supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportsimilar papers Open access

wm2398 scheme

Acta Cryst. (2010). E66, m1291-m1292    [ doi:10.1107/S1600536810036421 ]

Triimidazolium tris(pyridine-2,6-dicarboxylato)dysprosate(III) trihydrate

L. Meng and C. Duan

Abstract top

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.

Comment top

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.

Related literature top

For background to pyridine-2,6-dicarboxylic acid and structures of metal complexes with (pda2-) ligands, see: Ghosh et al. (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 top

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.

Refinement top

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).

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: 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).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title compound, showing displacement ellipsoids at the 50% probability level.
Triimidazolium tris(pyridine-2,6-dicarboxylato)dysprosate(III) trihydrate top
Crystal data top
(C3H5N2)3[Dy(C7H3NO4)3]·3H2OZ = 2
Mr = 919.13F(000) = 918
Triclinic, P1Dx = 1.782 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.939 (2) ÅCell parameters from 125 reflections
b = 12.099 (2) Åθ = 7.5–15°
c = 14.070 (3) ŵ = 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
Data collection top
Bruker APEXII CCD
diffractometer		7447 independent reflections
Radiation source: fine-focus sealed tube7223 reflections with I > 2σ(I)
graphiteRint = 0.022
φ and ω scansθmax = 27.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)		h = −13→13
Tmin = 0.504, Tmax = 0.601k = −13→15
27464 measured reflectionsl = −17→17
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.022Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.060H 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 parametersΔρmax = 0.69 e Å−3
3 restraintsΔρmin = −0.77 e Å−3
Crystal data top
(C3H5N2)3[Dy(C7H3NO4)3]·3H2Oγ = 67.28 (3)°
Mr = 919.13V = 1712.7 (6) Å3
Triclinic, P1Z = 2
a = 10.939 (2) ÅMo Kα radiation
b = 12.099 (2) ŵ = 2.27 mm−1
c = 14.070 (3) ÅT = 296 K
α = 88.57 (3)°0.35 × 0.25 × 0.25 mm
β = 85.64 (3)°
Data collection top
Bruker APEXII CCD
diffractometer		7447 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)		7223 reflections with I > 2σ(I)
Tmin = 0.504, Tmax = 0.601Rint = 0.022
27464 measured reflectionsθmax = 27.0°
Refinement top
R[F2 > 2σ(F2)] = 0.022H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.060Δρmax = 0.69 e Å−3
S = 1.10Δρmin = −0.77 e Å−3
7447 reflectionsAbsolute structure: ?
505 parametersFlack parameter: ?
3 restraintsRogers parameter: ?
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Dy20.492045 (10)0.266222 (9)0.252168 (7)0.02219 (4)
N10.38988 (19)0.43970 (17)0.36385 (14)0.0243 (4)
O110.31544 (18)0.41655 (17)0.17113 (13)0.0338 (4)
N20.5350 (2)0.05867 (18)0.30655 (14)0.0257 (4)
O30.29744 (19)0.27164 (17)0.34879 (14)0.0345 (4)
O90.71488 (18)0.14570 (17)0.18726 (13)0.0344 (4)
O70.40575 (19)0.15338 (17)0.15780 (13)0.0348 (4)
O10.60328 (17)0.40305 (16)0.25167 (13)0.0304 (4)
O50.6077 (2)0.20866 (16)0.39291 (13)0.0350 (4)
N30.5446 (2)0.29826 (18)0.07972 (14)0.0265 (4)
O100.8795 (2)0.1004 (2)0.07273 (15)0.0456 (5)
C60.5682 (3)0.4965 (2)0.30392 (18)0.0288 (5)
C140.4159 (3)0.0481 (2)0.17445 (18)0.0298 (5)
C130.6477 (3)0.1058 (2)0.42917 (18)0.0300 (5)
C50.2800 (2)0.4523 (2)0.41906 (17)0.0269 (5)
C10.4427 (2)0.5216 (2)0.36810 (17)0.0268 (5)
O80.3703 (2)−0.01097 (19)0.12661 (15)0.0432 (5)
C150.6663 (2)0.2410 (2)0.03876 (18)0.0290 (5)
C80.6011 (2)0.0175 (2)0.38414 (17)0.0270 (5)
C210.3162 (3)0.4294 (3)0.0813 (2)0.0388 (6)
O60.7192 (2)0.07182 (19)0.49629 (16)0.0475 (5)
C110.5093 (3)−0.1261 (2)0.2908 (2)0.0368 (6)
H110.4774−0.17360.25760.044*
O40.1420 (2)0.34799 (19)0.46686 (15)0.0419 (5)
C120.4892 (2)−0.0110 (2)0.26079 (18)0.0286 (5)
C200.7622 (3)0.1555 (2)0.10429 (19)0.0313 (5)
C70.2347 (2)0.3501 (2)0.41110 (18)0.0282 (5)
O20.6264 (2)0.5655 (2)0.30446 (17)0.0466 (5)
C20.3867 (3)0.6207 (2)0.4278 (2)0.0363 (6)
H20.42600.67620.43060.044*
C90.6241 (3)−0.0961 (2)0.4192 (2)0.0349 (6)
H90.6695−0.12310.47390.042*
C40.2156 (3)0.5508 (2)0.4781 (2)0.0355 (6)
H40.13690.56010.51350.043*
C190.4500 (3)0.3706 (2)0.02714 (18)0.0305 (5)
C160.6994 (3)0.2573 (3)−0.0559 (2)0.0388 (6)
H160.78580.2185−0.08240.047*
C170.6007 (3)0.3327 (3)−0.1099 (2)0.0445 (7)
H170.61990.3450−0.17390.053*
C180.4737 (3)0.3896 (3)−0.0690 (2)0.0413 (6)
H180.40570.4393−0.10470.050*
C100.5776 (3)−0.1689 (2)0.3708 (2)0.0391 (6)
H100.5924−0.24600.39220.047*
O120.2182 (2)0.4833 (3)0.03738 (18)0.0843 (11)
C30.2725 (3)0.6355 (3)0.4827 (2)0.0418 (7)
H30.23320.70170.52290.050*
C300.2356 (3)0.1317 (3)0.9875 (2)0.0349 (6)
H300.27160.07731.03560.042*
C290.3007 (4)0.1858 (4)0.9312 (3)0.0565 (9)
H290.38930.17540.93320.068*
N90.2143 (4)0.2573 (4)0.8719 (3)0.0879 (12)
H9A0.23050.30220.82850.105*
C280.0964 (3)0.2459 (3)0.8928 (2)0.0409 (6)
H280.01840.28560.86280.049*
N80.1118 (4)0.1690 (4)0.9629 (3)0.0694 (9)
H8A0.044 (4)0.144 (4)0.990 (3)0.083*
N70.0067 (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)
H25−0.14680.95700.29590.069*
C260.1345 (3)0.9451 (3)0.2428 (2)0.0461 (7)
H260.20190.95610.20430.055*
N60.0242 (3)0.8977 (3)0.3600 (2)0.0556 (7)
H60.00430.87140.41380.067*
C270.1448 (4)0.8969 (3)0.3299 (3)0.0520 (8)
H270.22090.86820.36350.062*
C230.9146 (3)0.3939 (4)0.1412 (2)0.0529 (8)
H230.86540.44150.09370.063*
C240.8704 (3)0.3407 (3)0.2103 (2)0.0363 (6)
H240.78340.34550.22050.044*
C221.0765 (3)0.2936 (3)0.2290 (3)0.0520 (8)
H221.16000.26030.25290.062*
N51.0434 (3)0.3669 (4)0.1519 (3)0.0713 (10)
H51.09570.39120.11670.086*
O130.0930 (3)0.6349 (2)0.22816 (19)0.0625 (7)
H2W0.04690.61430.27100.094*
H1W0.16090.57400.20920.094*
O140.0736 (2)0.1513 (2)0.46679 (16)0.0482 (5)
H3W0.09360.21270.46520.072*
H4W0.14610.09040.45980.072*
O150.1116 (3)0.4098 (3)0.6635 (2)0.0794 (9)
H5W0.17820.42670.67290.119*
H6W0.11590.39820.60380.119*
N40.9700 (4)0.2789 (3)0.2631 (3)0.0758 (10)
H4A0.966 (5)0.231 (4)0.316 (3)0.091*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Dy20.02178 (6)0.02328 (6)0.02335 (7)−0.01066 (4)−0.00168 (4)−0.00032 (4)
N10.0258 (10)0.0247 (9)0.0244 (9)−0.0116 (8)−0.0031 (8)0.0020 (7)
O110.0279 (9)0.0380 (10)0.0295 (9)−0.0059 (7)−0.0021 (7)0.0010 (7)
N20.0259 (10)0.0265 (9)0.0266 (10)−0.0127 (8)−0.0001 (8)−0.0016 (8)
O30.0353 (10)0.0355 (9)0.0383 (10)−0.0213 (8)0.0089 (8)−0.0095 (8)
O90.0272 (9)0.0370 (10)0.0327 (10)−0.0062 (7)0.0007 (7)0.0046 (8)
O70.0442 (11)0.0354 (9)0.0324 (9)−0.0221 (8)−0.0110 (8)0.0018 (7)
O10.0286 (9)0.0306 (9)0.0349 (9)−0.0156 (7)0.0033 (7)−0.0038 (7)
O50.0469 (11)0.0284 (9)0.0335 (10)−0.0166 (8)−0.0143 (8)0.0015 (7)
N30.0265 (10)0.0279 (10)0.0261 (10)−0.0115 (8)−0.0020 (8)−0.0001 (8)
O100.0290 (10)0.0535 (13)0.0418 (11)−0.0038 (9)0.0053 (8)0.0010 (9)
C60.0294 (12)0.0286 (11)0.0321 (13)−0.0151 (10)−0.0045 (10)0.0031 (9)
C140.0282 (12)0.0353 (13)0.0298 (12)−0.0168 (10)0.0000 (10)−0.0045 (10)
C130.0334 (13)0.0297 (12)0.0282 (12)−0.0133 (10)−0.0045 (10)−0.0008 (9)
C50.0279 (12)0.0271 (11)0.0256 (11)−0.0108 (9)−0.0008 (9)0.0015 (9)
C10.0293 (12)0.0262 (11)0.0277 (12)−0.0133 (9)−0.0045 (9)0.0019 (9)
O80.0535 (12)0.0449 (11)0.0446 (11)−0.0312 (10)−0.0158 (10)−0.0016 (9)
C150.0276 (12)0.0324 (12)0.0278 (12)−0.0128 (10)−0.0004 (9)−0.0022 (9)
C80.0271 (12)0.0279 (11)0.0264 (12)−0.0111 (9)−0.0002 (9)−0.0005 (9)
C210.0306 (13)0.0470 (16)0.0327 (14)−0.0074 (12)−0.0071 (11)0.0016 (12)
O60.0633 (14)0.0397 (11)0.0435 (12)−0.0200 (10)−0.0295 (11)0.0068 (9)
C110.0399 (15)0.0316 (13)0.0454 (15)−0.0207 (11)−0.0034 (12)−0.0024 (11)
O40.0411 (11)0.0447 (11)0.0454 (12)−0.0255 (9)0.0149 (9)−0.0085 (9)
C120.0286 (12)0.0300 (12)0.0312 (12)−0.0158 (10)−0.0008 (10)−0.0025 (10)
C200.0256 (12)0.0313 (12)0.0350 (14)−0.0090 (10)−0.0001 (10)−0.0028 (10)
C70.0269 (12)0.0307 (12)0.0290 (12)−0.0136 (10)−0.0002 (9)0.0015 (9)
O20.0484 (12)0.0445 (11)0.0597 (14)−0.0336 (10)0.0092 (10)−0.0107 (10)
C20.0434 (15)0.0301 (12)0.0396 (15)−0.0191 (11)0.0000 (12)−0.0049 (11)
C90.0339 (13)0.0321 (13)0.0399 (14)−0.0138 (11)−0.0055 (11)0.0069 (11)
C40.0378 (14)0.0338 (13)0.0348 (14)−0.0154 (11)0.0080 (11)−0.0058 (11)
C190.0314 (13)0.0335 (12)0.0260 (12)−0.0118 (10)−0.0035 (10)0.0020 (10)
C160.0351 (14)0.0504 (16)0.0304 (13)−0.0170 (12)0.0055 (11)−0.0030 (12)
C170.0501 (18)0.0593 (19)0.0244 (13)−0.0221 (15)0.0007 (12)0.0048 (12)
C180.0438 (16)0.0486 (16)0.0296 (14)−0.0155 (13)−0.0068 (12)0.0077 (12)
C100.0413 (15)0.0291 (13)0.0514 (17)−0.0186 (11)−0.0044 (13)0.0082 (12)
O120.0377 (13)0.131 (3)0.0416 (14)0.0155 (15)−0.0127 (11)0.0054 (15)
C30.0505 (17)0.0311 (13)0.0430 (16)−0.0161 (12)0.0083 (13)−0.0122 (12)
C300.0391 (14)0.0399 (14)0.0301 (13)−0.0187 (12)−0.0093 (11)−0.0013 (11)
C290.0447 (18)0.069 (2)0.057 (2)−0.0227 (17)−0.0042 (16)0.0032 (17)
N90.097 (3)0.088 (3)0.072 (2)−0.031 (2)0.000 (2)0.019 (2)
C280.0372 (15)0.0498 (16)0.0341 (14)−0.0145 (13)−0.0077 (12)0.0051 (12)
N80.069 (2)0.079 (2)0.068 (2)−0.0367 (19)−0.0072 (17)−0.0045 (18)
N70.0380 (13)0.0514 (15)0.0421 (14)−0.0099 (11)−0.0052 (11)0.0048 (12)
C250.0390 (17)0.072 (2)0.056 (2)−0.0163 (16)0.0029 (15)0.0062 (18)
C260.0381 (15)0.0491 (17)0.0527 (18)−0.0185 (13)−0.0025 (13)−0.0035 (14)
N60.0671 (19)0.0552 (17)0.0408 (15)−0.0205 (15)0.0000 (13)0.0057 (12)
C270.0521 (19)0.0497 (18)0.056 (2)−0.0181 (15)−0.0202 (16)−0.0003 (15)
C230.0414 (17)0.073 (2)0.0451 (18)−0.0223 (16)−0.0081 (14)0.0018 (16)
C240.0236 (12)0.0502 (16)0.0407 (15)−0.0206 (11)0.0011 (10)−0.0094 (12)
C220.0242 (14)0.061 (2)0.064 (2)−0.0068 (13)−0.0130 (14)−0.0145 (17)
N50.0547 (19)0.094 (3)0.079 (2)−0.0465 (19)0.0196 (17)−0.026 (2)
O130.0524 (14)0.0571 (15)0.0597 (15)−0.0014 (12)−0.0012 (12)−0.0022 (12)
O140.0477 (12)0.0453 (12)0.0567 (14)−0.0235 (10)−0.0070 (10)0.0091 (10)
O150.090 (2)0.102 (2)0.0473 (15)−0.0424 (19)0.0164 (14)−0.0014 (15)
N40.093 (3)0.058 (2)0.071 (2)−0.023 (2)−0.009 (2)0.0016 (17)
Geometric parameters (Å, °) top
Dy2—O52.3745 (19)C4—H40.9300
Dy2—O12.4032 (17)C19—C181.388 (4)
Dy2—O72.4072 (18)C16—C171.381 (4)
Dy2—O32.4167 (19)C16—H160.9300
Dy2—O112.420 (2)C17—C181.376 (4)
Dy2—O92.426 (2)C17—H170.9300
Dy2—N22.482 (2)C18—H180.9300
Dy2—N12.492 (2)C10—H100.9300
Dy2—N32.506 (2)C3—H30.9300
N1—C11.331 (3)C30—N81.322 (4)
N1—C51.339 (3)C30—C291.345 (5)
O11—C211.270 (3)C30—H300.9300
N2—C81.333 (3)C29—N91.339 (5)
N2—C121.334 (3)C29—H290.9300
O3—C71.260 (3)N9—C281.359 (5)
O9—C201.262 (3)N9—H9A0.8600
O7—C141.253 (3)C28—N81.313 (5)
O1—C61.277 (3)C28—H280.9300
O5—C131.258 (3)N8—H8A0.960 (19)
N3—C191.330 (3)N7—C251.304 (4)
N3—C151.333 (3)N7—C261.359 (4)
O10—C201.246 (3)N7—H7A0.873 (18)
C6—O21.230 (3)C25—N61.315 (5)
C6—C11.515 (4)C25—H250.9300
C14—O81.250 (3)C26—C271.338 (5)
C14—C121.514 (4)C26—H260.9300
C13—O61.232 (3)N6—C271.351 (5)
C13—C81.518 (3)N6—H60.8600
C5—C41.385 (4)C27—H270.9300
C5—C71.510 (3)C23—C241.317 (5)
C1—C21.387 (4)C23—N51.337 (5)
C15—C161.383 (4)C23—H230.9300
C15—C201.511 (4)C24—N41.328 (5)
C8—C91.384 (3)C24—H240.9300
C21—O121.223 (4)C22—N41.301 (5)
C21—C191.511 (4)C22—N51.362 (5)
C11—C101.375 (4)C22—H220.9300
C11—C121.383 (4)N5—H50.8600
C11—H110.9300O13—H2W0.8499
O4—C71.241 (3)O13—H1W0.8500
C2—C31.369 (4)O14—H3W0.8501
C2—H20.9300O14—H4W0.8500
C9—C101.388 (4)O15—H5W0.8500
C9—H90.9300O15—H6W0.8501
C4—C31.395 (4)N4—H4A0.937 (19)
O5—Dy2—O178.70 (7)O10—C20—O9125.6 (3)
O5—Dy2—O7129.04 (6)O10—C20—C15118.3 (2)
O1—Dy2—O7146.45 (6)O9—C20—C15116.1 (2)
O5—Dy2—O386.53 (7)O4—C7—O3125.3 (2)
O1—Dy2—O3128.79 (6)O4—C7—C5118.4 (2)
O7—Dy2—O377.27 (7)O3—C7—C5116.3 (2)
O5—Dy2—O11147.58 (7)C3—C2—C1119.0 (2)
O1—Dy2—O1188.66 (7)C3—C2—H2120.5
O7—Dy2—O1175.43 (7)C1—C2—H2120.5
O3—Dy2—O1178.34 (7)C8—C9—C10118.3 (3)
O5—Dy2—O978.53 (7)C8—C9—H9120.8
O1—Dy2—O977.03 (7)C10—C9—H9120.8
O7—Dy2—O989.53 (7)C5—C4—C3117.9 (3)
O3—Dy2—O9147.00 (7)C5—C4—H4121.1
O11—Dy2—O9127.78 (6)C3—C4—H4121.1
O5—Dy2—N264.77 (7)N3—C19—C18122.3 (3)
O1—Dy2—N2137.08 (6)N3—C19—C21114.1 (2)
O7—Dy2—N264.30 (7)C18—C19—C21123.6 (2)
O3—Dy2—N272.61 (7)C17—C16—C15118.2 (3)
O11—Dy2—N2134.24 (7)C17—C16—H16120.9
O9—Dy2—N274.41 (7)C15—C16—H16120.9
O5—Dy2—N174.09 (7)C18—C17—C16119.8 (3)
O1—Dy2—N164.41 (6)C18—C17—H17120.1
O7—Dy2—N1134.39 (7)C16—C17—H17120.1
O3—Dy2—N164.39 (7)C17—C18—C19118.2 (3)
O11—Dy2—N173.51 (7)C17—C18—H18120.9
O9—Dy2—N1136.03 (7)C19—C18—H18120.9
N2—Dy2—N1121.12 (7)C11—C10—C9119.5 (2)
O5—Dy2—N3137.66 (7)C11—C10—H10120.2
O1—Dy2—N374.77 (7)C9—C10—H10120.2
O7—Dy2—N371.72 (7)C2—C3—C4119.6 (3)
O3—Dy2—N3135.76 (7)C2—C3—H3120.2
O11—Dy2—N363.97 (7)C4—C3—H3120.2
O9—Dy2—N363.82 (7)N8—C30—C29108.5 (3)
N2—Dy2—N3118.21 (7)N8—C30—H30125.7
N1—Dy2—N3120.61 (7)C29—C30—H30125.7
C1—N1—C5119.4 (2)N9—C29—C30107.2 (3)
C1—N1—Dy2120.34 (16)N9—C29—H29126.4
C5—N1—Dy2120.26 (15)C30—C29—H29126.4
C21—O11—Dy2124.08 (17)C29—N9—C28107.4 (3)
C8—N2—C12119.5 (2)C29—N9—H9A126.3
C8—N2—Dy2119.67 (16)C28—N9—H9A126.3
C12—N2—Dy2120.78 (16)N8—C28—N9108.0 (3)
C7—O3—Dy2124.83 (16)N8—C28—H28126.0
C20—O9—Dy2125.16 (16)N9—C28—H28126.0
C14—O7—Dy2125.14 (16)C28—N8—C30108.8 (3)
C6—O1—Dy2125.57 (16)C28—N8—H8A124 (3)
C13—O5—Dy2125.83 (16)C30—N8—H8A127 (3)
C19—N3—C15119.0 (2)C25—N7—C26108.6 (3)
C19—N3—Dy2120.24 (17)C25—N7—H7A123 (3)
C15—N3—Dy2120.71 (16)C26—N7—H7A128 (3)
O2—C6—O1125.4 (2)N7—C25—N6109.0 (3)
O2—C6—C1119.6 (2)N7—C25—H25125.5
O1—C6—C1115.0 (2)N6—C25—H25125.5
O8—C14—O7125.7 (2)C27—C26—N7106.8 (3)
O8—C14—C12118.0 (2)C27—C26—H26126.6
O7—C14—C12116.3 (2)N7—C26—H26126.6
O6—C13—O5126.3 (2)C25—N6—C27108.3 (3)
O6—C13—C8118.5 (2)C25—N6—H6125.8
O5—C13—C8115.2 (2)C27—N6—H6125.8
N1—C5—C4122.2 (2)C26—C27—N6107.3 (3)
N1—C5—C7114.0 (2)C26—C27—H27126.4
C4—C5—C7123.8 (2)N6—C27—H27126.4
N1—C1—C2121.8 (2)C24—C23—N5107.4 (3)
N1—C1—C6114.6 (2)C24—C23—H23126.3
C2—C1—C6123.5 (2)N5—C23—H23126.3
N3—C15—C16122.4 (2)C23—C24—N4108.9 (3)
N3—C15—C20113.9 (2)C23—C24—H24125.5
C16—C15—C20123.7 (2)N4—C24—H24125.5
N2—C8—C9122.0 (2)N4—C22—N5107.5 (3)
N2—C8—C13114.1 (2)N4—C22—H22126.3
C9—C8—C13123.9 (2)N5—C22—H22126.3
O12—C21—O11125.0 (3)C23—N5—C22107.4 (3)
O12—C21—C19119.4 (3)C23—N5—H5126.3
O11—C21—C19115.6 (2)C22—N5—H5126.3
C10—C11—C12118.7 (2)H2W—O13—H1W109.8
C10—C11—H11120.6H3W—O14—H4W107.0
C12—C11—H11120.6H5W—O15—H6W105.4
N2—C12—C11121.9 (2)C22—N4—C24108.8 (3)
N2—C12—C14113.5 (2)C22—N4—H4A125 (3)
C11—C12—C14124.6 (2)C24—N4—H4A126 (3)
O5—Dy2—N1—C185.81 (18)N1—Dy2—N3—C15126.34 (18)
O1—Dy2—N1—C10.95 (16)Dy2—O1—C6—O2178.9 (2)
O7—Dy2—N1—C1−144.58 (16)Dy2—O1—C6—C1−2.1 (3)
O3—Dy2—N1—C1179.64 (19)Dy2—O7—C14—O8179.2 (2)
O11—Dy2—N1—C1−95.64 (18)Dy2—O7—C14—C12−0.3 (3)
O9—Dy2—N1—C132.2 (2)Dy2—O5—C13—O6172.1 (2)
N2—Dy2—N1—C1132.20 (17)Dy2—O5—C13—C8−8.0 (3)
N3—Dy2—N1—C1−50.61 (19)C1—N1—C5—C42.7 (4)
O5—Dy2—N1—C5−95.26 (18)Dy2—N1—C5—C4−176.21 (19)
O1—Dy2—N1—C5179.88 (19)C1—N1—C5—C7−177.0 (2)
O7—Dy2—N1—C534.4 (2)Dy2—N1—C5—C74.1 (3)
O3—Dy2—N1—C5−1.43 (16)C5—N1—C1—C2−0.4 (4)
O11—Dy2—N1—C583.29 (17)Dy2—N1—C1—C2178.49 (19)
O9—Dy2—N1—C5−148.86 (16)C5—N1—C1—C6178.8 (2)
N2—Dy2—N1—C5−48.87 (19)Dy2—N1—C1—C6−2.2 (3)
N3—Dy2—N1—C5128.32 (17)O2—C6—C1—N1−178.2 (2)
O5—Dy2—O11—C21153.0 (2)O1—C6—C1—N12.7 (3)
O1—Dy2—O11—C2186.7 (2)O2—C6—C1—C21.1 (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—C162.4 (4)
O9—Dy2—O11—C2114.3 (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—C21150.4 (2)Dy2—N3—C15—C202.1 (3)
N3—Dy2—O11—C2113.0 (2)C12—N2—C8—C90.0 (4)
O5—Dy2—N2—C8−1.01 (17)Dy2—N2—C8—C9177.92 (19)
O1—Dy2—N2—C833.4 (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—N26.2 (3)
O9—Dy2—N2—C883.44 (18)O6—C13—C8—C96.1 (4)
N1—Dy2—N2—C8−51.34 (19)O5—C13—C8—C9−173.8 (3)
N3—Dy2—N2—C8131.40 (17)Dy2—O11—C21—O12161.7 (3)
O5—Dy2—N2—C12176.9 (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—C1282.45 (18)C8—N2—C12—C14179.8 (2)
O11—Dy2—N2—C1229.4 (2)Dy2—N2—C12—C141.9 (3)
O9—Dy2—N2—C12−98.66 (19)C10—C11—C12—N20.7 (4)
N1—Dy2—N2—C12126.56 (18)C10—C11—C12—C14−179.9 (3)
N3—Dy2—N2—C12−50.7 (2)O8—C14—C12—N2179.4 (2)
O5—Dy2—O3—C771.8 (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—C11179.5 (3)
O11—Dy2—O3—C7−79.3 (2)Dy2—O9—C20—O10174.2 (2)
O9—Dy2—O3—C7134.5 (2)Dy2—O9—C20—C15−6.4 (3)
N2—Dy2—O3—C7136.5 (2)N3—C15—C20—O10−178.0 (2)
N1—Dy2—O3—C7−2.17 (19)C16—C15—C20—O103.3 (4)
N3—Dy2—O3—C7−110.7 (2)N3—C15—C20—O92.5 (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—C2075.2 (2)Dy2—O3—C7—C55.0 (3)
O3—Dy2—O9—C20140.5 (2)N1—C5—C7—O4172.6 (2)
O11—Dy2—O9—C204.1 (2)C4—C5—C7—O4−7.1 (4)
N2—Dy2—O9—C20138.6 (2)N1—C5—C7—O3−5.8 (3)
N1—Dy2—O9—C20−102.5 (2)C4—C5—C7—O3174.5 (3)
N3—Dy2—O9—C205.4 (2)N1—C1—C2—C3−1.1 (4)
O5—Dy2—O7—C14−1.0 (2)C6—C1—C2—C3179.7 (3)
O1—Dy2—O7—C14139.05 (19)N2—C8—C9—C100.7 (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—C1473.8 (2)C7—C5—C4—C3176.3 (3)
N2—Dy2—O7—C140.9 (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—C14136.3 (2)C15—N3—C19—C21179.4 (2)
O5—Dy2—O1—C6−76.9 (2)Dy2—N3—C19—C211.2 (3)
O7—Dy2—O1—C6133.71 (19)O12—C21—C19—N3−169.3 (3)
O3—Dy2—O1—C6−0.8 (2)O11—C21—C19—N39.8 (4)
O11—Dy2—O1—C673.1 (2)O12—C21—C19—C1810.8 (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—C60.76 (18)C20—C15—C16—C17176.2 (3)
N3—Dy2—O1—C6136.4 (2)C15—C16—C17—C180.4 (5)
O1—Dy2—O5—C13−151.7 (2)C16—C17—C18—C191.4 (5)
O7—Dy2—O5—C137.1 (3)N3—C19—C18—C17−1.3 (4)
O3—Dy2—O5—C1377.6 (2)C21—C19—C18—C17178.7 (3)
O11—Dy2—O5—C13139.3 (2)C12—C11—C10—C90.1 (4)
O9—Dy2—O5—C13−72.8 (2)C8—C9—C10—C11−0.8 (4)
N2—Dy2—O5—C135.2 (2)C1—C2—C3—C40.4 (5)
N1—Dy2—O5—C13141.9 (2)C5—C4—C3—C21.7 (4)
N3—Dy2—O5—C13−99.8 (2)N8—C30—C29—N90.2 (4)
O5—Dy2—N3—C19−155.57 (17)C30—C29—N9—C280.0 (5)
O1—Dy2—N3—C19−102.47 (19)C29—N9—C28—N8−0.2 (5)
O7—Dy2—N3—C1975.94 (19)N9—C28—N8—C300.4 (4)
O3—Dy2—N3—C1928.1 (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—C19174.7 (2)C25—N7—C26—C270.1 (4)
N2—Dy2—N3—C19121.87 (18)N7—C25—N6—C270.3 (4)
N1—Dy2—N3—C19−55.4 (2)N7—C26—C27—N60.1 (4)
O5—Dy2—N3—C1526.2 (2)C25—N6—C27—C26−0.2 (4)
O1—Dy2—N3—C1579.27 (18)N5—C23—C24—N4−1.1 (4)
O7—Dy2—N3—C15−102.32 (19)C24—C23—N5—C221.0 (4)
O3—Dy2—N3—C15−150.11 (17)N4—C22—N5—C23−0.6 (4)
O11—Dy2—N3—C15175.4 (2)N5—C22—N4—C24−0.1 (4)
O9—Dy2—N3—C15−3.53 (17)C23—C24—N4—C220.8 (4)
N2—Dy2—N3—C15−56.4 (2)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N4—H4A···O14i0.94 (2)2.50 (3)3.286 (4)141 (4)
N5—H5···O12i0.862.273.121 (5)171
N8—H8A···O10ii0.96 (2)2.29 (2)3.241 (4)172 (4)
N7—H7A···O10iii0.87 (2)1.82 (2)2.695 (4)177 (4)
N7—H7A···O9iii0.87 (2)2.60 (3)3.127 (3)120 (3)
N6—H6···O14iv0.861.892.731 (4)167
O13—H2W···O15iv0.852.022.828 (4)159
O13—H1W···O110.852.052.896 (3)174
O13—H1W···O120.852.613.192 (4)127
O14—H3W···O40.851.912.756 (3)178
O14—H4W···O6v0.852.062.842 (3)153
O15—H5W···O2vi0.852.223.061 (4)169
O15—H6W···O40.852.002.845 (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.
Table 1
Selected geometric parameters (Å) top
Dy2—O52.3745 (19)Dy2—O92.426 (2)
Dy2—O12.4032 (17)Dy2—N22.482 (2)
Dy2—O72.4072 (18)Dy2—N12.492 (2)
Dy2—O32.4167 (19)Dy2—N32.506 (2)
Dy2—O112.420 (2)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N4—H4A···O14i0.94 (2)2.50 (3)3.286 (4)141 (4)
N5—H5···O12i0.862.273.121 (5)171
N8—H8A···O10ii0.96 (2)2.29 (2)3.241 (4)172 (4)
N7—H7A···O10iii0.87 (2)1.82 (2)2.695 (4)177 (4)
N7—H7A···O9iii0.87 (2)2.60 (3)3.127 (3)120 (3)
N6—H6···O14iv0.861.892.731 (4)167
O13—H2W···O15iv0.852.022.828 (4)159
O13—H1W···O110.852.052.896 (3)174
O13—H1W···O120.852.613.192 (4)127
O14—H3W···O40.851.912.756 (3)178
O14—H4W···O6v0.852.062.842 (3)153
O15—H5W···O2vi0.852.223.061 (4)169
O15—H6W···O40.852.002.845 (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.
references
References top

Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.

Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.

Ghosh, S. K. & Bharadwaj, P. K. (2005). Inorg. Chem. 44, 3156–3161.

Huang, Y.-G., Yuan, D.-Q., Gong, Y.-Q., Jiang, F.-L. & Hong, M.-C. (2008). J. Mol. Struct. 872, 99–104.

Kjell, H., Martin, L., Goran, S. & Jorgen, A. (1993). Acta Chem. Scand. 47, 449–455.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.

Song, Y.-S., Yan, B. & Chen, Z.-X. (2005). J. Mol. Struct. 750, 101–108.

Wu, J.-Y., Yin, J.-F., Tseng, T.-W. & Lu, K.-L. (2008). Inorg. Chem. Commun. 11, 314–317.

Yue, Q., Yang, J., Li, G.-H., Xu, W., Chen, J.-S. & Wang, S.-N. (2005). Inorg. Chem. 44, 5241–5246.

Zhao, B., Yi, L., Dai, Y., Chen, X.-Y., Cheng, F., Liao, D.-Z., Yan, S.-P. & Jiang, Z.-H. (2005). Inorg. Chem. 44, 911–920.

Zhao, X.-Q., Zhao, B., Ma, Y., Shi, W., Cheng, P., Jiang, Z.-H., Liao, D.-Z. & Yan, S.-P. (2007). Inorg. Chem. 46, 5832–5834.