supplementary materials


su2704 scheme

Acta Cryst. (2014). E70, m162-m163    [ doi:10.1107/S1600536814006060 ]

Bis[2,6-bis­(1H-pyrazol-1-yl)pyridine]­deca­kis­([mu]2-3-nitro­benzoato)bis­(3-nitro­benzoato)tetra­dysprosium(III): a linear tetra­nuclear dysprosium compound based on mixed N- and O-donor ligands

R. Hua, X.-L. Wu and J.-Y. Li

CCDC reference: 992494

Abstract top

The title compound, [Dy4(C7H4NO4)12(C11H9N5)2] or Dy4(L1)12(L2)2, where HL1 = 3-nitro­benzoic acid and HL2 = 2,6-bis­(1H-pyrazol-1-y1)pyridine, is a linear tetra­nuclear complex possessing inversion symmetry. The two central inversion-related DyIII atoms are seven-coordinate, DyO7, with a monocapped triangular-prismatic geometry. The outer two DyIII atoms are eight-coordinate, DyO5N3, with a bicapped triangular-prismatic geometry. The outer adjacent DyIII atoms are bridged by three L1- carboxyl­ate groups, while the inner inversion-related DyIII atoms are bridged by four L1- carboxyl­ate groups. The L2 ligands are terminally coordinated to the outer DyIII atoms in a tridentate manner. In the crystal, mol­ecules are linked via C-H...O hydrogen bonds, forming a two-dimensional network parallel to (001). Two carboxyl­ate O atoms, and N and O atoms of three nitro groups, are disordered over two positions, with a refined occupancy ratio of 0.552 (6):0.448 (6).

Comment top

Single molecule magnets (SMMs) have potential applications in data storage, quantum information processing (Zheng et al., 2008), magnetic refrigeration, and high-density information storage (Wu et al., 2009).SMMs are mononuclear or multinuclear transition metal-based clusters or rare-earth metal-based clusters with no interactions between molecules. MnII-based SMMs were the first to be fully investigated, whereas recently 4f- or 5f-based compounds, especially DyIII-based compounds, have been investigated because of their potential significant magnetic anisotropy and large energy barriers (Guo et al., 2012). A number of multinuclear Dy-based compounds have been synthesized, for example, Dy2 (Xu et al., 2010), Dy3 (Hussain et al., 2009), Dy4 (Abbas et al., 2010), Dy5 (Blagg et al., 2011), and Dy8 (Tian et al., 2012). In line with our interest in designing multinuclear Dy-based compounds, we report herein on the synthesis and crystal structure of a new and novel linear tetranuclear dysprosium compound, which is based on mixed N-donor and O-donor ligands.

The molecular structure of the title compound is illustrated in Fig. 1. It possesses inversion symmetry and the asymmetric unit is composed of two crystallographic independent DyIII ions, six crystallographic independent 3-nitro benzoate L1- ligands, and one crystallographic independent 2,6-di(1H-pyrazol-1-y1)pyridine L2 ligand. The coordination spheres of the two DyIII ion are different. Atom Dy1 has a DyO5N3 bi-capped triangular-prism geometry, completed by three nitrogen atoms (N1, N3, N5) from one L2 ligand, and five oxygen atoms (O1, O2, O5, O9, O13) from three L1- ligands, where the capped atoms are N5, O9. Atom Dy2 has a DyO7 monocapped triangular-prism geometry, created by seven oxygen atoms (O6, O10, O14, O17, O18, O21, O22) from seven L1- ligands, where the capped atom is O10. The Dy—O/N bond length are in the normal range. The L2 ligand coordinates to the Dy1 atoms in a tridentate manner, whereas the L1- ligands display two kinds of coordination mode, chelate and bidentate. The chelate mode involves the outer pair of Dy atoms, while the bidentate mode involves the inversion related Dy2 atoms in the center of the tetranuclear complex.

The overall structure of the title compound is a tetranuclear cluster in the Dy1—Dy2—Dy2A—Dy1A arrangement, see Figs. 1, 2, and 3. Atoms Dy1 and Dy2 are bridged by three L1- carboxylate ligands with a metal-to-metal distance of 4.88 (2) Å. Through inversion symmetry the Dy1—Dy2 fragment connects to the symmetry-related Dy2A···Dy1A fragment via the Dy2—Dy2A connection linked by four L1- carboxyl groups. The Dy2···Dy2A distance is 4.34 (2) Å. The span of this tetranuclear cluster estimated by the distance of two terminal metal ions Dy1 and Dy1A is 14.07 (2) Å [symmetry code: A = -x, -y+1, -z].

In the crystal, molecules are linked via C-H···O hydrogen bonds forming a two-dimensional network parallel to (001); see Table 1 and Fig. 4.

Although the ligand 2,6-di(1H-pyrazol-1-y1) pyridine is extensively used to construct metal-organic compounds, it has rarely been used in combination with lanthanide ions, and there is no precedent of a cluster compound containing a lanthanide ion and the ligand 2,6-di(1H-pyrazol-1-y1)pyridine. The title compound is the first such compound to be synthesized and is a promising way to target multinuclear lanthanide clusters.

Moreover, in the literature, there is only one other report of a linear tetranuclear DyIII complex (Lin et al., 2012), [Dy4(L)2(C6H5COO)12(MeOH)4] (L = 2,6-bis((furan-2-ylmethylimino)methyl)-4-methyl-phenol), where the DyIII sites are fully coordinated by O atoms, rather than being coordinated by both O and N atoms as observed in the title compound. Interestingly the metal-to-metal distances (4.24 (2) Å and 4.06 (2) Å) reported there are slightly shorter than those observed in the title compound.

Related literature top

For background to single molecular magnets, see: Zheng et al. (2008); Wu et al. (2009); Guo et al. (2012). For examples of multinuclear Dy-based compounds, see: Abbas et al. (2010); Blagg et al. (2011); Hussain et al. (2009); Tian et al. (2012); Xu et al. (2010). For details of a linear tetranuclear DyIII complex, see: Lin et al. (2012).

Experimental top

DyCl3 (0.2 mmol), 2,6-di(1H-pyrazol-1-y1)pyridine (2 mmol), nitro benzoic acid (0.8 mmol), Na2CO3 (0.4 mmol) and H2O (10 mL) were mixed together, then transferred into a 25 ml Teflon-lined reactor. This was heated at 483 K for 3 days. The mixture was then cooled to room temperature, at a rate of 3 K/h, and yielded block-like colourles crystals in a 58% yield based on Dy.

Refinement top

The NH H atoms could be located in a difference Fourier map. The C and N-bound H atoms were included in calculated positions and treated as riding: N-H = 0.86 Å, C—H = 0.93 – 0.97 Å with Uiso(H) = 1.2Ueq(N/C). Two O atoms of carboxyl groups (O10/O10' and O14/O14') and atoms in three nitro groups

(N10/N10', O19/O19', O20/O20', N11/N11', O23/O23', O24/O24' and O16/O16') are disordered over two positions with a refined occupancy ratio of 0.448 (6):0.552 (6).

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: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The coordination environment of the DyIII ions in the title compound, with atom labelling of heteroatoms only. Displacement ellipsoids are drawn at the 50% probability level [H atoms have been omitted for clarity; Dy/pink, C/bright green, N/blue, O/red; symmetry code: A = -x, -y+1, -z].
[Figure 2] Fig. 2. A view of the simplified tetranuclear structure of the title compound.
[Figure 3] Fig. 3. The polyhedral view of the tetranuclear structure of the title compound.
[Figure 4] Fig. 4. A view along the b axis of the crystal packing of the title compound [Dy/pink, C/bright green, N/blue, O/red].
Bis[2,6-bis(1H-pyrazol-1-yl)pyridine]decakis(µ2-3-nitrobenzoato)bis(3-nitrobenzoato)tetradysprosium(III) top
Crystal data top
[Dy4(C7H4NO4)12(C11H9N5)2]Z = 1
Mr = 3065.81F(000) = 1504
Triclinic, P1Dx = 1.812 Mg m3
a = 14.2514 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 14.9274 (5) ÅCell parameters from 9289 reflections
c = 14.9616 (3) Åθ = 2.6–27.7°
α = 100.443 (2)°µ = 2.74 mm1
β = 111.754 (1)°T = 296 K
γ = 99.695 (2)°Block, colourless
V = 2808.87 (12) Å30.20 × 0.20 × 0.19 mm
Data collection top
Bruker APEX2 CCD area-detector
diffractometer
11020 independent reflections
Radiation source: fine-focus sealed tube9747 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
phi and ω scansθmax = 26.0°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1717
Tmin = 0.611, Tmax = 0.624k = 1818
42971 measured reflectionsl = 1818
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) = 0.058H-atom parameters constrained
S = 1.13 w = 1/[σ2(Fo2) + (0.0235P)2 + 2.1975P]
where P = (Fo2 + 2Fc2)/3
11020 reflections(Δ/σ)max = 0.004
848 parametersΔρmax = 0.66 e Å3
24 restraintsΔρmin = 0.67 e Å3
Crystal data top
[Dy4(C7H4NO4)12(C11H9N5)2]γ = 99.695 (2)°
Mr = 3065.81V = 2808.87 (12) Å3
Triclinic, P1Z = 1
a = 14.2514 (3) ÅMo Kα radiation
b = 14.9274 (5) ŵ = 2.74 mm1
c = 14.9616 (3) ÅT = 296 K
α = 100.443 (2)°0.20 × 0.20 × 0.19 mm
β = 111.754 (1)°
Data collection top
Bruker APEX2 CCD area-detector
diffractometer
11020 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
9747 reflections with I > 2σ(I)
Tmin = 0.611, Tmax = 0.624Rint = 0.025
42971 measured reflectionsθmax = 26.0°
Refinement top
R[F2 > 2σ(F2)] = 0.022H-atom parameters constrained
wR(F2) = 0.058Δρmax = 0.66 e Å3
S = 1.13Δρmin = 0.67 e Å3
11020 reflectionsAbsolute structure: ?
848 parametersAbsolute structure parameter: ?
24 restraintsRogers parameter: ?
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

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 > 2sigma(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)
Dy10.28833 (1)0.97110 (1)0.24389 (1)0.0340 (1)
Dy20.08445 (1)0.64772 (1)0.06388 (1)0.0293 (1)
O10.40358 (19)1.09572 (16)0.2241 (2)0.0577 (9)
O20.47835 (18)1.01655 (16)0.32745 (18)0.0527 (8)
O30.9290 (2)1.0903 (3)0.3411 (3)0.0988 (15)
O40.8535 (3)1.0435 (3)0.4309 (3)0.0911 (16)
O50.12405 (17)0.91358 (14)0.23748 (18)0.0488 (7)
O60.04254 (16)0.78523 (13)0.11067 (16)0.0395 (7)
O70.3214 (3)0.5943 (3)0.1974 (3)0.1315 (19)
O80.2587 (2)0.5695 (2)0.0899 (3)0.0816 (11)
O90.31791 (19)0.85744 (14)0.32943 (17)0.0510 (8)
O100.2210 (13)0.7314 (10)0.2201 (14)0.052 (3)0.552 (6)
O110.2006 (12)0.4349 (6)0.3129 (7)0.108 (4)0.552 (6)
O120.3409 (4)0.4208 (3)0.4299 (4)0.138 (2)
O130.32544 (18)0.87284 (14)0.13393 (18)0.0486 (7)
O140.2068 (17)0.7471 (12)0.0279 (17)0.042 (3)0.552 (6)
O150.7221 (3)0.8169 (3)0.0730 (4)0.121 (2)
O160.6931 (6)0.9069 (6)0.1817 (8)0.118 (3)0.552 (6)
O170.02219 (19)0.43184 (17)0.15496 (19)0.0551 (8)
O180.0549 (2)0.58560 (17)0.10098 (17)0.0579 (8)
O190.093 (5)0.274 (3)0.499 (4)0.124 (9)0.552 (6)
O200.002 (3)0.310 (3)0.564 (3)0.131 (10)0.552 (6)
O210.1757 (2)0.53620 (17)0.0789 (2)0.0587 (9)
O220.09576 (17)0.38329 (17)0.02968 (18)0.0543 (8)
O230.5378 (9)0.6545 (7)0.2803 (8)0.097 (3)0.552 (6)
O240.6252 (6)0.5694 (7)0.3608 (7)0.096 (2)0.552 (6)
N10.3146 (3)1.06292 (18)0.4102 (2)0.0534 (10)
N20.2726 (3)1.13707 (19)0.4196 (3)0.0622 (11)
N30.2018 (2)1.10703 (16)0.2480 (2)0.0447 (9)
N40.1392 (2)1.06919 (19)0.0772 (2)0.0512 (9)
N50.1847 (2)0.9962 (2)0.0805 (2)0.0485 (9)
N60.8551 (3)1.0784 (3)0.3639 (3)0.0704 (14)
N70.2562 (2)0.6148 (2)0.1655 (3)0.0654 (13)
N80.2854 (5)0.4694 (3)0.3926 (5)0.101 (2)
N90.6611 (3)0.8432 (3)0.1008 (4)0.110 (2)
N100.030 (5)0.329 (5)0.505 (2)0.087 (9)0.552 (6)
N110.5474 (8)0.5820 (7)0.2990 (9)0.065 (3)0.552 (6)
C10.4830 (3)1.0713 (2)0.2735 (2)0.0456 (10)
C20.5837 (3)1.1049 (2)0.2650 (3)0.0485 (10)
C30.6724 (3)1.0806 (2)0.3206 (3)0.0491 (11)
C40.7627 (3)1.1081 (2)0.3079 (3)0.0557 (11)
C50.7681 (4)1.1602 (3)0.2423 (3)0.0727 (17)
C60.6801 (4)1.1851 (4)0.1880 (4)0.0850 (17)
C70.5876 (3)1.1573 (3)0.1984 (3)0.0684 (14)
C80.0542 (2)0.83835 (19)0.1921 (2)0.0368 (9)
C90.0221 (2)0.8101 (2)0.2355 (2)0.0398 (9)
C100.1026 (2)0.7295 (2)0.1832 (2)0.0413 (10)
C110.1725 (3)0.7025 (2)0.2226 (3)0.0513 (11)
C120.1656 (4)0.7535 (3)0.3120 (3)0.0702 (17)
C130.0863 (4)0.8335 (3)0.3631 (3)0.0757 (17)
C140.0138 (3)0.8627 (3)0.3259 (3)0.0596 (14)
C150.2815 (2)0.7701 (2)0.3055 (2)0.0427 (9)
C160.3276 (2)0.7174 (2)0.3800 (2)0.0411 (9)
C170.2849 (3)0.6216 (2)0.3564 (3)0.0490 (11)
C180.3326 (4)0.5723 (2)0.4209 (3)0.0654 (13)
C190.4211 (5)0.6131 (3)0.5060 (4)0.091 (2)
C200.4609 (4)0.7092 (4)0.5317 (3)0.0933 (19)
C210.4127 (3)0.7618 (3)0.4685 (3)0.0651 (13)
C220.3011 (2)0.7914 (2)0.0792 (2)0.0404 (10)
C230.3859 (2)0.7554 (2)0.0603 (2)0.0392 (9)
C240.4835 (3)0.8154 (2)0.0919 (3)0.0534 (11)
C250.5576 (3)0.7806 (3)0.0687 (3)0.0627 (14)
C260.5394 (3)0.6899 (3)0.0168 (3)0.0631 (14)
C270.4431 (3)0.6301 (3)0.0120 (3)0.0621 (13)
C280.3669 (3)0.6623 (2)0.0094 (3)0.0500 (11)
C290.0260 (2)0.5067 (2)0.1618 (2)0.0413 (10)
C300.0528 (2)0.5006 (2)0.2499 (2)0.0413 (10)
C310.0034 (3)0.4220 (2)0.3311 (3)0.0508 (11)
C320.0345 (4)0.4164 (3)0.4083 (3)0.0675 (16)
C330.1132 (4)0.4829 (4)0.4071 (4)0.084 (2)
C340.1607 (4)0.5611 (4)0.3273 (4)0.086 (2)
C350.1301 (3)0.5707 (3)0.2492 (3)0.0609 (12)
C360.1746 (2)0.4516 (2)0.0751 (2)0.0399 (9)
C370.2766 (2)0.4314 (2)0.1309 (2)0.0368 (9)
C380.3648 (3)0.5048 (2)0.1863 (2)0.0483 (10)
C390.4567 (3)0.4834 (4)0.2389 (3)0.0678 (16)
C400.4638 (4)0.3935 (5)0.2368 (4)0.086 (2)
C410.3769 (4)0.3214 (4)0.1822 (4)0.0787 (17)
C420.2830 (3)0.3397 (2)0.1286 (3)0.0535 (11)
C430.3712 (4)1.0616 (3)0.5023 (3)0.0725 (14)
C440.3677 (6)1.1353 (4)0.5717 (4)0.105 (2)
C450.3065 (5)1.1821 (3)0.5178 (4)0.097 (2)
C460.2056 (3)1.1571 (2)0.3338 (3)0.0560 (13)
C470.1488 (4)1.2217 (3)0.3384 (5)0.084 (2)
C480.0890 (4)1.2382 (3)0.2532 (6)0.096 (2)
C490.0825 (3)1.1894 (3)0.1616 (4)0.0776 (16)
C500.1413 (3)1.1238 (2)0.1650 (3)0.0510 (13)
C510.0960 (3)1.0761 (3)0.0173 (3)0.0741 (16)
C520.1132 (3)1.0081 (3)0.0761 (3)0.0746 (16)
C530.1689 (3)0.9601 (3)0.0123 (3)0.0605 (12)
O20'0.038 (4)0.335 (4)0.545 (3)0.131 (10)0.448 (6)
O23'0.5492 (14)0.6242 (11)0.3178 (12)0.097 (3)0.448 (6)
O10'0.1998 (17)0.7139 (14)0.2273 (18)0.052 (3)0.448 (6)
O11'0.1934 (14)0.4500 (8)0.3720 (15)0.126 (7)0.448 (6)
O14'0.214 (2)0.7289 (15)0.042 (2)0.042 (3)0.448 (6)
O16'0.6648 (8)0.9344 (7)0.1136 (10)0.118 (3)0.448 (6)
O19'0.108 (7)0.296 (3)0.508 (5)0.124 (9)0.448 (6)
N10'0.007 (6)0.337 (6)0.483 (3)0.087 (9)0.448 (6)
N11'0.5531 (11)0.5397 (8)0.3049 (11)0.065 (3)0.448 (6)
O24'0.6316 (8)0.5128 (8)0.3434 (9)0.096 (2)0.448 (6)
H30.671101.046000.366100.0590*
H50.830001.178300.234900.0870*
H240.498800.877700.127800.0640*
H260.590900.669100.001500.0750*
H270.429100.567500.046200.0740*
H280.301800.621100.010600.0600*
H310.049400.374300.333300.0610*
H330.134200.475500.459200.1010*
H340.213800.608000.325600.1040*
H350.161800.624600.195900.0730*
H380.362300.566900.188200.0580*
H400.527300.381500.272300.1040*
H410.380600.259600.180700.0940*
H420.223800.289900.091000.0640*
H430.408601.017100.518700.0870*
H440.400901.149100.640900.1260*
H450.290001.236000.543000.1160*
H470.151601.253500.399200.1010*
H480.051101.283000.255200.1150*
H490.041201.200100.101800.0930*
H510.060301.120500.038000.0890*
H520.092500.995700.144800.0890*
H530.192100.908900.032800.0730*
H60.682401.221000.143700.1020*
H70.528101.173900.160600.0820*
H100.109500.694000.122200.0500*
H120.214000.734000.337100.0850*
H130.080700.868900.423600.0910*
H140.040100.917300.361400.0720*
H170.225100.591300.298300.0590*
H190.454000.576800.545900.1100*
H200.519600.739100.590900.1110*
H210.438400.827000.486400.0780*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Dy10.0390 (1)0.0263 (1)0.0321 (1)0.0088 (1)0.0106 (1)0.0058 (1)
Dy20.0289 (1)0.0241 (1)0.0308 (1)0.0085 (1)0.0087 (1)0.0040 (1)
O10.0515 (14)0.0458 (13)0.0725 (18)0.0122 (11)0.0169 (13)0.0270 (12)
O20.0466 (13)0.0539 (13)0.0456 (14)0.0027 (10)0.0076 (11)0.0193 (11)
O30.0574 (19)0.103 (3)0.130 (3)0.0175 (17)0.041 (2)0.015 (2)
O40.074 (2)0.104 (3)0.089 (3)0.0355 (19)0.0183 (19)0.033 (2)
O50.0477 (13)0.0326 (10)0.0584 (15)0.0039 (9)0.0203 (12)0.0038 (10)
O60.0451 (12)0.0308 (9)0.0488 (13)0.0148 (9)0.0252 (10)0.0081 (9)
O70.107 (3)0.140 (3)0.144 (4)0.031 (2)0.093 (3)0.001 (3)
O80.076 (2)0.0680 (18)0.089 (2)0.0116 (15)0.0469 (19)0.0062 (16)
O90.0629 (15)0.0348 (11)0.0460 (13)0.0095 (10)0.0117 (12)0.0154 (10)
O100.050 (6)0.032 (5)0.044 (3)0.014 (4)0.003 (3)0.014 (3)
O110.151 (9)0.039 (3)0.101 (7)0.004 (4)0.031 (6)0.016 (4)
O120.202 (5)0.060 (2)0.152 (4)0.054 (3)0.053 (4)0.051 (2)
O130.0517 (13)0.0397 (11)0.0555 (14)0.0112 (10)0.0279 (12)0.0031 (10)
O140.043 (3)0.029 (6)0.061 (6)0.011 (4)0.026 (4)0.019 (3)
O150.061 (2)0.099 (3)0.204 (5)0.0131 (18)0.072 (3)0.016 (3)
O160.067 (4)0.085 (4)0.165 (7)0.007 (3)0.049 (5)0.029 (4)
O170.0608 (15)0.0584 (14)0.0568 (15)0.0169 (12)0.0302 (13)0.0261 (12)
O180.0690 (16)0.0609 (15)0.0369 (13)0.0142 (12)0.0218 (12)0.0002 (11)
O190.172 (18)0.076 (16)0.078 (9)0.023 (12)0.026 (10)0.021 (11)
O200.16 (2)0.151 (19)0.059 (12)0.058 (15)0.041 (13)0.035 (8)
O210.0644 (16)0.0552 (14)0.0718 (17)0.0395 (12)0.0304 (14)0.0254 (12)
O220.0328 (12)0.0683 (15)0.0464 (14)0.0111 (11)0.0068 (10)0.0016 (12)
O230.074 (3)0.081 (6)0.097 (7)0.011 (4)0.026 (5)0.019 (4)
O240.043 (2)0.137 (6)0.073 (4)0.003 (4)0.000 (2)0.017 (5)
N10.075 (2)0.0376 (14)0.0430 (17)0.0071 (13)0.0259 (15)0.0038 (12)
N20.092 (2)0.0386 (15)0.061 (2)0.0106 (15)0.045 (2)0.0016 (14)
N30.0488 (15)0.0282 (12)0.0622 (18)0.0115 (11)0.0266 (14)0.0144 (12)
N40.0386 (14)0.0497 (15)0.0631 (19)0.0124 (12)0.0111 (14)0.0306 (14)
N50.0460 (15)0.0551 (16)0.0456 (17)0.0200 (13)0.0141 (13)0.0202 (13)
N60.051 (2)0.066 (2)0.077 (3)0.0081 (16)0.0181 (19)0.0032 (19)
N70.0507 (18)0.067 (2)0.083 (3)0.0026 (15)0.0379 (19)0.0202 (18)
N80.146 (5)0.047 (2)0.124 (5)0.027 (3)0.059 (4)0.045 (3)
N90.052 (2)0.078 (3)0.177 (5)0.0016 (19)0.057 (3)0.023 (3)
N100.12 (2)0.097 (10)0.022 (13)0.054 (15)0.007 (13)0.009 (13)
N110.041 (2)0.084 (7)0.052 (3)0.004 (5)0.012 (2)0.006 (5)
C10.0457 (18)0.0337 (15)0.0420 (18)0.0002 (13)0.0094 (15)0.0029 (13)
C20.0490 (19)0.0403 (16)0.0444 (19)0.0012 (14)0.0123 (16)0.0082 (14)
C30.052 (2)0.0444 (17)0.0407 (18)0.0045 (15)0.0127 (16)0.0089 (14)
C40.049 (2)0.0493 (19)0.054 (2)0.0027 (15)0.0149 (17)0.0020 (16)
C50.063 (3)0.077 (3)0.074 (3)0.001 (2)0.032 (2)0.020 (2)
C60.080 (3)0.096 (3)0.082 (3)0.004 (3)0.033 (3)0.049 (3)
C70.062 (2)0.069 (2)0.068 (3)0.007 (2)0.017 (2)0.034 (2)
C80.0401 (16)0.0288 (13)0.0453 (18)0.0153 (12)0.0187 (14)0.0104 (12)
C90.0440 (17)0.0371 (15)0.0420 (17)0.0160 (13)0.0202 (14)0.0086 (13)
C100.0434 (17)0.0414 (15)0.0448 (18)0.0148 (13)0.0234 (15)0.0099 (13)
C110.051 (2)0.0530 (19)0.059 (2)0.0158 (16)0.0315 (18)0.0151 (16)
C120.077 (3)0.076 (3)0.075 (3)0.020 (2)0.052 (3)0.016 (2)
C130.098 (3)0.082 (3)0.059 (3)0.026 (3)0.051 (3)0.004 (2)
C140.073 (3)0.053 (2)0.051 (2)0.0110 (18)0.032 (2)0.0007 (16)
C150.0442 (17)0.0385 (15)0.0344 (17)0.0085 (13)0.0055 (14)0.0093 (13)
C160.0493 (18)0.0332 (14)0.0324 (16)0.0070 (13)0.0096 (14)0.0082 (12)
C170.058 (2)0.0356 (15)0.048 (2)0.0082 (14)0.0183 (17)0.0098 (14)
C180.101 (3)0.0413 (18)0.057 (2)0.021 (2)0.031 (2)0.0216 (17)
C190.136 (5)0.069 (3)0.063 (3)0.044 (3)0.018 (3)0.040 (2)
C200.103 (4)0.084 (3)0.052 (3)0.015 (3)0.010 (3)0.022 (2)
C210.075 (3)0.0438 (18)0.044 (2)0.0058 (17)0.0064 (19)0.0116 (16)
C220.0413 (17)0.0393 (15)0.0431 (18)0.0090 (13)0.0215 (15)0.0093 (13)
C230.0398 (16)0.0387 (15)0.0400 (17)0.0100 (12)0.0181 (14)0.0092 (13)
C240.0422 (18)0.0444 (17)0.062 (2)0.0041 (14)0.0205 (17)0.0045 (16)
C250.0394 (19)0.060 (2)0.080 (3)0.0047 (16)0.0264 (19)0.0022 (19)
C260.052 (2)0.062 (2)0.080 (3)0.0217 (18)0.035 (2)0.007 (2)
C270.062 (2)0.0450 (18)0.080 (3)0.0138 (17)0.037 (2)0.0017 (18)
C280.0507 (19)0.0395 (16)0.060 (2)0.0075 (14)0.0283 (18)0.0056 (15)
C290.0412 (16)0.0485 (17)0.0344 (17)0.0147 (14)0.0146 (14)0.0112 (14)
C300.0480 (18)0.0410 (15)0.0360 (17)0.0133 (13)0.0177 (14)0.0106 (13)
C310.063 (2)0.0459 (17)0.0428 (19)0.0204 (16)0.0194 (17)0.0096 (15)
C320.093 (3)0.075 (3)0.043 (2)0.044 (2)0.030 (2)0.0107 (19)
C330.101 (4)0.120 (4)0.065 (3)0.053 (3)0.057 (3)0.034 (3)
C340.084 (3)0.103 (4)0.090 (4)0.012 (3)0.056 (3)0.036 (3)
C350.064 (2)0.061 (2)0.054 (2)0.0015 (18)0.027 (2)0.0146 (18)
C360.0382 (16)0.0457 (16)0.0357 (16)0.0210 (14)0.0124 (14)0.0075 (13)
C370.0334 (15)0.0376 (14)0.0383 (16)0.0134 (12)0.0131 (13)0.0075 (12)
C380.0411 (17)0.0530 (18)0.0443 (19)0.0070 (14)0.0175 (15)0.0026 (15)
C390.0320 (18)0.119 (4)0.037 (2)0.010 (2)0.0090 (15)0.005 (2)
C400.061 (3)0.157 (5)0.062 (3)0.067 (3)0.024 (2)0.047 (3)
C410.092 (3)0.090 (3)0.093 (3)0.066 (3)0.049 (3)0.053 (3)
C420.058 (2)0.0457 (18)0.068 (2)0.0253 (16)0.0300 (19)0.0217 (17)
C430.102 (3)0.061 (2)0.041 (2)0.003 (2)0.025 (2)0.0086 (18)
C440.172 (6)0.076 (3)0.051 (3)0.001 (4)0.052 (4)0.003 (2)
C450.160 (5)0.062 (3)0.072 (3)0.012 (3)0.073 (4)0.011 (2)
C460.066 (2)0.0283 (15)0.083 (3)0.0068 (15)0.047 (2)0.0066 (16)
C470.090 (3)0.044 (2)0.134 (5)0.025 (2)0.068 (4)0.006 (2)
C480.073 (3)0.042 (2)0.181 (6)0.027 (2)0.063 (4)0.017 (3)
C490.049 (2)0.048 (2)0.137 (4)0.0214 (18)0.029 (3)0.040 (3)
C500.0394 (17)0.0357 (15)0.080 (3)0.0110 (13)0.0233 (18)0.0224 (17)
C510.060 (2)0.073 (3)0.070 (3)0.010 (2)0.002 (2)0.043 (2)
C520.064 (3)0.089 (3)0.050 (2)0.001 (2)0.002 (2)0.034 (2)
C530.056 (2)0.075 (2)0.041 (2)0.0142 (19)0.0110 (17)0.0153 (18)
O20'0.16 (2)0.151 (19)0.059 (12)0.058 (15)0.041 (13)0.035 (8)
O23'0.074 (3)0.081 (6)0.097 (7)0.011 (4)0.026 (5)0.019 (4)
O10'0.050 (6)0.032 (5)0.044 (3)0.014 (4)0.003 (3)0.014 (3)
O11'0.127 (9)0.051 (5)0.213 (17)0.008 (5)0.094 (12)0.026 (8)
O14'0.043 (3)0.029 (6)0.061 (6)0.011 (4)0.026 (4)0.019 (3)
O16'0.067 (4)0.085 (4)0.165 (7)0.007 (3)0.049 (5)0.029 (4)
O19'0.172 (18)0.076 (16)0.078 (9)0.023 (12)0.026 (10)0.021 (11)
N10'0.12 (2)0.097 (10)0.022 (13)0.054 (15)0.007 (13)0.009 (13)
N11'0.041 (2)0.084 (7)0.052 (3)0.004 (5)0.012 (2)0.006 (5)
O24'0.043 (2)0.137 (6)0.073 (4)0.003 (4)0.000 (2)0.017 (5)
Geometric parameters (Å, º) top
Dy1—O12.404 (3)C9—C101.380 (4)
Dy1—O22.433 (3)C9—C141.387 (5)
Dy1—O52.314 (3)C10—C111.374 (5)
Dy1—O92.307 (2)C11—C121.374 (6)
Dy1—O132.274 (3)C12—C131.365 (7)
Dy1—N12.472 (3)C13—C141.389 (7)
Dy1—N32.549 (3)C15—C161.497 (4)
Dy1—N52.478 (3)C16—C171.380 (4)
Dy2—O62.294 (2)C16—C211.373 (5)
Dy2—O102.358 (19)C17—C181.369 (5)
Dy2—O142.38 (2)C18—C191.361 (8)
Dy2—O182.322 (2)C19—C201.375 (8)
Dy2—O212.272 (3)C20—C211.397 (7)
Dy2—O10'2.29 (2)C22—C231.499 (4)
Dy2—O14'2.20 (3)C23—C241.378 (5)
Dy2—O17i2.277 (3)C23—C281.386 (5)
Dy2—O22i2.339 (3)C24—C251.377 (6)
O1—C11.256 (5)C25—C261.362 (6)
O2—C11.259 (4)C26—C271.370 (6)
O3—N61.218 (6)C27—C281.375 (6)
O4—N61.216 (6)C29—C301.494 (4)
O5—C81.249 (4)C30—C311.385 (5)
O6—C81.263 (4)C30—C351.381 (6)
O7—N71.213 (6)C31—C321.376 (7)
O8—N71.193 (5)C32—C331.359 (8)
O9—C151.250 (4)C33—C341.370 (8)
O10—C151.207 (19)C34—C351.384 (7)
O10'—C151.32 (2)C36—C371.497 (4)
O11—N81.283 (14)C37—C421.382 (4)
O11'—N81.20 (2)C37—C381.379 (5)
O12—N81.215 (8)C38—C391.380 (6)
O13—C221.247 (4)C39—C401.358 (9)
O14—C221.26 (2)C40—C411.357 (9)
O14'—C221.28 (3)C41—C421.384 (7)
O15—N91.186 (7)C43—C441.391 (8)
O16—N91.267 (12)C44—C451.337 (9)
O16'—N91.329 (12)C46—C471.368 (7)
O17—C291.251 (4)C47—C481.338 (10)
O18—C291.247 (4)C48—C491.392 (9)
O19—N101.15 (10)C49—C501.388 (6)
O19'—N10'1.34 (13)C51—C521.336 (6)
O20—N101.15 (7)C52—C531.390 (6)
O20'—N10'1.31 (9)C3—H30.9300
O21—C361.251 (4)C5—H50.9300
O22—C361.249 (4)C6—H60.9300
O23—N111.183 (15)C7—H70.9300
O23'—N11'1.26 (2)C10—H100.9300
O24—N111.222 (15)C12—H120.9300
O24'—N11'1.23 (2)C13—H130.9300
N1—C431.320 (5)C14—H140.9300
N1—N21.354 (5)C17—H170.9300
N2—C451.360 (7)C19—H190.9300
N2—C461.406 (6)C20—H200.9300
N3—C461.340 (5)C21—H210.9300
N3—C501.319 (5)C24—H240.9300
N4—C511.348 (5)C26—H260.9300
N4—N51.358 (4)C27—H270.9300
N4—C501.402 (5)C28—H280.9300
N5—C531.313 (5)C31—H310.9300
N6—C41.465 (6)C33—H330.9300
N7—C111.476 (5)C34—H340.9300
N8—C181.482 (6)C35—H350.9300
N9—C251.459 (7)C38—H380.9300
N10—C321.60 (5)C40—H400.9300
N10'—C321.34 (6)C41—H410.9300
N11—C391.632 (13)C42—H420.9300
N11'—C391.369 (16)C43—H430.9300
C1—C21.498 (6)C44—H440.9300
C2—C31.381 (6)C45—H450.9300
C2—C71.385 (6)C47—H470.9300
C3—C41.376 (6)C48—H480.9300
C4—C51.374 (6)C49—H490.9300
C5—C61.372 (8)C51—H510.9300
C6—C71.388 (8)C52—H520.9300
C8—C91.500 (4)C53—H530.9300
O1—Dy1—O253.79 (9)C9—C14—C13119.7 (4)
O1—Dy1—O5146.83 (9)O9—C15—O10118.4 (8)
O1—Dy1—O9132.71 (10)O9—C15—C16117.9 (3)
O1—Dy1—O1385.78 (9)O9—C15—O10'130.9 (10)
O1—Dy1—N192.97 (10)O10—C15—C16123.0 (8)
O1—Dy1—N376.10 (9)O10'—C15—C16110.9 (10)
O1—Dy1—N575.17 (10)C15—C16—C21121.4 (3)
O2—Dy1—O5152.54 (8)C17—C16—C21120.1 (3)
O2—Dy1—O979.08 (9)C15—C16—C17118.5 (3)
O2—Dy1—O1380.33 (9)C16—C17—C18118.3 (4)
O2—Dy1—N179.47 (12)N8—C18—C19120.1 (4)
O2—Dy1—N3115.08 (9)C17—C18—C19123.0 (4)
O2—Dy1—N5124.91 (9)N8—C18—C17116.9 (4)
O5—Dy1—O978.83 (9)C18—C19—C20118.6 (5)
O5—Dy1—O13112.50 (9)C19—C20—C21119.7 (4)
O5—Dy1—N181.09 (11)C16—C21—C20120.1 (4)
O5—Dy1—N372.07 (8)O14'—C22—C23113.0 (13)
O5—Dy1—N582.41 (9)O14—C22—C23120.0 (11)
O9—Dy1—O1382.31 (8)O13—C22—O14121.1 (11)
O9—Dy1—N180.84 (9)O13—C22—C23117.7 (3)
O9—Dy1—N3136.38 (9)O13—C22—O14'129.0 (13)
O9—Dy1—N5143.44 (9)C22—C23—C28120.7 (3)
O13—Dy1—N1155.77 (11)C24—C23—C28119.2 (3)
O13—Dy1—N3138.76 (8)C22—C23—C24120.1 (3)
O13—Dy1—N576.31 (9)C23—C24—C25118.2 (3)
N1—Dy1—N363.33 (10)N9—C25—C24119.0 (4)
N1—Dy1—N5126.76 (10)N9—C25—C26117.7 (4)
N3—Dy1—N563.43 (9)C24—C25—C26123.3 (4)
O6—Dy2—O1074.2 (4)C25—C26—C27118.1 (4)
O6—Dy2—O1483.5 (5)C26—C27—C28120.3 (4)
O6—Dy2—O18120.81 (8)C23—C28—C27120.9 (4)
O6—Dy2—O21157.47 (9)O17—C29—O18125.8 (3)
O6—Dy2—O10'74.9 (6)O17—C29—C30117.0 (3)
O6—Dy2—O14'89.4 (7)O18—C29—C30117.1 (3)
O6—Dy2—O17i96.50 (9)C29—C30—C31119.9 (3)
O6—Dy2—O22i75.08 (9)C29—C30—C35120.5 (3)
O10—Dy2—O1474.4 (7)C31—C30—C35119.5 (3)
O10—Dy2—O18141.0 (5)C30—C31—C32118.2 (4)
O10—Dy2—O2183.4 (4)N10—C32—C33120 (2)
O10—Dy2—O17i84.3 (4)C31—C32—C33123.1 (4)
O10—Dy2—O22i143.1 (5)N10'—C32—C31118 (4)
O14—Dy2—O1872.3 (5)N10'—C32—C33118 (4)
O14—Dy2—O2192.8 (5)N10—C32—C31117 (2)
O14—Dy2—O17i157.9 (6)C32—C33—C34118.4 (5)
O14—Dy2—O22i121.6 (6)C33—C34—C35120.4 (5)
O18—Dy2—O2178.58 (10)C30—C35—C34120.3 (4)
O10'—Dy2—O18149.3 (7)O21—C36—C37116.7 (3)
O14'—Dy2—O1874.0 (7)O21—C36—O22125.6 (3)
O17i—Dy2—O18124.71 (9)O22—C36—C37117.7 (3)
O18—Dy2—O22i73.73 (10)C38—C37—C42119.6 (3)
O10'—Dy2—O2182.6 (6)C36—C37—C38119.9 (3)
O14'—Dy2—O2185.2 (7)C36—C37—C42120.6 (3)
O17i—Dy2—O2178.66 (10)C37—C38—C39118.1 (3)
O21—Dy2—O22i124.61 (9)N11—C39—C40129.1 (6)
O10'—Dy2—O14'80.4 (9)C38—C39—C40122.7 (5)
O10'—Dy2—O17i74.1 (6)N11'—C39—C38131.6 (7)
O10'—Dy2—O22i136.8 (7)N11'—C39—C40105.6 (7)
O14'—Dy2—O17i151.3 (7)N11—C39—C38108.2 (6)
O14'—Dy2—O22i129.3 (7)C39—C40—C41119.0 (6)
O17i—Dy2—O22i79.31 (9)C40—C41—C42120.2 (5)
Dy1—O1—C192.2 (2)C37—C42—C41120.4 (4)
Dy1—O2—C190.7 (2)N1—C43—C44111.2 (5)
Dy1—O5—C8134.5 (2)C43—C44—C45105.4 (5)
Dy2—O6—C8135.76 (19)N2—C45—C44108.0 (5)
Dy1—O9—C15133.2 (2)N2—C46—N3114.3 (3)
Dy2—O10—C15171.1 (14)N2—C46—C47122.4 (4)
Dy2—O10'—C15159.6 (16)N3—C46—C47123.4 (4)
Dy1—O13—C22145.6 (2)C46—C47—C48118.4 (6)
Dy2—O14—C22132.3 (14)C47—C48—C49121.1 (5)
Dy2—O14'—C22148.8 (19)C48—C49—C50115.9 (5)
Dy2i—O17—C29149.3 (2)N3—C50—C49124.2 (4)
Dy2—O18—C29138.4 (2)N4—C50—C49120.9 (4)
Dy2—O21—C36147.8 (2)N3—C50—N4114.9 (3)
Dy2i—O22—C36139.9 (2)N4—C51—C52108.2 (4)
Dy1—N1—N2120.7 (2)C51—C52—C53105.0 (4)
Dy1—N1—C43133.6 (3)N5—C53—C52111.6 (4)
N2—N1—C43105.4 (3)C2—C3—H3120.00
N1—N2—C45109.9 (4)C4—C3—H3120.00
C45—N2—C46130.3 (4)C4—C5—H5121.00
N1—N2—C46119.8 (3)C6—C5—H5121.00
Dy1—N3—C50121.3 (2)C5—C6—H6120.00
Dy1—N3—C46121.2 (2)C7—C6—H6120.00
C46—N3—C50117.0 (3)C2—C7—H7120.00
N5—N4—C51110.3 (3)C6—C7—H7120.00
N5—N4—C50120.0 (3)C9—C10—H10121.00
C50—N4—C51129.7 (3)C11—C10—H10120.00
N4—N5—C53104.9 (3)C11—C12—H12121.00
Dy1—N5—N4119.76 (19)C13—C12—H12121.00
Dy1—N5—C53134.9 (3)C12—C13—H13120.00
O4—N6—C4117.9 (4)C14—C13—H13120.00
O3—N6—C4118.3 (4)C9—C14—H14120.00
O3—N6—O4123.8 (5)C13—C14—H14120.00
O7—N7—O8123.3 (4)C16—C17—H17121.00
O7—N7—C11117.2 (4)C18—C17—H17121.00
O8—N7—C11119.5 (3)C18—C19—H19121.00
O11—N8—O12122.2 (7)C20—C19—H19121.00
O11'—N8—O12121.9 (9)C19—C20—H20120.00
O11'—N8—C18113.0 (8)C21—C20—H20120.00
O11—N8—C18117.5 (6)C16—C21—H21120.00
O12—N8—C18117.5 (6)C20—C21—H21120.00
O15—N9—O16'116.4 (7)C23—C24—H24121.00
O15—N9—O16120.0 (6)C25—C24—H24121.00
O15—N9—C25119.6 (5)C25—C26—H26121.00
O16'—N9—C25115.4 (7)C27—C26—H26121.00
O16—N9—C25115.8 (6)C26—C27—H27120.00
O19—N10—C32116 (4)C28—C27—H27120.00
O20—N10—C32121 (6)C23—C28—H28120.00
O19—N10—O20121 (6)C27—C28—H28120.00
O19'—N10'—C32115 (6)C30—C31—H31121.00
O19'—N10'—O20'125 (5)C32—C31—H31121.00
O20'—N10'—C32113 (7)C32—C33—H33121.00
O23—N11—C39122.6 (11)C34—C33—H33121.00
O24—N11—C39111.3 (9)C33—C34—H34120.00
O23—N11—O24126.0 (12)C35—C34—H34120.00
O23'—N11'—C39108.9 (14)C30—C35—H35120.00
O24'—N11'—C39125.9 (12)C34—C35—H35120.00
O23'—N11'—O24'125.1 (16)C37—C38—H38121.00
O1—C1—C2119.5 (3)C39—C38—H38121.00
O2—C1—C2119.5 (3)C39—C40—H40121.00
O1—C1—O2121.0 (4)C41—C40—H40120.00
C1—C2—C3120.2 (3)C40—C41—H41120.00
C3—C2—C7119.4 (4)C42—C41—H41120.00
C1—C2—C7120.3 (4)C37—C42—H42120.00
C2—C3—C4119.3 (3)C41—C42—H42120.00
C3—C4—C5122.1 (4)N1—C43—H43124.00
N6—C4—C3118.9 (3)C44—C43—H43124.00
N6—C4—C5119.0 (4)C43—C44—H44127.00
C4—C5—C6118.4 (5)C45—C44—H44127.00
C5—C6—C7120.7 (5)N2—C45—H45126.00
C2—C7—C6120.1 (4)C44—C45—H45126.00
O6—C8—C9117.8 (3)C46—C47—H47121.00
O5—C8—O6124.0 (3)C48—C47—H47121.00
O5—C8—C9118.2 (3)C47—C48—H48119.00
C8—C9—C14121.9 (3)C49—C48—H48119.00
C10—C9—C14119.7 (3)C48—C49—H49122.00
C8—C9—C10118.5 (2)C50—C49—H49122.00
C9—C10—C11119.0 (3)N4—C51—H51126.00
N7—C11—C12120.3 (4)C52—C51—H51126.00
C10—C11—C12122.2 (4)C51—C52—H52127.00
N7—C11—C10117.4 (3)C53—C52—H52128.00
C11—C12—C13118.5 (5)N5—C53—H53124.00
C12—C13—C14120.9 (4)C52—C53—H53124.00
O2—Dy1—O1—C18.58 (18)C45—N2—C46—N3169.9 (5)
O5—Dy1—O1—C1161.44 (18)N1—N2—C45—C441.9 (7)
O9—Dy1—O1—C13.0 (2)N1—N2—C46—N39.4 (6)
O13—Dy1—O1—C172.5 (2)Dy1—N3—C46—N28.7 (4)
N1—Dy1—O1—C183.2 (2)Dy1—N3—C50—N47.3 (4)
N3—Dy1—O1—C1144.8 (2)C46—N3—C50—N4179.5 (3)
N5—Dy1—O1—C1149.5 (2)C50—N3—C46—C471.5 (6)
O1—Dy1—O2—C18.55 (18)Dy1—N3—C50—C49172.3 (3)
O5—Dy1—O2—C1155.8 (2)C46—N3—C50—C490.1 (6)
O9—Dy1—O2—C1167.2 (2)C50—N3—C46—N2179.1 (3)
O13—Dy1—O2—C183.29 (19)Dy1—N3—C46—C47170.7 (4)
N1—Dy1—O2—C1110.2 (2)C51—N4—N5—C530.4 (4)
N3—Dy1—O2—C156.4 (2)C51—N4—C50—C498.9 (6)
N5—Dy1—O2—C117.6 (2)C50—N4—N5—C53179.8 (4)
O1—Dy1—O5—C8124.8 (3)C51—N4—N5—Dy1173.7 (3)
O2—Dy1—O5—C8108.2 (3)C50—N4—C51—C52179.5 (4)
O9—Dy1—O5—C871.2 (3)N5—N4—C51—C520.2 (5)
O13—Dy1—O5—C85.6 (3)N5—N4—C50—C49170.4 (4)
N1—Dy1—O5—C8153.5 (3)C50—N4—N5—Dy16.9 (4)
N3—Dy1—O5—C8141.8 (3)C51—N4—C50—N3171.5 (4)
N5—Dy1—O5—C877.3 (3)N5—N4—C50—N39.2 (5)
O1—Dy1—O9—C15130.3 (3)N4—N5—C53—C520.4 (5)
O2—Dy1—O9—C15135.0 (3)Dy1—N5—C53—C52172.2 (3)
O5—Dy1—O9—C1561.5 (3)O3—N6—C4—C3168.8 (4)
O13—Dy1—O9—C1553.4 (3)O3—N6—C4—C59.4 (6)
N1—Dy1—O9—C15144.1 (3)O4—N6—C4—C311.5 (6)
N3—Dy1—O9—C15110.0 (3)O4—N6—C4—C5170.4 (4)
N5—Dy1—O9—C151.0 (4)O8—N7—C11—C12177.2 (4)
O1—Dy1—O13—C22168.1 (4)O8—N7—C11—C102.2 (5)
O2—Dy1—O13—C22137.9 (4)O7—N7—C11—C125.1 (6)
O5—Dy1—O13—C2216.7 (4)O7—N7—C11—C10175.6 (4)
O9—Dy1—O13—C2257.7 (4)O11—N8—C18—C173.6 (12)
N1—Dy1—O13—C22104.0 (4)O11—N8—C18—C19178.4 (10)
N3—Dy1—O13—C22104.9 (4)O12—N8—C18—C17158.2 (6)
N5—Dy1—O13—C2292.4 (4)O12—N8—C18—C1919.9 (10)
O1—Dy1—N1—N272.0 (3)O16—N9—C25—C2431.5 (8)
O1—Dy1—N1—C43101.8 (4)O15—N9—C25—C267.4 (7)
O2—Dy1—N1—N2124.3 (3)O15—N9—C25—C24172.6 (5)
O2—Dy1—N1—C4349.5 (4)O16—N9—C25—C26148.5 (6)
O5—Dy1—N1—N275.2 (3)O20—N10—C32—C3317 (7)
O5—Dy1—N1—C43111.0 (4)O19—N10—C32—C33177 (5)
O9—Dy1—N1—N2155.2 (3)O20—N10—C32—C31166 (5)
O9—Dy1—N1—C4331.0 (4)O19—N10—C32—C315 (7)
O13—Dy1—N1—N2158.3 (3)O23—N11—C39—C3815.1 (14)
O13—Dy1—N1—C4315.5 (6)O24—N11—C39—C38167.6 (8)
N3—Dy1—N1—N20.8 (3)O24—N11—C39—C4012.5 (13)
N3—Dy1—N1—C43174.7 (5)O23—N11—C39—C40164.8 (11)
N5—Dy1—N1—N21.7 (4)O2—C1—C2—C7173.5 (3)
N5—Dy1—N1—C43175.5 (4)O1—C1—C2—C74.2 (5)
O1—Dy1—N3—C46105.0 (3)O2—C1—C2—C33.9 (5)
O1—Dy1—N3—C5083.1 (3)O1—C1—C2—C3178.4 (3)
O2—Dy1—N3—C4667.0 (3)C1—C2—C7—C6177.5 (4)
O2—Dy1—N3—C50121.1 (3)C3—C2—C7—C60.1 (6)
O5—Dy1—N3—C4684.4 (3)C7—C2—C3—C40.7 (6)
O5—Dy1—N3—C5087.4 (3)C1—C2—C3—C4176.7 (3)
O9—Dy1—N3—C4633.8 (3)C2—C3—C4—C50.8 (6)
O9—Dy1—N3—C50138.0 (3)C2—C3—C4—N6177.3 (4)
O13—Dy1—N3—C46171.6 (3)N6—C4—C5—C6178.0 (4)
O13—Dy1—N3—C5016.5 (3)C3—C4—C5—C60.1 (6)
N1—Dy1—N3—C464.4 (3)C4—C5—C6—C70.7 (7)
N1—Dy1—N3—C50176.3 (3)C5—C6—C7—C20.8 (7)
N5—Dy1—N3—C46174.8 (3)O6—C8—C9—C14178.3 (3)
N5—Dy1—N3—C503.0 (3)O6—C8—C9—C101.9 (4)
O1—Dy1—N5—N479.5 (2)O5—C8—C9—C10176.8 (3)
O1—Dy1—N5—C5391.4 (4)O5—C8—C9—C143.0 (5)
O2—Dy1—N5—N4101.1 (2)C14—C9—C10—C110.7 (5)
O2—Dy1—N5—C5369.8 (4)C8—C9—C14—C13179.9 (4)
O5—Dy1—N5—N475.8 (2)C8—C9—C10—C11179.5 (3)
O5—Dy1—N5—C53113.3 (4)C10—C9—C14—C130.3 (6)
O9—Dy1—N5—N4135.3 (2)C9—C10—C11—N7178.7 (3)
O9—Dy1—N5—C5353.8 (4)C9—C10—C11—C120.6 (6)
O13—Dy1—N5—N4168.7 (3)C10—C11—C12—C130.2 (7)
O13—Dy1—N5—C532.2 (4)N7—C11—C12—C13179.2 (4)
N1—Dy1—N5—N43.0 (3)C11—C12—C13—C140.2 (7)
N1—Dy1—N5—C53173.9 (4)C12—C13—C14—C90.2 (7)
N3—Dy1—N5—N42.1 (2)O9—C15—C16—C17177.0 (3)
N3—Dy1—N5—C53173.0 (4)O10—C15—C16—C21165.1 (12)
O10—Dy2—O6—C834.4 (5)O9—C15—C16—C215.3 (5)
O14—Dy2—O6—C8110.0 (6)O10—C15—C16—C1712.6 (12)
O18—Dy2—O6—C8174.9 (3)C21—C16—C17—C183.1 (6)
O21—Dy2—O6—C828.2 (4)C17—C16—C21—C204.5 (6)
O17i—Dy2—O6—C847.8 (3)C15—C16—C17—C18174.6 (4)
O22i—Dy2—O6—C8124.9 (3)C15—C16—C21—C20173.1 (4)
O6—Dy2—O14—C2292.0 (19)C16—C17—C18—N8179.3 (5)
O10—Dy2—O14—C2216.6 (18)C16—C17—C18—C191.3 (8)
O18—Dy2—O14—C22143 (2)C17—C18—C19—C204.2 (9)
O21—Dy2—O14—C2265.7 (19)N8—C18—C19—C20177.9 (6)
O17i—Dy2—O14—C221 (3)C18—C19—C20—C212.6 (9)
O22i—Dy2—O14—C22160.0 (16)C19—C20—C21—C161.6 (8)
O6—Dy2—O18—C29142.6 (3)O14—C22—C23—C2819.0 (12)
O10—Dy2—O18—C29114.0 (7)O14—C22—C23—C24159.7 (11)
O14—Dy2—O18—C29146.6 (7)O13—C22—C23—C28172.9 (3)
O21—Dy2—O18—C2949.8 (4)O13—C22—C23—C248.4 (4)
O17i—Dy2—O18—C2917.6 (4)C28—C23—C24—C251.9 (5)
O22i—Dy2—O18—C2981.7 (4)C22—C23—C24—C25176.9 (3)
O6—Dy2—O21—C36124.1 (4)C24—C23—C28—C271.7 (5)
O10—Dy2—O21—C36130.1 (6)C22—C23—C28—C27177.1 (3)
O14—Dy2—O21—C36155.9 (7)C23—C24—C25—C260.5 (6)
O18—Dy2—O21—C3684.6 (4)C23—C24—C25—N9179.5 (4)
O17i—Dy2—O21—C3644.6 (4)C24—C25—C26—C271.3 (6)
O22i—Dy2—O21—C3623.7 (5)N9—C25—C26—C27178.8 (4)
O6—Dy2—O17i—C29i139.3 (5)C25—C26—C27—C281.5 (6)
O10—Dy2—O17i—C29i147.4 (6)C26—C27—C28—C230.0 (6)
O14—Dy2—O17i—C29i131.9 (15)O18—C29—C30—C3518.0 (5)
O18—Dy2—O17i—C29i4.4 (5)O17—C29—C30—C35161.0 (3)
O21—Dy2—O17i—C29i63.0 (5)O17—C29—C30—C3115.9 (5)
O6—Dy2—O22i—C36i157.9 (3)O18—C29—C30—C31165.1 (3)
O10—Dy2—O22i—C36i123.4 (7)C31—C30—C35—C342.3 (6)
O14—Dy2—O22i—C36i129.6 (7)C35—C30—C31—C320.7 (6)
O18—Dy2—O22i—C36i73.1 (3)C29—C30—C31—C32176.3 (4)
O21—Dy2—O22i—C36i9.9 (4)C29—C30—C35—C34174.6 (4)
Dy1—O1—C1—O215.7 (3)C30—C31—C32—C332.0 (7)
Dy1—O1—C1—C2161.9 (3)C30—C31—C32—N10175 (3)
Dy1—O2—C1—O115.5 (3)C31—C32—C33—C342.9 (8)
Dy1—O2—C1—C2162.1 (3)N10—C32—C33—C34174 (3)
Dy1—O5—C8—C9155.8 (2)C32—C33—C34—C351.2 (9)
Dy1—O5—C8—O625.6 (5)C33—C34—C35—C301.4 (8)
Dy2—O6—C8—C980.8 (4)O22—C36—C37—C422.3 (4)
Dy2—O6—C8—O5100.6 (3)O21—C36—C37—C382.6 (4)
Dy1—O9—C15—C16174.5 (2)O21—C36—C37—C42178.3 (3)
Dy1—O9—C15—O103.7 (12)O22—C36—C37—C38176.8 (3)
Dy1—O13—C22—C23150.7 (3)C36—C37—C38—C39178.2 (3)
Dy1—O13—C22—O1441.3 (13)C42—C37—C38—C390.9 (5)
Dy2—O14—C22—O1388.0 (17)C38—C37—C42—C410.6 (6)
Dy2—O14—C22—C23104.4 (17)C36—C37—C42—C41178.5 (4)
Dy2i—O17—C29—C30170.0 (3)C37—C38—C39—N11179.0 (5)
Dy2i—O17—C29—O188.9 (7)C37—C38—C39—C401.1 (6)
Dy2—O18—C29—O1719.0 (6)N11—C39—C40—C41179.0 (7)
Dy2—O18—C29—C30159.9 (2)C38—C39—C40—C411.1 (8)
Dy2—O21—C36—C37157.9 (3)C39—C40—C41—C420.8 (8)
Dy2—O21—C36—O2221.4 (6)C40—C41—C42—C370.6 (8)
Dy2i—O22—C36—C37176.2 (2)N1—C43—C44—C450.2 (8)
Dy2i—O22—C36—O213.1 (5)C43—C44—C45—N21.2 (8)
C43—N1—N2—C46178.9 (4)N2—C46—C47—C48178.3 (5)
Dy1—N1—C43—C44173.6 (4)N3—C46—C47—C482.3 (8)
N2—N1—C43—C440.9 (6)C46—C47—C48—C491.5 (8)
Dy1—N1—N2—C45173.7 (4)C47—C48—C49—C500.0 (8)
Dy1—N1—N2—C465.8 (5)C48—C49—C50—N30.9 (7)
C43—N1—N2—C451.7 (6)C48—C49—C50—N4178.7 (4)
C46—N2—C45—C44178.8 (5)N4—C51—C52—C530.1 (5)
N1—N2—C46—C47170.0 (4)C51—C52—C53—N50.3 (5)
C45—N2—C46—C4710.7 (8)
Symmetry code: (i) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C10—H10···O22i0.932.453.366 (4)170
C43—H43···O2ii0.932.473.212 (5)137
C51—H51···O6iii0.932.323.243 (5)172
Symmetry codes: (i) x, y+1, z; (ii) x+1, y+2, z+1; (iii) x, y+2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C10—H10···O22i0.932.453.366 (4)170
C43—H43···O2ii0.932.473.212 (5)137
C51—H51···O6iii0.932.323.243 (5)172
Symmetry codes: (i) x, y+1, z; (ii) x+1, y+2, z+1; (iii) x, y+2, z.
Acknowledgements top

This work was supported by the Foundation of Jiangxi Educational Committee (No. GJJ13472).

references
References top

Abbas, G. L. Y.-H., Kostakis, G. E., Wernsdorfer, W., Anson, C. E. & Powell, A. K. (2010). Inorg. Chem. 49, 8067–8072.

Blagg, R. J., Muryn, C. A., Mcinnes, E. L., Tuna, F. & Winpenny, R. E. P. (2011). Angew. Chem. Int. Ed. 50, 1–5.

Brandenburg, K. (2005). DIAMOND. Crystal Impact GbR, Bonn,Germany.

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

Guo, P.-H., Liu, J.-L., Zhang, M.-Z., Ungur, L., Chibotaru, L. F., Leng, J.-D., Guo, F.-S. & Tong, M.-L. (2012). Inorg. Chem. 51, 1233–1235.

Hussain, B., Savard, D., Burchell, T. J., Wernsdorfer, W. & Murugesu, M. (2009). Chem. Commun. pp. 1100–1102.

Lin, S.-Y., Zhao, L., Ke, H.-S., Guo, Y.-N., Tang, J.-K., Guo, Y. & Dou, J.-M. (2012). Dalton Trans. 41, 3248–3252.

Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.

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

Tian, H.-Q., Zhao, L., Guo, Y.-N., Tang, J.-K. & Liu, Z.-L. (2012). Chem. Commun. 48, 708–710.

Wu, D.-Y., Guo, D., Song, Y., Huang, W., Duan, C.-Y. & Meng, Q.-J. (2009). Inorg. Chem. 48, 854–860.

Xu, G.-F., Wang, Q.-L., Gamez, P., Ma, Y., Clerac, R., Tang, J.-K., Yan, S.-P., Cheng, P. & Liao, D.-Z. (2010). Chem. Commun. 46, 1506–1508.

Zheng, Y.-Z., Xue, W., Tong, M.-L., Chen, X.-M. & Zheng, S.-L. (2008). Inorg. Chem. 47, 11202–11211.