO4)3]·3H2O, contains a mononuclear DyIII complex with the rare earth metal cation in a distorted tricapped trigonal–prismatic environment. The DyIII ion is in each case O,N,O′-chelated by three tridentate pyridine-2,6-dicarboxylate anions. Three protonated imidazole molecules act as counter-cations and three lattice water molecules are also present. Numerous N—H⋯O and O—H⋯O hydrogen bonding interactions, some of which are bifurcated, help to stabilize the packing of the structure.
Related literature
For background to pyridine-2,6-dicarboxylic acid (H2pda) and structures of metal complexes with (pda2−) ligands, see: Ghosh & Bharadwaj (2005); Huang et al. (2008); Kjell et al. (1993); Song et al. (2005); Wu et al. (2008); Yue et al. (2005); Zhao et al. (2005, 2007).
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2008); cell SAINT (Bruker, 2008); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.
Supporting information
10.1107/S1600536810036421/wm2398sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536810036421/wm2398Isup2.hkl
The title compound was synthesized under solvothermal conditions. A mixture of pyridine-2,6-dicarboxylic acid (0.0334 g, 0.2 mmol), Dy(NO3)3.6H2O (0.0245 g, 0.06 mmol), imidazole (0.0340 g, 0.5 mmol) and H2O / C2H5OH (v / v = 1: 1, 2.5 ml) was sealed in a 6 ml glass tube and heated to 393 K for 72 h. After cooling to room temperature, colorless block-like crystals were obtained.
H atoms bound to C and N atoms were placed in calculated positions with C—H = 0.93 and N—H = 0.86 Å and refined in riding mode, with Uiso(H) = 1.2 Ueq(N, C). H atoms attached to water molecules were located in Fourier maps and refined with distance constraints of 0.85 Å and Uiso(H) = 1.5 Ueq(O).
Data collection: APEX2 (Bruker, 2008); cell
SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).Fig. 1. The asymmetric unit of the title compound, showing displacement ellipsoids at the 50% probability level. |
(C3H5N2)3[Dy(C7H3NO4)3]·3H2O | Z = 2 |
Mr = 919.13 | F(000) = 918 |
Triclinic, P1 | Dx = 1.782 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.939 (2) Å | Cell parameters from 125 reflections |
b = 12.099 (2) Å | θ = 7.5–15° |
c = 14.070 (3) Å | µ = 2.27 mm−1 |
α = 88.57 (3)° | T = 296 K |
β = 85.64 (3)° | Block, colourless |
γ = 67.28 (3)° | 0.35 × 0.25 × 0.25 mm |
V = 1712.7 (6) Å3 |
Bruker APEXII CCD diffractometer | 7447 independent reflections |
Radiation source: fine-focus sealed tube | 7223 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
ϕ and ω scans | θmax = 27.0°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −13→13 |
Tmin = 0.504, Tmax = 0.601 | k = −13→15 |
27464 measured reflections | l = −17→17 |
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)] = 0.022 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.060 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0314P)2 + 1.7104P] where P = (Fo2 + 2Fc2)/3 |
7447 reflections | (Δ/σ)max = 0.001 |
505 parameters | Δρmax = 0.69 e Å−3 |
3 restraints | Δρmin = −0.77 e Å−3 |
(C3H5N2)3[Dy(C7H3NO4)3]·3H2O | γ = 67.28 (3)° |
Mr = 919.13 | V = 1712.7 (6) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.939 (2) Å | Mo Kα radiation |
b = 12.099 (2) Å | µ = 2.27 mm−1 |
c = 14.070 (3) Å | T = 296 K |
α = 88.57 (3)° | 0.35 × 0.25 × 0.25 mm |
β = 85.64 (3)° |
Bruker APEXII CCD diffractometer | 7447 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 7223 reflections with I > 2σ(I) |
Tmin = 0.504, Tmax = 0.601 | Rint = 0.022 |
27464 measured reflections |
R[F2 > 2σ(F2)] = 0.022 | 3 restraints |
wR(F2) = 0.060 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.10 | Δρmax = 0.69 e Å−3 |
7447 reflections | Δρmin = −0.77 e Å−3 |
505 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 | ||
Dy2 | 0.492045 (10) | 0.266222 (9) | 0.252168 (7) | 0.02219 (4) | |
N1 | 0.38988 (19) | 0.43970 (17) | 0.36385 (14) | 0.0243 (4) | |
O11 | 0.31544 (18) | 0.41655 (17) | 0.17113 (13) | 0.0338 (4) | |
N2 | 0.5350 (2) | 0.05867 (18) | 0.30655 (14) | 0.0257 (4) | |
O3 | 0.29744 (19) | 0.27164 (17) | 0.34879 (14) | 0.0345 (4) | |
O9 | 0.71488 (18) | 0.14570 (17) | 0.18726 (13) | 0.0344 (4) | |
O7 | 0.40575 (19) | 0.15338 (17) | 0.15780 (13) | 0.0348 (4) | |
O1 | 0.60328 (17) | 0.40305 (16) | 0.25167 (13) | 0.0304 (4) | |
O5 | 0.6077 (2) | 0.20866 (16) | 0.39291 (13) | 0.0350 (4) | |
N3 | 0.5446 (2) | 0.29826 (18) | 0.07972 (14) | 0.0265 (4) | |
O10 | 0.8795 (2) | 0.1004 (2) | 0.07273 (15) | 0.0456 (5) | |
C6 | 0.5682 (3) | 0.4965 (2) | 0.30392 (18) | 0.0288 (5) | |
C14 | 0.4159 (3) | 0.0481 (2) | 0.17445 (18) | 0.0298 (5) | |
C13 | 0.6477 (3) | 0.1058 (2) | 0.42917 (18) | 0.0300 (5) | |
C5 | 0.2800 (2) | 0.4523 (2) | 0.41906 (17) | 0.0269 (5) | |
C1 | 0.4427 (2) | 0.5216 (2) | 0.36810 (17) | 0.0268 (5) | |
O8 | 0.3703 (2) | −0.01097 (19) | 0.12661 (15) | 0.0432 (5) | |
C15 | 0.6663 (2) | 0.2410 (2) | 0.03876 (18) | 0.0290 (5) | |
C8 | 0.6011 (2) | 0.0175 (2) | 0.38414 (17) | 0.0270 (5) | |
C21 | 0.3162 (3) | 0.4294 (3) | 0.0813 (2) | 0.0388 (6) | |
O6 | 0.7192 (2) | 0.07182 (19) | 0.49629 (16) | 0.0475 (5) | |
C11 | 0.5093 (3) | −0.1261 (2) | 0.2908 (2) | 0.0368 (6) | |
H11 | 0.4774 | −0.1736 | 0.2576 | 0.044* | |
O4 | 0.1420 (2) | 0.34799 (19) | 0.46686 (15) | 0.0419 (5) | |
C12 | 0.4892 (2) | −0.0110 (2) | 0.26079 (18) | 0.0286 (5) | |
C20 | 0.7622 (3) | 0.1555 (2) | 0.10429 (19) | 0.0313 (5) | |
C7 | 0.2347 (2) | 0.3501 (2) | 0.41110 (18) | 0.0282 (5) | |
O2 | 0.6264 (2) | 0.5655 (2) | 0.30446 (17) | 0.0466 (5) | |
C2 | 0.3867 (3) | 0.6207 (2) | 0.4278 (2) | 0.0363 (6) | |
H2 | 0.4260 | 0.6762 | 0.4306 | 0.044* | |
C9 | 0.6241 (3) | −0.0961 (2) | 0.4192 (2) | 0.0349 (6) | |
H9 | 0.6695 | −0.1231 | 0.4739 | 0.042* | |
C4 | 0.2156 (3) | 0.5508 (2) | 0.4781 (2) | 0.0355 (6) | |
H4 | 0.1369 | 0.5601 | 0.5135 | 0.043* | |
C19 | 0.4500 (3) | 0.3706 (2) | 0.02714 (18) | 0.0305 (5) | |
C16 | 0.6994 (3) | 0.2573 (3) | −0.0559 (2) | 0.0388 (6) | |
H16 | 0.7858 | 0.2185 | −0.0824 | 0.047* | |
C17 | 0.6007 (3) | 0.3327 (3) | −0.1099 (2) | 0.0445 (7) | |
H17 | 0.6199 | 0.3450 | −0.1739 | 0.053* | |
C18 | 0.4737 (3) | 0.3896 (3) | −0.0690 (2) | 0.0413 (6) | |
H18 | 0.4057 | 0.4393 | −0.1047 | 0.050* | |
C10 | 0.5776 (3) | −0.1689 (2) | 0.3708 (2) | 0.0391 (6) | |
H10 | 0.5924 | −0.2460 | 0.3922 | 0.047* | |
O12 | 0.2182 (2) | 0.4833 (3) | 0.03738 (18) | 0.0843 (11) | |
C3 | 0.2725 (3) | 0.6355 (3) | 0.4827 (2) | 0.0418 (7) | |
H3 | 0.2332 | 0.7017 | 0.5229 | 0.050* | |
C30 | 0.2356 (3) | 0.1317 (3) | 0.9875 (2) | 0.0349 (6) | |
H30 | 0.2716 | 0.0773 | 1.0356 | 0.042* | |
C29 | 0.3007 (4) | 0.1858 (4) | 0.9312 (3) | 0.0565 (9) | |
H29 | 0.3893 | 0.1754 | 0.9332 | 0.068* | |
N9 | 0.2143 (4) | 0.2573 (4) | 0.8719 (3) | 0.0879 (12) | |
H9A | 0.2305 | 0.3022 | 0.8285 | 0.105* | |
C28 | 0.0964 (3) | 0.2459 (3) | 0.8928 (2) | 0.0409 (6) | |
H28 | 0.0184 | 0.2856 | 0.8628 | 0.049* | |
N8 | 0.1118 (4) | 0.1690 (4) | 0.9629 (3) | 0.0694 (9) | |
H8A | 0.044 (4) | 0.144 (4) | 0.990 (3) | 0.083* | |
N7 | 0.0067 (3) | 0.9748 (3) | 0.22123 (19) | 0.0460 (6) | |
H7A | −0.032 (3) | 1.016 (3) | 0.172 (2) | 0.055* | |
C25 | −0.0575 (3) | 0.9456 (4) | 0.2928 (3) | 0.0577 (9) | |
H25 | −0.1468 | 0.9570 | 0.2959 | 0.069* | |
C26 | 0.1345 (3) | 0.9451 (3) | 0.2428 (2) | 0.0461 (7) | |
H26 | 0.2019 | 0.9561 | 0.2043 | 0.055* | |
N6 | 0.0242 (3) | 0.8977 (3) | 0.3600 (2) | 0.0556 (7) | |
H6 | 0.0043 | 0.8714 | 0.4138 | 0.067* | |
C27 | 0.1448 (4) | 0.8969 (3) | 0.3299 (3) | 0.0520 (8) | |
H27 | 0.2209 | 0.8682 | 0.3635 | 0.062* | |
C23 | 0.9146 (3) | 0.3939 (4) | 0.1412 (2) | 0.0529 (8) | |
H23 | 0.8654 | 0.4415 | 0.0937 | 0.063* | |
C24 | 0.8704 (3) | 0.3407 (3) | 0.2103 (2) | 0.0363 (6) | |
H24 | 0.7834 | 0.3455 | 0.2205 | 0.044* | |
C22 | 1.0765 (3) | 0.2936 (3) | 0.2290 (3) | 0.0520 (8) | |
H22 | 1.1600 | 0.2603 | 0.2529 | 0.062* | |
N5 | 1.0434 (3) | 0.3669 (4) | 0.1519 (3) | 0.0713 (10) | |
H5 | 1.0957 | 0.3912 | 0.1167 | 0.086* | |
O13 | 0.0930 (3) | 0.6349 (2) | 0.22816 (19) | 0.0625 (7) | |
H2W | 0.0469 | 0.6143 | 0.2710 | 0.094* | |
H1W | 0.1609 | 0.5740 | 0.2092 | 0.094* | |
O14 | 0.0736 (2) | 0.1513 (2) | 0.46679 (16) | 0.0482 (5) | |
H3W | 0.0936 | 0.2127 | 0.4652 | 0.072* | |
H4W | 0.1461 | 0.0904 | 0.4598 | 0.072* | |
O15 | 0.1116 (3) | 0.4098 (3) | 0.6635 (2) | 0.0794 (9) | |
H5W | 0.1782 | 0.4267 | 0.6729 | 0.119* | |
H6W | 0.1159 | 0.3982 | 0.6038 | 0.119* | |
N4 | 0.9700 (4) | 0.2789 (3) | 0.2631 (3) | 0.0758 (10) | |
H4A | 0.966 (5) | 0.231 (4) | 0.316 (3) | 0.091* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Dy2 | 0.02178 (6) | 0.02328 (6) | 0.02335 (7) | −0.01066 (4) | −0.00168 (4) | −0.00032 (4) |
N1 | 0.0258 (10) | 0.0247 (9) | 0.0244 (9) | −0.0116 (8) | −0.0031 (8) | 0.0020 (7) |
O11 | 0.0279 (9) | 0.0380 (10) | 0.0295 (9) | −0.0059 (7) | −0.0021 (7) | 0.0010 (7) |
N2 | 0.0259 (10) | 0.0265 (9) | 0.0266 (10) | −0.0127 (8) | −0.0001 (8) | −0.0016 (8) |
O3 | 0.0353 (10) | 0.0355 (9) | 0.0383 (10) | −0.0213 (8) | 0.0089 (8) | −0.0095 (8) |
O9 | 0.0272 (9) | 0.0370 (10) | 0.0327 (10) | −0.0062 (7) | 0.0007 (7) | 0.0046 (8) |
O7 | 0.0442 (11) | 0.0354 (9) | 0.0324 (9) | −0.0221 (8) | −0.0110 (8) | 0.0018 (7) |
O1 | 0.0286 (9) | 0.0306 (9) | 0.0349 (9) | −0.0156 (7) | 0.0033 (7) | −0.0038 (7) |
O5 | 0.0469 (11) | 0.0284 (9) | 0.0335 (10) | −0.0166 (8) | −0.0143 (8) | 0.0015 (7) |
N3 | 0.0265 (10) | 0.0279 (10) | 0.0261 (10) | −0.0115 (8) | −0.0020 (8) | −0.0001 (8) |
O10 | 0.0290 (10) | 0.0535 (13) | 0.0418 (11) | −0.0038 (9) | 0.0053 (8) | 0.0010 (9) |
C6 | 0.0294 (12) | 0.0286 (11) | 0.0321 (13) | −0.0151 (10) | −0.0045 (10) | 0.0031 (9) |
C14 | 0.0282 (12) | 0.0353 (13) | 0.0298 (12) | −0.0168 (10) | 0.0000 (10) | −0.0045 (10) |
C13 | 0.0334 (13) | 0.0297 (12) | 0.0282 (12) | −0.0133 (10) | −0.0045 (10) | −0.0008 (9) |
C5 | 0.0279 (12) | 0.0271 (11) | 0.0256 (11) | −0.0108 (9) | −0.0008 (9) | 0.0015 (9) |
C1 | 0.0293 (12) | 0.0262 (11) | 0.0277 (12) | −0.0133 (9) | −0.0045 (9) | 0.0019 (9) |
O8 | 0.0535 (12) | 0.0449 (11) | 0.0446 (11) | −0.0312 (10) | −0.0158 (10) | −0.0016 (9) |
C15 | 0.0276 (12) | 0.0324 (12) | 0.0278 (12) | −0.0128 (10) | −0.0004 (9) | −0.0022 (9) |
C8 | 0.0271 (12) | 0.0279 (11) | 0.0264 (12) | −0.0111 (9) | −0.0002 (9) | −0.0005 (9) |
C21 | 0.0306 (13) | 0.0470 (16) | 0.0327 (14) | −0.0074 (12) | −0.0071 (11) | 0.0016 (12) |
O6 | 0.0633 (14) | 0.0397 (11) | 0.0435 (12) | −0.0200 (10) | −0.0295 (11) | 0.0068 (9) |
C11 | 0.0399 (15) | 0.0316 (13) | 0.0454 (15) | −0.0207 (11) | −0.0034 (12) | −0.0024 (11) |
O4 | 0.0411 (11) | 0.0447 (11) | 0.0454 (12) | −0.0255 (9) | 0.0149 (9) | −0.0085 (9) |
C12 | 0.0286 (12) | 0.0300 (12) | 0.0312 (12) | −0.0158 (10) | −0.0008 (10) | −0.0025 (10) |
C20 | 0.0256 (12) | 0.0313 (12) | 0.0350 (14) | −0.0090 (10) | −0.0001 (10) | −0.0028 (10) |
C7 | 0.0269 (12) | 0.0307 (12) | 0.0290 (12) | −0.0136 (10) | −0.0002 (9) | 0.0015 (9) |
O2 | 0.0484 (12) | 0.0445 (11) | 0.0597 (14) | −0.0336 (10) | 0.0092 (10) | −0.0107 (10) |
C2 | 0.0434 (15) | 0.0301 (12) | 0.0396 (15) | −0.0191 (11) | 0.0000 (12) | −0.0049 (11) |
C9 | 0.0339 (13) | 0.0321 (13) | 0.0399 (14) | −0.0138 (11) | −0.0055 (11) | 0.0069 (11) |
C4 | 0.0378 (14) | 0.0338 (13) | 0.0348 (14) | −0.0154 (11) | 0.0080 (11) | −0.0058 (11) |
C19 | 0.0314 (13) | 0.0335 (12) | 0.0260 (12) | −0.0118 (10) | −0.0035 (10) | 0.0020 (10) |
C16 | 0.0351 (14) | 0.0504 (16) | 0.0304 (13) | −0.0170 (12) | 0.0055 (11) | −0.0030 (12) |
C17 | 0.0501 (18) | 0.0593 (19) | 0.0244 (13) | −0.0221 (15) | 0.0007 (12) | 0.0048 (12) |
C18 | 0.0438 (16) | 0.0486 (16) | 0.0296 (14) | −0.0155 (13) | −0.0068 (12) | 0.0077 (12) |
C10 | 0.0413 (15) | 0.0291 (13) | 0.0514 (17) | −0.0186 (11) | −0.0044 (13) | 0.0082 (12) |
O12 | 0.0377 (13) | 0.131 (3) | 0.0416 (14) | 0.0155 (15) | −0.0127 (11) | 0.0054 (15) |
C3 | 0.0505 (17) | 0.0311 (13) | 0.0430 (16) | −0.0161 (12) | 0.0083 (13) | −0.0122 (12) |
C30 | 0.0391 (14) | 0.0399 (14) | 0.0301 (13) | −0.0187 (12) | −0.0093 (11) | −0.0013 (11) |
C29 | 0.0447 (18) | 0.069 (2) | 0.057 (2) | −0.0227 (17) | −0.0042 (16) | 0.0032 (17) |
N9 | 0.097 (3) | 0.088 (3) | 0.072 (2) | −0.031 (2) | 0.000 (2) | 0.019 (2) |
C28 | 0.0372 (15) | 0.0498 (16) | 0.0341 (14) | −0.0145 (13) | −0.0077 (12) | 0.0051 (12) |
N8 | 0.069 (2) | 0.079 (2) | 0.068 (2) | −0.0367 (19) | −0.0072 (17) | −0.0045 (18) |
N7 | 0.0380 (13) | 0.0514 (15) | 0.0421 (14) | −0.0099 (11) | −0.0052 (11) | 0.0048 (12) |
C25 | 0.0390 (17) | 0.072 (2) | 0.056 (2) | −0.0163 (16) | 0.0029 (15) | 0.0062 (18) |
C26 | 0.0381 (15) | 0.0491 (17) | 0.0527 (18) | −0.0185 (13) | −0.0025 (13) | −0.0035 (14) |
N6 | 0.0671 (19) | 0.0552 (17) | 0.0408 (15) | −0.0205 (15) | 0.0000 (13) | 0.0057 (12) |
C27 | 0.0521 (19) | 0.0497 (18) | 0.056 (2) | −0.0181 (15) | −0.0202 (16) | −0.0003 (15) |
C23 | 0.0414 (17) | 0.073 (2) | 0.0451 (18) | −0.0223 (16) | −0.0081 (14) | 0.0018 (16) |
C24 | 0.0236 (12) | 0.0502 (16) | 0.0407 (15) | −0.0206 (11) | 0.0011 (10) | −0.0094 (12) |
C22 | 0.0242 (14) | 0.061 (2) | 0.064 (2) | −0.0068 (13) | −0.0130 (14) | −0.0145 (17) |
N5 | 0.0547 (19) | 0.094 (3) | 0.079 (2) | −0.0465 (19) | 0.0196 (17) | −0.026 (2) |
O13 | 0.0524 (14) | 0.0571 (15) | 0.0597 (15) | −0.0014 (12) | −0.0012 (12) | −0.0022 (12) |
O14 | 0.0477 (12) | 0.0453 (12) | 0.0567 (14) | −0.0235 (10) | −0.0070 (10) | 0.0091 (10) |
O15 | 0.090 (2) | 0.102 (2) | 0.0473 (15) | −0.0424 (19) | 0.0164 (14) | −0.0014 (15) |
N4 | 0.093 (3) | 0.058 (2) | 0.071 (2) | −0.023 (2) | −0.009 (2) | 0.0016 (17) |
Dy2—O5 | 2.3745 (19) | C4—H4 | 0.9300 |
Dy2—O1 | 2.4032 (17) | C19—C18 | 1.388 (4) |
Dy2—O7 | 2.4072 (18) | C16—C17 | 1.381 (4) |
Dy2—O3 | 2.4167 (19) | C16—H16 | 0.9300 |
Dy2—O11 | 2.420 (2) | C17—C18 | 1.376 (4) |
Dy2—O9 | 2.426 (2) | C17—H17 | 0.9300 |
Dy2—N2 | 2.482 (2) | C18—H18 | 0.9300 |
Dy2—N1 | 2.492 (2) | C10—H10 | 0.9300 |
Dy2—N3 | 2.506 (2) | C3—H3 | 0.9300 |
N1—C1 | 1.331 (3) | C30—N8 | 1.322 (4) |
N1—C5 | 1.339 (3) | C30—C29 | 1.345 (5) |
O11—C21 | 1.270 (3) | C30—H30 | 0.9300 |
N2—C8 | 1.333 (3) | C29—N9 | 1.339 (5) |
N2—C12 | 1.334 (3) | C29—H29 | 0.9300 |
O3—C7 | 1.260 (3) | N9—C28 | 1.359 (5) |
O9—C20 | 1.262 (3) | N9—H9A | 0.8600 |
O7—C14 | 1.253 (3) | C28—N8 | 1.313 (5) |
O1—C6 | 1.277 (3) | C28—H28 | 0.9300 |
O5—C13 | 1.258 (3) | N8—H8A | 0.960 (19) |
N3—C19 | 1.330 (3) | N7—C25 | 1.304 (4) |
N3—C15 | 1.333 (3) | N7—C26 | 1.359 (4) |
O10—C20 | 1.246 (3) | N7—H7A | 0.873 (18) |
C6—O2 | 1.230 (3) | C25—N6 | 1.315 (5) |
C6—C1 | 1.515 (4) | C25—H25 | 0.9300 |
C14—O8 | 1.250 (3) | C26—C27 | 1.338 (5) |
C14—C12 | 1.514 (4) | C26—H26 | 0.9300 |
C13—O6 | 1.232 (3) | N6—C27 | 1.351 (5) |
C13—C8 | 1.518 (3) | N6—H6 | 0.8600 |
C5—C4 | 1.385 (4) | C27—H27 | 0.9300 |
C5—C7 | 1.510 (3) | C23—C24 | 1.317 (5) |
C1—C2 | 1.387 (4) | C23—N5 | 1.337 (5) |
C15—C16 | 1.383 (4) | C23—H23 | 0.9300 |
C15—C20 | 1.511 (4) | C24—N4 | 1.328 (5) |
C8—C9 | 1.384 (3) | C24—H24 | 0.9300 |
C21—O12 | 1.223 (4) | C22—N4 | 1.301 (5) |
C21—C19 | 1.511 (4) | C22—N5 | 1.362 (5) |
C11—C10 | 1.375 (4) | C22—H22 | 0.9300 |
C11—C12 | 1.383 (4) | N5—H5 | 0.8600 |
C11—H11 | 0.9300 | O13—H2W | 0.8499 |
O4—C7 | 1.241 (3) | O13—H1W | 0.8500 |
C2—C3 | 1.369 (4) | O14—H3W | 0.8501 |
C2—H2 | 0.9300 | O14—H4W | 0.8500 |
C9—C10 | 1.388 (4) | O15—H5W | 0.8500 |
C9—H9 | 0.9300 | O15—H6W | 0.8501 |
C4—C3 | 1.395 (4) | N4—H4A | 0.937 (19) |
O5—Dy2—O1 | 78.70 (7) | O10—C20—O9 | 125.6 (3) |
O5—Dy2—O7 | 129.04 (6) | O10—C20—C15 | 118.3 (2) |
O1—Dy2—O7 | 146.45 (6) | O9—C20—C15 | 116.1 (2) |
O5—Dy2—O3 | 86.53 (7) | O4—C7—O3 | 125.3 (2) |
O1—Dy2—O3 | 128.79 (6) | O4—C7—C5 | 118.4 (2) |
O7—Dy2—O3 | 77.27 (7) | O3—C7—C5 | 116.3 (2) |
O5—Dy2—O11 | 147.58 (7) | C3—C2—C1 | 119.0 (2) |
O1—Dy2—O11 | 88.66 (7) | C3—C2—H2 | 120.5 |
O7—Dy2—O11 | 75.43 (7) | C1—C2—H2 | 120.5 |
O3—Dy2—O11 | 78.34 (7) | C8—C9—C10 | 118.3 (3) |
O5—Dy2—O9 | 78.53 (7) | C8—C9—H9 | 120.8 |
O1—Dy2—O9 | 77.03 (7) | C10—C9—H9 | 120.8 |
O7—Dy2—O9 | 89.53 (7) | C5—C4—C3 | 117.9 (3) |
O3—Dy2—O9 | 147.00 (7) | C5—C4—H4 | 121.1 |
O11—Dy2—O9 | 127.78 (6) | C3—C4—H4 | 121.1 |
O5—Dy2—N2 | 64.77 (7) | N3—C19—C18 | 122.3 (3) |
O1—Dy2—N2 | 137.08 (6) | N3—C19—C21 | 114.1 (2) |
O7—Dy2—N2 | 64.30 (7) | C18—C19—C21 | 123.6 (2) |
O3—Dy2—N2 | 72.61 (7) | C17—C16—C15 | 118.2 (3) |
O11—Dy2—N2 | 134.24 (7) | C17—C16—H16 | 120.9 |
O9—Dy2—N2 | 74.41 (7) | C15—C16—H16 | 120.9 |
O5—Dy2—N1 | 74.09 (7) | C18—C17—C16 | 119.8 (3) |
O1—Dy2—N1 | 64.41 (6) | C18—C17—H17 | 120.1 |
O7—Dy2—N1 | 134.39 (7) | C16—C17—H17 | 120.1 |
O3—Dy2—N1 | 64.39 (7) | C17—C18—C19 | 118.2 (3) |
O11—Dy2—N1 | 73.51 (7) | C17—C18—H18 | 120.9 |
O9—Dy2—N1 | 136.03 (7) | C19—C18—H18 | 120.9 |
N2—Dy2—N1 | 121.12 (7) | C11—C10—C9 | 119.5 (2) |
O5—Dy2—N3 | 137.66 (7) | C11—C10—H10 | 120.2 |
O1—Dy2—N3 | 74.77 (7) | C9—C10—H10 | 120.2 |
O7—Dy2—N3 | 71.72 (7) | C2—C3—C4 | 119.6 (3) |
O3—Dy2—N3 | 135.76 (7) | C2—C3—H3 | 120.2 |
O11—Dy2—N3 | 63.97 (7) | C4—C3—H3 | 120.2 |
O9—Dy2—N3 | 63.82 (7) | N8—C30—C29 | 108.5 (3) |
N2—Dy2—N3 | 118.21 (7) | N8—C30—H30 | 125.7 |
N1—Dy2—N3 | 120.61 (7) | C29—C30—H30 | 125.7 |
C1—N1—C5 | 119.4 (2) | N9—C29—C30 | 107.2 (3) |
C1—N1—Dy2 | 120.34 (16) | N9—C29—H29 | 126.4 |
C5—N1—Dy2 | 120.26 (15) | C30—C29—H29 | 126.4 |
C21—O11—Dy2 | 124.08 (17) | C29—N9—C28 | 107.4 (3) |
C8—N2—C12 | 119.5 (2) | C29—N9—H9A | 126.3 |
C8—N2—Dy2 | 119.67 (16) | C28—N9—H9A | 126.3 |
C12—N2—Dy2 | 120.78 (16) | N8—C28—N9 | 108.0 (3) |
C7—O3—Dy2 | 124.83 (16) | N8—C28—H28 | 126.0 |
C20—O9—Dy2 | 125.16 (16) | N9—C28—H28 | 126.0 |
C14—O7—Dy2 | 125.14 (16) | C28—N8—C30 | 108.8 (3) |
C6—O1—Dy2 | 125.57 (16) | C28—N8—H8A | 124 (3) |
C13—O5—Dy2 | 125.83 (16) | C30—N8—H8A | 127 (3) |
C19—N3—C15 | 119.0 (2) | C25—N7—C26 | 108.6 (3) |
C19—N3—Dy2 | 120.24 (17) | C25—N7—H7A | 123 (3) |
C15—N3—Dy2 | 120.71 (16) | C26—N7—H7A | 128 (3) |
O2—C6—O1 | 125.4 (2) | N7—C25—N6 | 109.0 (3) |
O2—C6—C1 | 119.6 (2) | N7—C25—H25 | 125.5 |
O1—C6—C1 | 115.0 (2) | N6—C25—H25 | 125.5 |
O8—C14—O7 | 125.7 (2) | C27—C26—N7 | 106.8 (3) |
O8—C14—C12 | 118.0 (2) | C27—C26—H26 | 126.6 |
O7—C14—C12 | 116.3 (2) | N7—C26—H26 | 126.6 |
O6—C13—O5 | 126.3 (2) | C25—N6—C27 | 108.3 (3) |
O6—C13—C8 | 118.5 (2) | C25—N6—H6 | 125.8 |
O5—C13—C8 | 115.2 (2) | C27—N6—H6 | 125.8 |
N1—C5—C4 | 122.2 (2) | C26—C27—N6 | 107.3 (3) |
N1—C5—C7 | 114.0 (2) | C26—C27—H27 | 126.4 |
C4—C5—C7 | 123.8 (2) | N6—C27—H27 | 126.4 |
N1—C1—C2 | 121.8 (2) | C24—C23—N5 | 107.4 (3) |
N1—C1—C6 | 114.6 (2) | C24—C23—H23 | 126.3 |
C2—C1—C6 | 123.5 (2) | N5—C23—H23 | 126.3 |
N3—C15—C16 | 122.4 (2) | C23—C24—N4 | 108.9 (3) |
N3—C15—C20 | 113.9 (2) | C23—C24—H24 | 125.5 |
C16—C15—C20 | 123.7 (2) | N4—C24—H24 | 125.5 |
N2—C8—C9 | 122.0 (2) | N4—C22—N5 | 107.5 (3) |
N2—C8—C13 | 114.1 (2) | N4—C22—H22 | 126.3 |
C9—C8—C13 | 123.9 (2) | N5—C22—H22 | 126.3 |
O12—C21—O11 | 125.0 (3) | C23—N5—C22 | 107.4 (3) |
O12—C21—C19 | 119.4 (3) | C23—N5—H5 | 126.3 |
O11—C21—C19 | 115.6 (2) | C22—N5—H5 | 126.3 |
C10—C11—C12 | 118.7 (2) | H2W—O13—H1W | 109.8 |
C10—C11—H11 | 120.6 | H3W—O14—H4W | 107.0 |
C12—C11—H11 | 120.6 | H5W—O15—H6W | 105.4 |
N2—C12—C11 | 121.9 (2) | C22—N4—C24 | 108.8 (3) |
N2—C12—C14 | 113.5 (2) | C22—N4—H4A | 125 (3) |
C11—C12—C14 | 124.6 (2) | C24—N4—H4A | 126 (3) |
O5—Dy2—N1—C1 | 85.81 (18) | N1—Dy2—N3—C15 | 126.34 (18) |
O1—Dy2—N1—C1 | 0.95 (16) | Dy2—O1—C6—O2 | 178.9 (2) |
O7—Dy2—N1—C1 | −144.58 (16) | Dy2—O1—C6—C1 | −2.1 (3) |
O3—Dy2—N1—C1 | 179.64 (19) | Dy2—O7—C14—O8 | 179.2 (2) |
O11—Dy2—N1—C1 | −95.64 (18) | Dy2—O7—C14—C12 | −0.3 (3) |
O9—Dy2—N1—C1 | 32.2 (2) | Dy2—O5—C13—O6 | 172.1 (2) |
N2—Dy2—N1—C1 | 132.20 (17) | Dy2—O5—C13—C8 | −8.0 (3) |
N3—Dy2—N1—C1 | −50.61 (19) | C1—N1—C5—C4 | 2.7 (4) |
O5—Dy2—N1—C5 | −95.26 (18) | Dy2—N1—C5—C4 | −176.21 (19) |
O1—Dy2—N1—C5 | 179.88 (19) | C1—N1—C5—C7 | −177.0 (2) |
O7—Dy2—N1—C5 | 34.4 (2) | Dy2—N1—C5—C7 | 4.1 (3) |
O3—Dy2—N1—C5 | −1.43 (16) | C5—N1—C1—C2 | −0.4 (4) |
O11—Dy2—N1—C5 | 83.29 (17) | Dy2—N1—C1—C2 | 178.49 (19) |
O9—Dy2—N1—C5 | −148.86 (16) | C5—N1—C1—C6 | 178.8 (2) |
N2—Dy2—N1—C5 | −48.87 (19) | Dy2—N1—C1—C6 | −2.2 (3) |
N3—Dy2—N1—C5 | 128.32 (17) | O2—C6—C1—N1 | −178.2 (2) |
O5—Dy2—O11—C21 | 153.0 (2) | O1—C6—C1—N1 | 2.7 (3) |
O1—Dy2—O11—C21 | 86.7 (2) | O2—C6—C1—C2 | 1.1 (4) |
O7—Dy2—O11—C21 | −63.5 (2) | O1—C6—C1—C2 | −178.0 (2) |
O3—Dy2—O11—C21 | −143.2 (2) | C19—N3—C15—C16 | 2.4 (4) |
O9—Dy2—O11—C21 | 14.3 (3) | Dy2—N3—C15—C16 | −179.3 (2) |
N2—Dy2—O11—C21 | −92.0 (2) | C19—N3—C15—C20 | −176.2 (2) |
N1—Dy2—O11—C21 | 150.4 (2) | Dy2—N3—C15—C20 | 2.1 (3) |
N3—Dy2—O11—C21 | 13.0 (2) | C12—N2—C8—C9 | 0.0 (4) |
O5—Dy2—N2—C8 | −1.01 (17) | Dy2—N2—C8—C9 | 177.92 (19) |
O1—Dy2—N2—C8 | 33.4 (2) | C12—N2—C8—C13 | −180.0 (2) |
O7—Dy2—N2—C8 | −179.4 (2) | Dy2—N2—C8—C13 | −2.1 (3) |
O3—Dy2—N2—C8 | −95.45 (18) | O6—C13—C8—N2 | −173.9 (2) |
O11—Dy2—N2—C8 | −148.54 (16) | O5—C13—C8—N2 | 6.2 (3) |
O9—Dy2—N2—C8 | 83.44 (18) | O6—C13—C8—C9 | 6.1 (4) |
N1—Dy2—N2—C8 | −51.34 (19) | O5—C13—C8—C9 | −173.8 (3) |
N3—Dy2—N2—C8 | 131.40 (17) | Dy2—O11—C21—O12 | 161.7 (3) |
O5—Dy2—N2—C12 | 176.9 (2) | Dy2—O11—C21—C19 | −17.3 (4) |
O1—Dy2—N2—C12 | −148.70 (17) | C8—N2—C12—C11 | −0.7 (4) |
O7—Dy2—N2—C12 | −1.49 (17) | Dy2—N2—C12—C11 | −178.6 (2) |
O3—Dy2—N2—C12 | 82.45 (18) | C8—N2—C12—C14 | 179.8 (2) |
O11—Dy2—N2—C12 | 29.4 (2) | Dy2—N2—C12—C14 | 1.9 (3) |
O9—Dy2—N2—C12 | −98.66 (19) | C10—C11—C12—N2 | 0.7 (4) |
N1—Dy2—N2—C12 | 126.56 (18) | C10—C11—C12—C14 | −179.9 (3) |
N3—Dy2—N2—C12 | −50.7 (2) | O8—C14—C12—N2 | 179.4 (2) |
O5—Dy2—O3—C7 | 71.8 (2) | O7—C14—C12—N2 | −1.0 (3) |
O1—Dy2—O3—C7 | −0.7 (2) | O8—C14—C12—C11 | −0.1 (4) |
O7—Dy2—O3—C7 | −156.8 (2) | O7—C14—C12—C11 | 179.5 (3) |
O11—Dy2—O3—C7 | −79.3 (2) | Dy2—O9—C20—O10 | 174.2 (2) |
O9—Dy2—O3—C7 | 134.5 (2) | Dy2—O9—C20—C15 | −6.4 (3) |
N2—Dy2—O3—C7 | 136.5 (2) | N3—C15—C20—O10 | −178.0 (2) |
N1—Dy2—O3—C7 | −2.17 (19) | C16—C15—C20—O10 | 3.3 (4) |
N3—Dy2—O3—C7 | −110.7 (2) | N3—C15—C20—O9 | 2.5 (3) |
O5—Dy2—O9—C20 | −154.7 (2) | C16—C15—C20—O9 | −176.1 (3) |
O1—Dy2—O9—C20 | −73.8 (2) | Dy2—O3—C7—O4 | −173.2 (2) |
O7—Dy2—O9—C20 | 75.2 (2) | Dy2—O3—C7—C5 | 5.0 (3) |
O3—Dy2—O9—C20 | 140.5 (2) | N1—C5—C7—O4 | 172.6 (2) |
O11—Dy2—O9—C20 | 4.1 (2) | C4—C5—C7—O4 | −7.1 (4) |
N2—Dy2—O9—C20 | 138.6 (2) | N1—C5—C7—O3 | −5.8 (3) |
N1—Dy2—O9—C20 | −102.5 (2) | C4—C5—C7—O3 | 174.5 (3) |
N3—Dy2—O9—C20 | 5.4 (2) | N1—C1—C2—C3 | −1.1 (4) |
O5—Dy2—O7—C14 | −1.0 (2) | C6—C1—C2—C3 | 179.7 (3) |
O1—Dy2—O7—C14 | 139.05 (19) | N2—C8—C9—C10 | 0.7 (4) |
O3—Dy2—O7—C14 | −75.7 (2) | C13—C8—C9—C10 | −179.3 (3) |
O11—Dy2—O7—C14 | −156.8 (2) | N1—C5—C4—C3 | −3.3 (4) |
O9—Dy2—O7—C14 | 73.8 (2) | C7—C5—C4—C3 | 176.3 (3) |
N2—Dy2—O7—C14 | 0.9 (2) | C15—N3—C19—C18 | −0.6 (4) |
N1—Dy2—O7—C14 | −108.4 (2) | Dy2—N3—C19—C18 | −178.9 (2) |
N3—Dy2—O7—C14 | 136.3 (2) | C15—N3—C19—C21 | 179.4 (2) |
O5—Dy2—O1—C6 | −76.9 (2) | Dy2—N3—C19—C21 | 1.2 (3) |
O7—Dy2—O1—C6 | 133.71 (19) | O12—C21—C19—N3 | −169.3 (3) |
O3—Dy2—O1—C6 | −0.8 (2) | O11—C21—C19—N3 | 9.8 (4) |
O11—Dy2—O1—C6 | 73.1 (2) | O12—C21—C19—C18 | 10.8 (5) |
O9—Dy2—O1—C6 | −157.6 (2) | O11—C21—C19—C18 | −170.2 (3) |
N2—Dy2—O1—C6 | −108.3 (2) | N3—C15—C16—C17 | −2.3 (4) |
N1—Dy2—O1—C6 | 0.76 (18) | C20—C15—C16—C17 | 176.2 (3) |
N3—Dy2—O1—C6 | 136.4 (2) | C15—C16—C17—C18 | 0.4 (5) |
O1—Dy2—O5—C13 | −151.7 (2) | C16—C17—C18—C19 | 1.4 (5) |
O7—Dy2—O5—C13 | 7.1 (3) | N3—C19—C18—C17 | −1.3 (4) |
O3—Dy2—O5—C13 | 77.6 (2) | C21—C19—C18—C17 | 178.7 (3) |
O11—Dy2—O5—C13 | 139.3 (2) | C12—C11—C10—C9 | 0.1 (4) |
O9—Dy2—O5—C13 | −72.8 (2) | C8—C9—C10—C11 | −0.8 (4) |
N2—Dy2—O5—C13 | 5.2 (2) | C1—C2—C3—C4 | 0.4 (5) |
N1—Dy2—O5—C13 | 141.9 (2) | C5—C4—C3—C2 | 1.7 (4) |
N3—Dy2—O5—C13 | −99.8 (2) | N8—C30—C29—N9 | 0.2 (4) |
O5—Dy2—N3—C19 | −155.57 (17) | C30—C29—N9—C28 | 0.0 (5) |
O1—Dy2—N3—C19 | −102.47 (19) | C29—N9—C28—N8 | −0.2 (5) |
O7—Dy2—N3—C19 | 75.94 (19) | N9—C28—N8—C30 | 0.4 (4) |
O3—Dy2—N3—C19 | 28.1 (2) | C29—C30—N8—C28 | −0.4 (4) |
O11—Dy2—N3—C19 | −6.39 (18) | C26—N7—C25—N6 | −0.2 (4) |
O9—Dy2—N3—C19 | 174.7 (2) | C25—N7—C26—C27 | 0.1 (4) |
N2—Dy2—N3—C19 | 121.87 (18) | N7—C25—N6—C27 | 0.3 (4) |
N1—Dy2—N3—C19 | −55.4 (2) | N7—C26—C27—N6 | 0.1 (4) |
O5—Dy2—N3—C15 | 26.2 (2) | C25—N6—C27—C26 | −0.2 (4) |
O1—Dy2—N3—C15 | 79.27 (18) | N5—C23—C24—N4 | −1.1 (4) |
O7—Dy2—N3—C15 | −102.32 (19) | C24—C23—N5—C22 | 1.0 (4) |
O3—Dy2—N3—C15 | −150.11 (17) | N4—C22—N5—C23 | −0.6 (4) |
O11—Dy2—N3—C15 | 175.4 (2) | N5—C22—N4—C24 | −0.1 (4) |
O9—Dy2—N3—C15 | −3.53 (17) | C23—C24—N4—C22 | 0.8 (4) |
N2—Dy2—N3—C15 | −56.4 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4A···O14i | 0.94 (2) | 2.50 (3) | 3.286 (4) | 141 (4) |
N5—H5···O12i | 0.86 | 2.27 | 3.121 (5) | 171 |
N8—H8A···O10ii | 0.96 (2) | 2.29 (2) | 3.241 (4) | 172 (4) |
N7—H7A···O10iii | 0.87 (2) | 1.82 (2) | 2.695 (4) | 177 (4) |
N7—H7A···O9iii | 0.87 (2) | 2.60 (3) | 3.127 (3) | 120 (3) |
N6—H6···O14iv | 0.86 | 1.89 | 2.731 (4) | 167 |
O13—H2W···O15iv | 0.85 | 2.02 | 2.828 (4) | 159 |
O13—H1W···O11 | 0.85 | 2.05 | 2.896 (3) | 174 |
O13—H1W···O12 | 0.85 | 2.61 | 3.192 (4) | 127 |
O14—H3W···O4 | 0.85 | 1.91 | 2.756 (3) | 178 |
O14—H4W···O6v | 0.85 | 2.06 | 2.842 (3) | 153 |
O15—H5W···O2vi | 0.85 | 2.22 | 3.061 (4) | 169 |
O15—H6W···O4 | 0.85 | 2.00 | 2.845 (4) | 172 |
Symmetry codes: (i) x+1, y, z; (ii) x−1, y, z+1; (iii) x−1, y+1, z; (iv) −x, −y+1, −z+1; (v) −x+1, −y, −z+1; (vi) −x+1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | (C3H5N2)3[Dy(C7H3NO4)3]·3H2O |
Mr | 919.13 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 296 |
a, b, c (Å) | 10.939 (2), 12.099 (2), 14.070 (3) |
α, β, γ (°) | 88.57 (3), 85.64 (3), 67.28 (3) |
V (Å3) | 1712.7 (6) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.27 |
Crystal size (mm) | 0.35 × 0.25 × 0.25 |
Data collection | |
Diffractometer | Bruker APEXII CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.504, 0.601 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 27464, 7447, 7223 |
Rint | 0.022 |
(sin θ/λ)max (Å−1) | 0.639 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.022, 0.060, 1.10 |
No. of reflections | 7447 |
No. of parameters | 505 |
No. of restraints | 3 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.69, −0.77 |
Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
Dy2—O5 | 2.3745 (19) | Dy2—O9 | 2.426 (2) |
Dy2—O1 | 2.4032 (17) | Dy2—N2 | 2.482 (2) |
Dy2—O7 | 2.4072 (18) | Dy2—N1 | 2.492 (2) |
Dy2—O3 | 2.4167 (19) | Dy2—N3 | 2.506 (2) |
Dy2—O11 | 2.420 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
N4—H4A···O14i | 0.937 (19) | 2.50 (3) | 3.286 (4) | 141 (4) |
N5—H5···O12i | 0.86 | 2.27 | 3.121 (5) | 170.8 |
N8—H8A···O10ii | 0.960 (19) | 2.29 (2) | 3.241 (4) | 172 (4) |
N7—H7A···O10iii | 0.873 (18) | 1.823 (19) | 2.695 (4) | 177 (4) |
N7—H7A···O9iii | 0.873 (18) | 2.60 (3) | 3.127 (3) | 120 (3) |
N6—H6···O14iv | 0.86 | 1.89 | 2.731 (4) | 166.5 |
O13—H2W···O15iv | 0.85 | 2.02 | 2.828 (4) | 158.9 |
O13—H1W···O11 | 0.85 | 2.05 | 2.896 (3) | 174.0 |
O13—H1W···O12 | 0.85 | 2.61 | 3.192 (4) | 126.8 |
O14—H3W···O4 | 0.85 | 1.91 | 2.756 (3) | 177.5 |
O14—H4W···O6v | 0.85 | 2.06 | 2.842 (3) | 152.5 |
O15—H5W···O2vi | 0.85 | 2.22 | 3.061 (4) | 169.4 |
O15—H6W···O4 | 0.85 | 2.00 | 2.845 (4) | 172.3 |
Symmetry codes: (i) x+1, y, z; (ii) x−1, y, z+1; (iii) x−1, y+1, z; (iv) −x, −y+1, −z+1; (v) −x+1, −y, −z+1; (vi) −x+1, −y+1, −z+1. |
References
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This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
In recent years, the interaction of pyridine-2,6-dicarboxylic acid (H2pdc) with several metal ions has been extensively studied due to its unique ability to form stable chelates in diverse coordination modes such as bidentate, meridian and bridging (Kjell et al., 1993). A considerable number of metal—pdc complexes have been synthesized and their structures determined over the past decade (Huang et al., 2008; Ghosh et al., 2005; Song et al., 2005; Wu et al., 2008; Yue et al., 2005; Zhao et al., 2005, 2007). Here we present the structure of the title compound (C3N2H5)3[Dy(C7H3NO4)3].(H2O)3, which includes pyridinedicarboxylate (pdc2-) anions and imidazolium (im) counter cations.
The crystal structure is composed of a mononuclear DyIII complex with the rare earth metal cation in a distorted tricapped trigonal-prismatic environment (Fig. 1, Table 1). The DyIII ion is in each case O,N,O-chelated by three tridentate pyridine-2,6-dicarboxylate (pda2-) ligands. Three imidazolium molecules act as counter cations. Moreover, three lattice water molecules are present. Numerous N—H···O, O—H···O and O—H···N hydrogen bonding interactions (Table 2), part of which are bifurcated, lead to a three-dimensional assembly of the structural building blocks.