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Acta Cryst. (2007). E63, m1910    [ doi:10.1107/S160053680702795X ]

[13,27-Dimethyl-3,6,9,17,20,23-hexaazatricyclo[23.3.1.111,15]triaconta-1(29),2,9,11,13,15(30),16,23,25,27-decaene-29,30-diol-[kappa]5N3,N6,N9,O29,O30]bis(nitrato-[kappa]2O,O')dysprosium(III) nitrate monohydrate

W.-B. Sun

Abstract top

The asymmetric unit of the title complex, [Dy(C26H34N6O2)(NO3)2]NO3·H2O, comprises two cations and two anions, together with two water molecules. The Dy atom exhibits a nine-coordinate distorted tricapped trigonal-prismatic coordination geometry. The water molecules are disordered over five positions, each with a site-occupation factor of 0.4. The crystal structure involves N-H...O and N-H...N hydrogen bonds.

Comment top

Lanthanide macrocyclic complexes have received much attention due to their unique properties and many valuable applications such as fluorescent probes in biological systems, material science and chemical processes (Bunzli & Piguet, 2002). Generally, the syntheses of lanthanide macrocyclic complexes are carried out in the presence of a suitable lanthanide ion which acts as a template for macrocycle formation, Most of them are symmetric (Hu et al., 2005). There have been few reports of asymmetric lanthanide complexes.

Recently, Hu et al. (Hu, Qiu et al., 2007; Hu, Chen et al., 2007) have reported the crystal structures of GdIII and LuIII complexes with a macrocyclic ligand derived from 2,6-diformyl-4-methylphenol and 1,5-diamino-3-azapentane: [Gd(C26H34N6O2)(NO3)2]+(NO3)−·H2O and [Lu(C26H34N6O2)(NO3)2]+(NO3)−·0.5H2O·0.25CH3COOC2H5. In these complexes, the central lanthanide ion is nine-coordinate, being bound to five donor atoms from the cyclic polydentate ligand and to four O of two bidentate nitrate anions. Reported here is a new DyIII analogue [Dy(III)(C26H34N6O2)(NO3)2]+(NO3)−·H2O, which exhibits a similar nine-coordinate distorted tricapped trigonal prismatic coordination geometry (Fig. 1 & Fig. 2). The title complex is not isostructural with its GdIII and LuIII analogues. (space groups Cc and C2/c, respectively).

Related literature top

For a general discussion of macrocyclic lanthanide complexes, see Bunzli & Piguet (2002). Some examples of symmetric macrocyclic lanthanide complexes are given in Hu et al. (2005). The GdIII and LuIII analogues of the title complex have been reported recently (Hu, Qiu et al., 2007; Hu, Chen et al., 2007).

Experimental top

To a methanolic solution (20 ml) of 2,6-diformyl-4-methylphenol (1 mmol) and Dy(NO3)3·6H2O (0.5 mmol), 1,5-diamino-3-azapentane (1 mmol) was added dropwise. After refluxing for 3 h, the solvent was removed. The resulting yellow solid was recrystallized from CH3CN, yielding yellow block crystals suitable for X-ray analysis.

Refinement top

H atoms bound to C atoms were placed geometrically (C—H 0.93 to 0.97 Å) and were allowed to ride during refinement with Uiso(H) = 1.2Ueq(C). H atoms bound to N atoms were visible in difference Fourier maps, but were placed geometrically with N—H = 0.90 or 0.91 Å for N(sp3) and 0.86 Å for N(sp2), and allowed to ride during refinement with Uiso(H) = 1.2Ueq(N). H atoms of the water molecules were located in difference Fourier maps, then their O—H distances were normalized to 0.85 Å and they were refined as riding with Uiso(H) = 1.2Ueq(O).

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title complex showing displacement ellipsoids at the 30% probability level. H atoms are omitted.
[Figure 2] Fig. 2. Distorted tricapped trigonal prismatic coordination environment of DyIII.
(13,27-Dimethyl-3,6,9,17,20,23-hexaazatricyclo[23.3.1.111,15]triaconta- 1(29),2,9,11,13,15 (30),16,23,25,27-decaene-29,30-diol- κ5N3,N6,N9,O29,O30)bis(nitrato-κ2O,O')dysprosium(III) nitrate monohydrate top
Crystal data top
[Dy(C26H34N6O2)(NO3)2]NO3·H2OZ = 4
Mr = 829.14F000 = 1668
Triclinic, P1Dx = 1.504 Mg m−3
Hall symbol: -P 1Mo Kα radiation
λ = 0.71073 Å
a = 14.005 (3) ÅCell parameters from 6195 reflections
b = 14.045 (3) Åθ = 2.5–22.7º
c = 21.896 (4) ŵ = 2.11 mm−1
α = 96.386 (3)ºT = 292 (2) K
β = 99.094 (3)ºBlock, yellow
γ = 118.217 (3)º0.30 × 0.22 × 0.20 mm
V = 3661.0 (13) Å3
Data collection top
Bruker SMART CCD
diffractometer		14395 independent reflections
Radiation source: sealed tube10889 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.042
T = 292(2) Kθmax = 26.0º
φ and ω scansθmin = 1.0º
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		h = −17→17
Tmin = 0.58, Tmax = 0.66k = −17→17
36705 measured reflectionsl = −27→27
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full with fixed elements per cycleHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.051H-atom parameters constrained
wR(F2) = 0.115  w = 1/[σ2(Fo2) + (0.06P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
14395 reflectionsΔρmax = 0.45 e Å−3
872 parametersΔρmin = −1.42 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Dy(C26H34N6O2)(NO3)2]NO3·H2Oγ = 118.217 (3)º
Mr = 829.14V = 3661.0 (13) Å3
Triclinic, P1Z = 4
a = 14.005 (3) ÅMo Kα
b = 14.045 (3) ŵ = 2.11 mm−1
c = 21.896 (4) ÅT = 292 (2) K
α = 96.386 (3)º0.30 × 0.22 × 0.20 mm
β = 99.094 (3)º
Data collection top
Bruker SMART CCD
diffractometer		14395 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		10889 reflections with I > 2σ(I)
Tmin = 0.58, Tmax = 0.66Rint = 0.042
36705 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.051872 parameters
wR(F2) = 0.115H-atom parameters constrained
S = 1.04Δρmax = 0.45 e Å−3
14395 reflectionsΔρmin = −1.42 e Å−3
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*/UeqOcc. (<1)
C10.47785 (19)0.8435 (3)0.33060 (16)0.0424 (11)
C20.3861 (3)0.7491 (2)0.33767 (16)0.0457 (11)
C30.2811 (2)0.7395 (2)0.32526 (17)0.0501 (12)
H30.21970.67630.33000.060*
C40.2679 (2)0.8243 (3)0.30578 (16)0.0487 (12)
C50.3597 (3)0.9188 (2)0.29872 (17)0.0518 (12)
H50.35090.97550.28570.062*
C60.4647 (2)0.9284 (2)0.31113 (17)0.0626 (15)
C70.3928 (4)0.6602 (4)0.3563 (2)0.0423 (11)
H70.32670.59880.35800.051*
C80.1511 (5)0.8098 (5)0.2895 (3)0.0620 (15)
H8A0.14690.86250.31920.093*
H8B0.09720.73630.29150.093*
H8C0.13570.82140.24750.093*
C90.5574 (5)1.0360 (5)0.3046 (3)0.0622 (14)
H90.53921.09010.29700.075*
C100.8457 (3)0.7694 (3)0.34372 (15)0.0533 (13)
C110.9485 (3)0.83720 (19)0.38639 (15)0.0465 (11)
C121.0079 (2)0.7912 (2)0.41481 (14)0.0528 (13)
H121.07670.83650.44340.063*
C130.9645 (3)0.6774 (2)0.40058 (15)0.0461 (11)
C140.8618 (3)0.60959 (19)0.35791 (16)0.0528 (13)
H140.83270.53340.34840.063*
C150.8024 (2)0.6556 (2)0.32948 (14)0.0560 (13)
C161.0050 (5)0.9589 (5)0.4031 (2)0.0616 (15)
H161.07940.99560.42540.074*
C171.0299 (4)0.6233 (5)0.4289 (2)0.0531 (13)
H17A1.06930.61170.39940.080*
H17B0.97880.55360.43710.080*
H17C1.08230.67110.46770.080*
C180.6876 (5)0.5791 (5)0.2826 (2)0.0580 (14)
H180.67390.50320.27300.070*
C190.4863 (4)0.5560 (4)0.3875 (3)0.0500 (12)
H19A0.41480.49120.36680.060*
H19B0.49630.56110.43280.060*
C200.5788 (5)0.5432 (5)0.3666 (3)0.0619 (15)
H20A0.64770.58630.39920.074*
H20B0.55950.46620.36040.074*
C210.4973 (4)0.5106 (5)0.2517 (3)0.0616 (16)
H21A0.43370.52000.25470.074*
H21B0.47510.43300.24760.074*
C220.5480 (4)0.5575 (4)0.1967 (2)0.0515 (13)
H22A0.52540.60910.18370.062*
H22B0.52550.49860.16050.062*
C231.0414 (4)1.1413 (5)0.4118 (3)0.0549 (14)
H23A1.09111.15670.45240.066*
H23B1.08651.16750.38160.066*
C240.9790 (4)1.1999 (4)0.4176 (2)0.0549 (14)
H24A1.02941.27910.42530.066*
H24B0.94461.18420.45310.066*
C250.8306 (4)1.2242 (5)0.3592 (2)0.0531 (13)
H25A0.88001.30120.35920.064*
H25B0.80291.22120.39730.064*
C260.7338 (5)1.1730 (5)0.3014 (3)0.0654 (15)
H26A0.69691.21650.29900.078*
H26B0.75991.16960.26320.078*
C270.2983 (4)−0.1020 (4)0.1215 (2)0.0450 (11)
C280.3961 (4)−0.1080 (5)0.1358 (2)0.0473 (12)
C290.3941 (4)−0.2033 (4)0.1516 (2)0.0446 (11)
H290.4603−0.20490.16120.054*
C300.2948 (4)−0.2947 (4)0.1532 (2)0.0450 (11)
C310.1949 (5)−0.2905 (5)0.1391 (3)0.0565 (13)
H310.1278−0.35080.14050.068*
C320.1965 (5)−0.1951 (4)0.1228 (3)0.0531 (12)
C330.5050 (4)−0.0196 (5)0.1327 (2)0.0498 (12)
H330.5624−0.03600.13790.060*
C340.2921 (5)−0.3957 (5)0.1720 (3)0.0557 (13)
H34A0.2948−0.44040.13660.084*
H34B0.2246−0.43770.18520.084*
H34C0.3553−0.37340.20640.084*
C350.0938 (4)−0.2017 (4)0.1077 (2)0.0420 (11)
H350.0314−0.26540.11090.050*
C360.2392 (4)0.2650 (4)0.1082 (3)0.0543 (13)
C370.2605 (4)0.3269 (4)0.0600 (2)0.0492 (12)
C380.1853 (4)0.3658 (4)0.0384 (3)0.0514 (13)
H380.19950.40790.00760.062*
C390.0952 (5)0.3430 (4)0.0615 (3)0.0572 (15)
C400.0692 (5)0.2750 (4)0.1055 (2)0.0539 (13)
H400.00340.25400.11870.065*
C410.1393 (4)0.2397 (4)0.1287 (2)0.0433 (11)
C420.3492 (4)0.3483 (4)0.0306 (2)0.0421 (10)
H42A0.35680.39140.00040.050*
C430.0218 (4)0.3921 (4)0.0331 (2)0.0550 (14)
H43A0.04790.46410.05820.083*
H43B−0.05470.34420.03330.083*
H43C0.02740.3979−0.00970.083*
C440.1037 (5)0.1637 (4)0.1756 (3)0.0586 (14)
H440.04030.16280.18970.070*
C450.1679 (4)0.0949 (5)0.2612 (2)0.0517 (12)
H45A0.22760.07750.26760.062*
H45B0.14780.10330.30110.062*
C460.0712 (4)0.0098 (5)0.2122 (2)0.0463 (11)
H46A0.0727−0.05890.20580.056*
H46B0.0021−0.00400.22320.056*
C47−0.0090 (4)−0.0068 (4)0.1010 (3)0.0521 (13)
H47A0.00660.03080.06620.062*
H47B−0.0762−0.01100.11030.062*
C48−0.0293 (4)−0.1248 (4)0.0808 (2)0.0458 (11)
H48A−0.0734−0.17190.10650.055*
H48B−0.0705−0.15520.03690.055*
C490.6479 (4)0.1487 (4)0.1208 (2)0.0435 (11)
H49A0.68550.10590.11960.052*
H49B0.68740.20860.15800.052*
C500.6474 (4)0.1958 (4)0.0607 (2)0.0470 (11)
H50A0.72350.24430.05840.056*
H50B0.61160.13580.02360.056*
C510.5600 (4)0.2838 (5)−0.0015 (2)0.0520 (13)
H51A0.50520.2163−0.03180.062*
H51B0.62650.3184−0.01750.062*
C520.5134 (4)0.3620 (4)0.0067 (2)0.0483 (12)
H52A0.57220.43420.03100.058*
H52B0.48500.3707−0.03440.058*
Dy10.75925 (2)0.95316 (2)0.336610 (11)0.05113 (8)
Dy20.407500 (18)0.16379 (2)0.100570 (12)0.04739 (8)
N10.4865 (4)0.6566 (4)0.3717 (2)0.0529 (11)
H1A0.54900.71380.37250.063*
N20.6562 (4)1.0606 (4)0.3082 (2)0.0573 (12)
N30.8918 (4)1.1639 (3)0.3585 (2)0.0463 (10)
H3A0.92671.17850.32620.056*
N40.9631 (4)1.0184 (4)0.3904 (2)0.0538 (11)
N50.6776 (4)0.6179 (4)0.2258 (2)0.0601 (12)
H5A0.71210.59970.19920.072*
H5B0.70720.69180.23420.072*
N60.5944 (3)0.5815 (4)0.3070 (2)0.0537 (11)
N70.7380 (4)0.9146 (4)0.1990 (2)0.0596 (12)
N80.7392 (4)0.9437 (4)0.4685 (2)0.0592 (13)
N90.5318 (4)0.0781 (4)0.1236 (2)0.0586 (12)
N100.0796 (3)−0.1221 (4)0.0888 (2)0.0480 (10)
H10A0.1353−0.06690.08100.058*
N110.0828 (3)0.0565 (3)0.15591 (19)0.0438 (9)
N120.2046 (4)0.2077 (4)0.2318 (2)0.0575 (12)
H12A0.21150.26410.25970.069*
H12B0.26860.22910.21920.069*
N130.4212 (4)0.3152 (4)0.0404 (2)0.0567 (12)
N140.5880 (3)0.2569 (3)0.06133 (18)0.0430 (9)
H14A0.63450.32270.08910.052*
N150.5202 (4)0.2597 (3)0.2372 (2)0.0504 (11)
N160.2567 (3)0.0129 (3)−0.01617 (18)0.0423 (9)
N170.1430 (4)0.3787 (3)0.3121 (2)0.0550 (12)
N180.8148 (4)0.5559 (4)0.1309 (2)0.0554 (11)
O10.5778 (3)0.8473 (3)0.33876 (17)0.0556 (9)
O20.7896 (3)0.8106 (3)0.31100 (18)0.0645 (11)
O30.6560 (3)0.8534 (3)0.22214 (19)0.0638 (11)
O40.8157 (3)0.9962 (3)0.23469 (16)0.0511 (9)
O50.7318 (3)0.8909 (3)0.14592 (18)0.0582 (10)
O60.7480 (3)0.8677 (3)0.43658 (16)0.0534 (9)
O70.7562 (3)1.0260 (3)0.44466 (17)0.0566 (10)
O80.7203 (3)0.9337 (3)0.52032 (18)0.0593 (10)
O90.2978 (3)−0.0141 (3)0.10996 (16)0.0466 (8)
O100.3063 (3)0.2363 (3)0.13515 (16)0.0457 (8)
O110.4298 (3)0.1682 (3)0.21994 (16)0.0539 (9)
O120.5602 (3)0.3048 (3)0.19477 (16)0.0469 (8)
O130.5665 (3)0.3021 (3)0.29462 (19)0.0620 (10)
O140.3596 (2)0.0465 (3)−0.00753 (15)0.0410 (7)
O150.2248 (3)0.0671 (3)0.01518 (15)0.0483 (8)
O160.1887 (3)−0.0741 (3)−0.05426 (17)0.0627 (11)
O170.0664 (3)0.2836 (3)0.28828 (18)0.0665 (12)
O180.2305 (3)0.4028 (3)0.29827 (19)0.0637 (11)
O190.1357 (3)0.4538 (3)0.34430 (18)0.0616 (10)
O200.7317 (3)0.5001 (3)0.13864 (19)0.0686 (12)
O210.8556 (4)0.6503 (4)0.15550 (19)0.0661 (11)
O220.8672 (3)0.5325 (4)0.09746 (18)0.0649 (11)
O230.9291 (9)0.4352 (9)0.2281 (5)0.071 (3)0.40
H23D0.94090.40810.25930.085*0.40
H23E0.89110.38360.19530.085*0.40
O240.2786 (8)0.5461 (8)0.5132 (4)0.058 (2)0.40
H24C0.25830.49910.53660.069*0.40
H24E0.22170.53580.48660.069*0.40
O250.6348 (8)0.7333 (8)0.5865 (4)0.065 (3)0.40
H25D0.65970.68940.59200.078*0.40
H25E0.66460.77130.56030.078*0.40
O260.4610 (10)0.8251 (10)0.5315 (6)0.087 (4)0.40
H26E0.51630.81740.54600.105*0.40
H26D0.47350.85360.49930.105*0.40
O270.3462 (10)0.6915 (12)0.5223 (5)0.097 (5)0.40
H27C0.33880.66550.55560.117*0.40
H27A0.28930.69670.50760.117*0.40
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.039 (2)0.056 (3)0.043 (2)0.033 (2)0.0094 (19)0.007 (2)
C20.036 (2)0.037 (3)0.072 (3)0.024 (2)0.012 (2)0.013 (2)
C30.041 (3)0.052 (3)0.050 (3)0.017 (2)0.016 (2)0.008 (2)
C40.040 (3)0.047 (3)0.061 (3)0.021 (2)0.016 (2)0.016 (2)
C50.051 (3)0.054 (3)0.052 (3)0.027 (3)0.014 (2)0.008 (2)
C60.060 (3)0.065 (4)0.048 (3)0.019 (3)0.018 (3)0.009 (3)
C70.040 (2)0.032 (2)0.038 (2)0.009 (2)0.0065 (18)−0.0072 (18)
C80.064 (4)0.055 (3)0.058 (3)0.021 (3)0.019 (3)0.012 (3)
C90.051 (3)0.051 (3)0.076 (4)0.019 (3)0.014 (3)0.014 (3)
C100.050 (3)0.062 (3)0.031 (2)0.016 (3)0.009 (2)0.004 (2)
C110.040 (3)0.039 (3)0.052 (3)0.012 (2)0.013 (2)0.013 (2)
C120.056 (3)0.037 (3)0.041 (2)0.007 (2)0.005 (2)0.008 (2)
C130.041 (3)0.054 (3)0.044 (2)0.021 (2)0.016 (2)0.019 (2)
C140.053 (3)0.031 (3)0.061 (3)0.009 (2)0.017 (2)0.009 (2)
C150.056 (3)0.047 (3)0.053 (3)0.017 (3)0.013 (2)0.006 (2)
C160.056 (3)0.059 (4)0.045 (3)0.013 (3)0.006 (2)0.002 (2)
C170.044 (3)0.051 (3)0.047 (3)0.012 (2)0.006 (2)0.010 (2)
C180.051 (3)0.059 (3)0.044 (3)0.021 (3)0.000 (2)−0.016 (2)
C190.041 (3)0.046 (3)0.055 (3)0.015 (2)0.009 (2)0.015 (2)
C200.042 (3)0.059 (4)0.066 (3)0.010 (3)0.019 (3)0.006 (3)
C210.038 (3)0.062 (4)0.056 (3)0.019 (3)−0.016 (2)−0.025 (3)
C220.043 (3)0.040 (3)0.047 (3)0.013 (2)−0.013 (2)−0.012 (2)
C230.030 (2)0.066 (4)0.051 (3)0.010 (2)0.013 (2)0.007 (3)
C240.048 (3)0.033 (3)0.055 (3)0.000 (2)0.006 (2)0.006 (2)
C250.045 (3)0.049 (3)0.050 (3)0.010 (2)0.010 (2)0.022 (2)
C260.061 (4)0.065 (4)0.067 (4)0.029 (3)0.014 (3)0.017 (3)
C270.048 (3)0.045 (3)0.033 (2)0.019 (2)0.0073 (19)−0.0041 (19)
C280.045 (3)0.053 (3)0.039 (2)0.027 (2)−0.004 (2)−0.001 (2)
C290.037 (2)0.046 (3)0.045 (2)0.022 (2)0.0017 (19)−0.007 (2)
C300.052 (3)0.039 (3)0.045 (2)0.030 (2)−0.002 (2)−0.001 (2)
C310.057 (3)0.042 (3)0.065 (3)0.020 (3)0.010 (3)0.022 (3)
C320.049 (3)0.041 (3)0.057 (3)0.017 (2)0.006 (2)0.003 (2)
C330.029 (2)0.062 (3)0.045 (3)0.019 (2)−0.0042 (19)−0.005 (2)
C340.047 (3)0.067 (4)0.054 (3)0.029 (3)0.011 (2)0.015 (3)
C350.030 (2)0.021 (2)0.060 (3)0.0082 (18)0.0037 (19)−0.0158 (19)
C360.041 (3)0.039 (3)0.062 (3)0.008 (2)0.008 (2)−0.001 (2)
C370.042 (3)0.040 (3)0.052 (3)0.016 (2)0.000 (2)−0.005 (2)
C380.043 (3)0.032 (3)0.058 (3)0.014 (2)−0.012 (2)−0.012 (2)
C390.060 (3)0.033 (3)0.060 (3)0.025 (3)−0.018 (3)−0.021 (2)
C400.059 (3)0.036 (3)0.044 (3)0.018 (2)−0.009 (2)−0.019 (2)
C410.039 (2)0.040 (3)0.049 (3)0.022 (2)0.005 (2)−0.006 (2)
C420.043 (3)0.034 (2)0.055 (3)0.023 (2)0.012 (2)0.009 (2)
C430.046 (3)0.042 (3)0.050 (3)0.014 (2)−0.021 (2)−0.010 (2)
C440.055 (3)0.035 (3)0.071 (4)0.011 (2)0.008 (3)0.020 (3)
C450.041 (3)0.049 (3)0.051 (3)0.012 (2)0.011 (2)0.009 (2)
C460.038 (2)0.054 (3)0.049 (3)0.021 (2)0.016 (2)0.019 (2)
C470.040 (3)0.043 (3)0.054 (3)0.014 (2)−0.010 (2)−0.001 (2)
C480.043 (3)0.038 (3)0.050 (3)0.017 (2)0.007 (2)0.005 (2)
C490.031 (2)0.040 (3)0.052 (3)0.008 (2)0.023 (2)0.005 (2)
C500.054 (3)0.030 (2)0.047 (3)0.013 (2)0.014 (2)0.006 (2)
C510.038 (3)0.056 (3)0.052 (3)0.015 (2)0.012 (2)0.010 (2)
C520.043 (3)0.045 (3)0.057 (3)0.017 (2)0.017 (2)0.031 (2)
Dy10.04810 (14)0.04859 (15)0.04748 (14)0.01280 (12)0.01949 (11)0.01889 (11)
Dy20.02832 (11)0.04888 (15)0.05916 (15)0.01496 (10)0.01314 (10)0.00690 (11)
N10.048 (2)0.037 (2)0.060 (3)0.008 (2)0.011 (2)0.027 (2)
N20.071 (3)0.052 (3)0.045 (2)0.019 (2)0.032 (2)0.027 (2)
N30.055 (3)0.036 (2)0.049 (2)0.020 (2)0.0164 (19)0.0164 (18)
N40.049 (3)0.053 (3)0.063 (3)0.025 (2)0.021 (2)0.014 (2)
N50.057 (3)0.053 (3)0.048 (2)0.019 (2)−0.005 (2)−0.009 (2)
N60.032 (2)0.057 (3)0.046 (2)0.011 (2)−0.0042 (17)−0.013 (2)
N70.057 (3)0.058 (3)0.048 (3)0.019 (3)0.010 (2)0.007 (2)
N80.053 (3)0.053 (3)0.046 (2)0.014 (2)0.005 (2)−0.015 (2)
N90.043 (2)0.045 (3)0.066 (3)0.006 (2)0.010 (2)0.009 (2)
N100.038 (2)0.048 (3)0.057 (2)0.0151 (19)0.0163 (19)0.029 (2)
N110.035 (2)0.044 (2)0.049 (2)0.0150 (18)0.0192 (17)0.0096 (18)
N120.054 (3)0.051 (3)0.044 (2)0.016 (2)−0.0008 (19)−0.0120 (19)
N130.043 (2)0.050 (3)0.057 (3)0.009 (2)0.011 (2)0.008 (2)
N140.045 (2)0.037 (2)0.0387 (19)0.0139 (18)0.0148 (16)0.0022 (16)
N150.050 (3)0.034 (2)0.049 (2)0.016 (2)−0.005 (2)−0.0042 (19)
N160.040 (2)0.030 (2)0.045 (2)0.0095 (18)0.0063 (17)0.0066 (17)
N170.063 (3)0.024 (2)0.053 (2)0.002 (2)0.015 (2)0.0093 (18)
N180.055 (3)0.054 (3)0.049 (2)0.019 (3)0.015 (2)0.013 (2)
O10.056 (2)0.044 (2)0.053 (2)0.0139 (18)0.0120 (17)0.0167 (16)
O20.056 (2)0.058 (3)0.052 (2)0.016 (2)−0.0029 (18)−0.0034 (18)
O30.048 (2)0.052 (2)0.066 (2)0.0084 (19)0.0002 (18)0.0196 (19)
O40.048 (2)0.043 (2)0.0514 (19)0.0108 (17)0.0169 (16)0.0214 (17)
O50.056 (2)0.052 (2)0.051 (2)0.0130 (19)0.0194 (17)0.0093 (17)
O60.056 (2)0.045 (2)0.0489 (19)0.0133 (18)0.0217 (17)0.0146 (16)
O70.049 (2)0.047 (2)0.049 (2)0.0067 (18)0.0152 (16)−0.0047 (17)
O80.046 (2)0.058 (2)0.060 (2)0.0141 (18)0.0161 (17)0.0123 (19)
O90.0417 (18)0.043 (2)0.0535 (19)0.0170 (16)0.0133 (15)0.0192 (16)
O100.051 (2)0.0321 (17)0.060 (2)0.0260 (16)0.0118 (16)0.0098 (15)
O110.064 (2)0.044 (2)0.0434 (18)0.0184 (19)0.0120 (16)0.0125 (15)
O120.0435 (19)0.044 (2)0.0459 (18)0.0181 (16)0.0133 (15)−0.0010 (15)
O130.059 (2)0.040 (2)0.067 (2)0.0138 (19)0.0045 (19)0.0006 (18)
O140.0268 (15)0.0415 (18)0.0496 (17)0.0160 (14)0.0104 (13)−0.0058 (14)
O150.0468 (19)0.045 (2)0.0423 (17)0.0196 (17)0.0039 (15)−0.0036 (15)
O160.045 (2)0.059 (2)0.052 (2)0.0145 (19)−0.0167 (17)−0.0159 (18)
O170.059 (2)0.046 (2)0.053 (2)−0.0071 (19)0.0226 (18)−0.0012 (17)
O180.050 (2)0.059 (3)0.064 (2)0.018 (2)0.0196 (18)−0.0154 (19)
O190.059 (2)0.053 (2)0.057 (2)0.017 (2)0.0195 (18)−0.0032 (18)
O200.053 (2)0.052 (2)0.060 (2)−0.001 (2)0.0174 (19)−0.0151 (19)
O210.070 (3)0.056 (3)0.061 (2)0.020 (2)0.019 (2)0.020 (2)
O220.061 (2)0.065 (3)0.053 (2)0.019 (2)0.0144 (19)0.0162 (19)
O230.068 (7)0.054 (6)0.067 (6)0.019 (5)−0.012 (5)0.021 (5)
O240.052 (5)0.054 (6)0.042 (4)0.008 (5)0.006 (4)0.016 (4)
O250.065 (6)0.054 (6)0.057 (5)0.022 (5)−0.015 (5)0.024 (5)
O260.064 (7)0.077 (8)0.084 (8)0.007 (6)0.032 (6)−0.005 (6)
O270.078 (8)0.112 (11)0.066 (7)0.046 (8)−0.028 (6)−0.046 (7)
Geometric parameters (Å, °) top
C1—O11.358 (4)C39—C431.576 (5)
C1—C21.390C40—C411.353 (6)
C1—C61.390C40—H400.930
C2—C31.390C41—C441.530 (8)
C2—C71.396 (6)C42—N131.296 (7)
C3—C41.390C42—H42A0.930
C3—H30.930C43—H43A0.960
C4—C51.390C43—H43B0.960
C4—C81.526 (6)C43—H43C0.960
C5—C61.390C44—N111.391 (7)
C5—H50.930C44—N121.533 (7)
C6—C91.498 (6)C44—H440.980
C7—N11.328 (5)C45—C461.463 (7)
C7—H70.930C45—N121.659 (7)
C8—H8A0.960C45—H45A0.970
C8—H8B0.960C45—H45B0.970
C8—H8C0.960C46—N111.455 (6)
C9—N21.244 (6)C46—H46A0.970
C9—H90.930C46—H46B0.970
C10—O21.346 (4)C47—N111.443 (6)
C10—C111.390C47—C481.541 (7)
C10—C151.390C47—H47A0.970
C11—C121.390C47—H47B0.970
C11—C161.474 (7)C48—N101.490 (6)
C12—C131.390C48—H48A0.970
C12—H120.930C48—H48B0.970
C13—C141.390C49—N91.467 (6)
C13—C171.542 (6)C49—C501.538 (7)
C14—C151.390C49—H49A0.970
C14—H140.930C49—H49B0.970
C15—C181.546 (5)C50—N141.451 (7)
C16—N41.259 (7)C50—H50A0.970
C16—H160.930C50—H50B0.970
C17—H17A0.960C51—N141.507 (6)
C17—H17B0.960C51—C521.528 (8)
C17—H17C0.960C51—H51A0.970
C18—N51.425 (6)C51—H51B0.970
C18—N61.501 (6)C52—N131.500 (6)
C18—H180.980C52—H52A0.970
C19—N11.490 (5)C52—H52B0.970
C19—C201.519 (8)Dy1—O22.265 (4)
C19—H19A0.970Dy1—O12.269 (4)
C19—H19B0.970Dy1—O72.486 (3)
C20—N61.475 (6)Dy1—O42.525 (3)
C20—H20A0.970Dy1—O32.548 (4)
C20—H20B0.970Dy1—N42.569 (5)
C21—N61.495 (5)Dy1—N32.578 (4)
C21—C221.548 (8)Dy1—N22.595 (5)
C21—H21A0.970Dy1—O62.602 (3)
C21—H21B0.970Dy2—O102.270 (3)
C22—N51.575 (5)Dy2—O92.287 (3)
C22—H22A0.970Dy2—O142.520 (3)
C22—H22B0.970Dy2—O122.538 (3)
C23—C241.467 (8)Dy2—O152.555 (3)
C23—N41.506 (6)Dy2—N92.564 (5)
C23—H23A0.970Dy2—N132.571 (5)
C23—H23B0.970Dy2—O112.573 (3)
C24—N31.480 (5)Dy2—N142.578 (4)
C24—H24A0.970N1—H1A0.860
C24—H24B0.970N3—H3A0.910
C25—N31.463 (6)N5—H5A0.900
C25—C261.513 (8)N5—H5B0.900
C25—H25A0.970N7—O51.151 (6)
C25—H25B0.970N7—O41.209 (6)
C26—N21.475 (6)N7—O31.288 (6)
C26—H26A0.970N8—O81.214 (6)
C26—H26B0.970N8—O71.257 (7)
C27—O91.291 (5)N8—O61.275 (6)
C27—C281.401 (7)N10—H10A0.860
C27—C321.415 (7)N12—H12A0.900
C28—C291.408 (7)N12—H12B0.900
C28—C331.460 (7)N14—H14A0.910
C29—C301.385 (7)N15—O121.240 (6)
C29—H290.930N15—O131.252 (5)
C30—C311.414 (7)N15—O111.265 (6)
C30—C341.507 (7)N16—O161.231 (5)
C31—C321.416 (8)N16—O151.246 (5)
C31—H310.930N16—O141.259 (5)
C32—C351.379 (7)N17—O181.206 (6)
C33—N91.289 (6)N17—O171.233 (5)
C33—H330.930N17—O191.257 (6)
C34—H34A0.960N18—O201.107 (6)
C34—H34B0.960N18—O211.185 (6)
C34—H34C0.960N18—O221.235 (6)
C35—N101.321 (5)O23—H23D0.850
C35—H350.930O23—H23E0.850
C36—O101.276 (6)O24—H24C0.850
C36—C371.421 (8)O24—H24E0.850
C36—C411.431 (6)O25—H25D0.850
C37—C421.411 (5)O25—H25E0.850
C37—C381.442 (7)O26—H26E0.850
C38—C391.343 (8)O26—H26D0.850
C38—H380.930O27—H27C0.850
C39—C401.400 (8)O27—H27A0.850
O1—C1—C2118.6 (2)N11—C47—H47B109.2
O1—C1—C6121.2 (2)C48—C47—H47B109.2
C2—C1—C6120.0H47A—C47—H47B107.9
C1—C2—C3120.0N10—C48—C47109.7 (4)
C1—C2—C7123.1 (3)N10—C48—H48A109.7
C3—C2—C7116.9 (3)C47—C48—H48A109.7
C4—C3—C2120.0N10—C48—H48B109.7
C4—C3—H3120.0C47—C48—H48B109.7
C2—C3—H3120.0H48A—C48—H48B108.2
C3—C4—C5120.0N9—C49—C50108.3 (4)
C3—C4—C8119.1 (3)N9—C49—H49A110.0
C5—C4—C8120.9 (3)C50—C49—H49A110.0
C6—C5—C4120.0N9—C49—H49B110.0
C6—C5—H5120.0C50—C49—H49B110.0
C4—C5—H5120.0H49A—C49—H49B108.4
C5—C6—C1120.0N14—C50—C49110.2 (4)
C5—C6—C9114.8 (3)N14—C50—H50A109.6
C1—C6—C9125.1 (3)C49—C50—H50A109.6
N1—C7—C2124.9 (4)N14—C50—H50B109.6
N1—C7—H7117.5C49—C50—H50B109.6
C2—C7—H7117.5H50A—C50—H50B108.1
C4—C8—H8A109.5N14—C51—C52109.6 (4)
C4—C8—H8B109.5N14—C51—H51A109.7
H8A—C8—H8B109.5C52—C51—H51A109.7
C4—C8—H8C109.5N14—C51—H51B109.7
H8A—C8—H8C109.5C52—C51—H51B109.7
H8B—C8—H8C109.5H51A—C51—H51B108.2
N2—C9—C6126.7 (5)N13—C52—C51109.2 (4)
N2—C9—H9116.7N13—C52—H52A109.8
C6—C9—H9116.7C51—C52—H52A109.8
O2—C10—C11122.2 (2)N13—C52—H52B109.8
O2—C10—C15117.6 (2)C51—C52—H52B109.8
C11—C10—C15120.0H52A—C52—H52B108.3
C12—C11—C10120.0O2—Dy1—O196.09 (15)
C12—C11—C16115.1 (3)O2—Dy1—O7124.77 (15)
C10—C11—C16124.9 (3)O1—Dy1—O777.37 (13)
C11—C12—C13120.0O2—Dy1—O482.30 (14)
C11—C12—H12120.0O1—Dy1—O4121.63 (12)
C13—C12—H12120.0O7—Dy1—O4147.27 (13)
C12—C13—C14120.0O2—Dy1—O370.77 (14)
C12—C13—C17121.7 (3)O1—Dy1—O374.58 (13)
C14—C13—C17118.3 (3)O7—Dy1—O3149.38 (13)
C15—C14—C13120.0O4—Dy1—O349.67 (12)
C15—C14—H14120.0O2—Dy1—N472.73 (14)
C13—C14—H14120.0O1—Dy1—N4145.61 (14)
C14—C15—C10120.0O7—Dy1—N482.75 (14)
C14—C15—C18119.4 (3)O4—Dy1—N489.71 (13)
C10—C15—C18120.6 (3)O3—Dy1—N4127.77 (14)
N4—C16—C11126.8 (5)O2—Dy1—N3130.87 (14)
N4—C16—H16116.6O1—Dy1—N3133.02 (14)
C11—C16—H16116.6O7—Dy1—N374.39 (13)
C13—C17—H17A109.5O4—Dy1—N373.54 (12)
C13—C17—H17B109.5O3—Dy1—N3117.53 (13)
H17A—C17—H17B109.5N4—Dy1—N365.19 (14)
C13—C17—H17C109.5O2—Dy1—N2149.91 (14)
H17A—C17—H17C109.5O1—Dy1—N271.76 (14)
H17B—C17—H17C109.5O7—Dy1—N280.41 (14)
N5—C18—N6100.7 (4)O4—Dy1—N281.32 (12)
N5—C18—C15112.2 (4)O3—Dy1—N279.39 (14)
N6—C18—C15111.9 (3)N4—Dy1—N2132.06 (15)
N5—C18—H18110.5N3—Dy1—N267.11 (14)
N6—C18—H18110.5O2—Dy1—O675.76 (14)
C15—C18—H18110.5O1—Dy1—O670.35 (12)
N1—C19—C20111.3 (4)O7—Dy1—O650.09 (13)
N1—C19—H19A109.4O4—Dy1—O6156.28 (13)
C20—C19—H19A109.4O3—Dy1—O6127.74 (12)
N1—C19—H19B109.4N4—Dy1—O675.35 (13)
C20—C19—H19B109.4N3—Dy1—O6114.73 (12)
H19A—C19—H19B108.0N2—Dy1—O6122.36 (12)
N6—C20—C19109.7 (5)O10—Dy2—O998.05 (12)
N6—C20—H20A109.7O10—Dy2—O14125.75 (11)
C19—C20—H20A109.7O9—Dy2—O1474.94 (12)
N6—C20—H20B109.7O10—Dy2—O1283.54 (12)
C19—C20—H20B109.7O9—Dy2—O12119.82 (12)
H20A—C20—H20B108.2O14—Dy2—O12147.03 (10)
N6—C21—C22100.6 (4)O10—Dy2—O1576.39 (12)
N6—C21—H21A111.7O9—Dy2—O1569.21 (12)
C22—C21—H21A111.7O14—Dy2—O1550.44 (10)
N6—C21—H21B111.7O12—Dy2—O15159.19 (11)
C22—C21—H21B111.7O10—Dy2—N9149.36 (14)
H21A—C21—H21B109.4O9—Dy2—N971.61 (13)
C21—C22—N5103.5 (3)O14—Dy2—N980.44 (13)
C21—C22—H22A111.1O12—Dy2—N977.60 (13)
N5—C22—H22A111.1O15—Dy2—N9122.92 (13)
C21—C22—H22B111.1O10—Dy2—N1371.20 (14)
N5—C22—H22B111.1O9—Dy2—N13145.54 (13)
H22A—C22—H22B109.0O14—Dy2—N1385.04 (13)
C24—C23—N4110.8 (4)O12—Dy2—N1392.10 (13)
C24—C23—H23A109.5O15—Dy2—N1376.39 (13)
N4—C23—H23A109.5N9—Dy2—N13132.80 (15)
C24—C23—H23B109.5O10—Dy2—O1172.68 (13)
N4—C23—H23B109.5O9—Dy2—O1173.55 (12)
H23A—C23—H23B108.1O14—Dy2—O11145.53 (12)
C23—C24—N3109.5 (4)O12—Dy2—O1149.39 (12)
C23—C24—H24A109.8O15—Dy2—O11126.79 (12)
N3—C24—H24A109.8N9—Dy2—O1176.71 (14)
C23—C24—H24B109.8N13—Dy2—O11129.33 (14)
N3—C24—H24B109.8O10—Dy2—N14129.84 (13)
H24A—C24—H24B108.2O9—Dy2—N14132.09 (13)
N3—C25—C26109.5 (4)O14—Dy2—N1475.68 (11)
N3—C25—H25A109.8O12—Dy2—N1473.20 (11)
C26—C25—H25A109.8O15—Dy2—N14116.04 (12)
N3—C25—H25B109.8N9—Dy2—N1466.83 (14)
C26—C25—H25B109.8N13—Dy2—N1466.10 (14)
H25A—C25—H25B108.2O11—Dy2—N14117.08 (12)
N2—C26—C25106.7 (4)C7—N1—C19121.9 (3)
N2—C26—H26A110.4C7—N1—H1A119.1
C25—C26—H26A110.4C19—N1—H1A119.0
N2—C26—H26B110.4C9—N2—C26117.1 (4)
C25—C26—H26B110.4C9—N2—Dy1130.9 (3)
H26A—C26—H26B108.6C26—N2—Dy1111.7 (3)
O9—C27—C28123.0 (4)C25—N3—C24112.7 (3)
O9—C27—C32118.8 (4)C25—N3—Dy1111.6 (2)
C28—C27—C32118.1 (5)C24—N3—Dy1110.0 (2)
C27—C28—C29121.3 (5)C25—N3—H3A107.4
C27—C28—C33123.0 (5)C24—N3—H3A107.4
C29—C28—C33115.7 (4)Dy1—N3—H3A107.4
C30—C29—C28121.0 (4)C16—N4—C23115.4 (3)
C30—C29—H29119.5C16—N4—Dy1127.2 (3)
C28—C29—H29119.5C23—N4—Dy1117.3 (2)
C29—C30—C31118.8 (5)C18—N5—C22104.1 (3)
C29—C30—C34121.4 (4)C18—N5—H5A110.9
C31—C30—C34119.8 (5)C22—N5—H5A110.9
C30—C31—C32120.4 (5)C18—N5—H5B110.9
C30—C31—H31119.8C22—N5—H5B110.9
C32—C31—H31119.8H5A—N5—H5B108.9
C35—C32—C27124.1 (5)C20—N6—C21113.7 (3)
C35—C32—C31115.5 (5)C20—N6—C18115.4 (3)
C27—C32—C31120.4 (5)C21—N6—C18101.1 (3)
N9—C33—C28128.5 (4)O5—N7—O4123.9 (5)
N9—C33—H33115.7O5—N7—O3118.9 (5)
C28—C33—H33115.7O4—N7—O3117.2 (4)
C30—C34—H34A109.5O8—N8—O7125.0 (5)
C30—C34—H34B109.5O8—N8—O6118.0 (5)
H34A—C34—H34B109.5O7—N8—O6116.8 (4)
C30—C34—H34C109.5C33—N9—C49116.4 (4)
H34A—C34—H34C109.5C33—N9—Dy2129.3 (3)
H34B—C34—H34C109.5C49—N9—Dy2114.2 (3)
N10—C35—C32123.4 (4)C35—N10—C48122.3 (4)
N10—C35—H35118.3C35—N10—H10A118.7
C32—C35—H35118.3C48—N10—H10A119.0
O10—C36—C37123.3 (5)C44—N11—C47113.7 (4)
O10—C36—C41119.8 (4)C44—N11—C46104.9 (4)
C37—C36—C41116.8 (5)C47—N11—C46115.4 (4)
C42—C37—C36123.2 (4)C44—N12—C4599.6 (4)
C42—C37—C38118.5 (5)C44—N12—H12A111.8
C36—C37—C38118.3 (5)C45—N12—H12A111.8
C39—C38—C37121.9 (6)C44—N12—H12B111.8
C39—C38—H38119.0C45—N12—H12B111.8
C37—C38—H38119.0H12A—N12—H12B109.6
C38—C39—C40119.9 (5)C42—N13—C52115.2 (5)
C38—C39—C43115.6 (5)C42—N13—Dy2126.2 (4)
C40—C39—C43124.4 (5)C52—N13—Dy2118.2 (3)
C41—C40—C39120.1 (5)C50—N14—C51114.0 (4)
C41—C40—H40119.9C50—N14—Dy2114.4 (3)
C39—C40—H40119.9C51—N14—Dy2108.1 (3)
C40—C41—C36122.7 (4)C50—N14—H14A106.6
C40—C41—C44116.9 (4)C51—N14—H14A106.6
C36—C41—C44120.3 (4)Dy2—N14—H14A106.6
N13—C42—C37127.9 (4)O12—N15—O13122.0 (4)
N13—C42—H42A116.1O12—N15—O11117.0 (4)
C37—C42—H42A116.1O13—N15—O11121.0 (5)
C39—C43—H43A109.5O16—N16—O15120.7 (4)
C39—C43—H43B109.5O16—N16—O14120.0 (4)
H43A—C43—H43B109.5O15—N16—O14119.4 (4)
C39—C43—H43C109.5O18—N17—O17115.5 (5)
H43A—C43—H43C109.5O18—N17—O19117.9 (4)
H43B—C43—H43C109.5O17—N17—O19126.3 (5)
N11—C44—C41116.3 (5)O20—N18—O21115.5 (5)
N11—C44—N12100.6 (4)O20—N18—O22128.0 (5)
C41—C44—N12107.4 (4)O21—N18—O22116.4 (5)
N11—C44—H44110.7C1—O1—Dy1143.9 (2)
C41—C44—H44110.7C10—O2—Dy1133.4 (2)
N12—C44—H44110.7N7—O3—Dy194.4 (3)
C46—C45—N12102.9 (4)N7—O4—Dy197.7 (3)
C46—C45—H45A111.2N8—O6—Dy193.0 (3)
N12—C45—H45A111.2N8—O7—Dy199.0 (3)
C46—C45—H45B111.2C27—O9—Dy2144.3 (2)
N12—C45—H45B111.2C36—O10—Dy2134.5 (3)
H45A—C45—H45B109.1N15—O11—Dy295.6 (3)
N11—C46—C45103.9 (4)N15—O12—Dy298.0 (3)
N11—C46—H46A111.0N16—O14—Dy293.6 (2)
C45—C46—H46A111.0N16—O15—Dy292.4 (3)
N11—C46—H46B111.0H23D—O23—H23E109.5
C45—C46—H46B111.0H24C—O24—H24E109.5
H46A—C46—H46B109.0H25D—O25—H25E109.5
N11—C47—C48112.1 (4)H26E—O26—H26D107.3
N11—C47—H47A109.2H27C—O27—H27A109.8
C48—C47—H47A109.2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N14—H14A···O200.912.233.118 (6)166
N12—H12B···O100.901.992.696 (6)134
N12—H12A···N170.902.503.332 (7)155
N12—H12A···O170.902.342.972 (7)127
N12—H12A···O180.901.912.786 (6)164
N5—H5B···O20.901.972.684 (6)135
N5—H5A···N180.902.453.348 (7)177
N5—H5A···O210.902.213.015 (7)149
N5—H5A···O200.901.962.809 (6)156
N1—H1A···O10.861.982.610 (5)130
N10—H10A···O90.861.992.620 (5)129
N3—H3A···O17i0.912.183.008 (5)151
Symmetry codes: (i) x+1, y+1, z.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N14—H14A···O200.912.233.118 (6)166
N12—H12B···O100.901.992.696 (6)134
N12—H12A···N170.902.503.332 (7)155
N12—H12A···O170.902.342.972 (7)127
N12—H12A···O180.901.912.786 (6)164
N5—H5B···O20.901.972.684 (6)135
N5—H5A···N180.902.453.348 (7)177
N5—H5A···O210.902.213.015 (7)149
N5—H5A···O200.901.962.809 (6)156
N1—H1A···O10.861.982.610 (5)130
N10—H10A···O90.861.992.620 (5)129
N3—H3A···O17i0.912.183.008 (5)151
Symmetry codes: (i) x+1, y+1, z.
references
References top

Bruker (2000). SMART (Version ?), SAINT (Version ?), SADABS (Version ?) and SHELXTL (Version 6.10). Bruker AXS Inc., Madison, Wisconsin, USA.

Bunzli, J.-C. G. & Piguet, C. (2002). Chem. Rev. 102, 1897–1928.

Hu, X.-L., Chen, Z., Qiu, L. & Pan, Z.-Q. (2007). Acta Cryst. E63, m1668–m1669.

Hu, X.-L., Liu, H., Hu, D., Yuan, J., Chen, Z., Huang, Q.-M. & Pan, Z.-Q. (2005). J. Rare Earths, 23(s1), 543–547.

Hu, X.-L., Qiu, L., Yuan, J. & Pan, Z.-Q. (2007). Acta Cryst. E63, m1438–?.