Triimidazolium tris-(pyridine-2,6-di-carboxyl-ato)dysprosate(III) trihydrate.

The structure of the title compound, (C(3)N(2)H(5))(3)[Dy(C(7)H(3)NO(4))(3)]·3H(2)O, contains a mononuclear Dy(III) complex with the rare earth metal cation in a distorted tricapped trigonal-prismatic environment. The Dy(III) ion is in each case O,N,O'-chelated by three tridentate pyridine-2,6-dicarboxyl-ate anions. Three protonated imidazole mol-ecules act as counter-cations and three lattice water mol-ecules are also present. Numerous N-H⋯O and O-H⋯O hydrogen bonding inter-actions, some of which are bifurcated, help to stabilize the packing of the structure.

Related literature

For background to pyridine-2,6-dicarb­oxy­lic acid (H2pda) and structures of metal complexes with (pda2−) ligands, see: Ghosh & Bharadwaj (2005 ▶); Huang et al. (2008 ▶); Kjell et al. (1993 ▶); Song et al. (2005 ▶); Wu et al. (2008 ▶); Yue et al. (2005 ▶); Zhao et al. (2005 ▶, 2007 ▶).

Experimental

Crystal data

(C3H5N2)3[Dy(C7H3NO4)3]·3H2O

M = 919.13

Triclinic,

a = 10.939 (2) Å

b = 12.099 (2) Å

c = 14.070 (3) Å

α = 88.57 (3)°

β = 85.64 (3)°

γ = 67.28 (3)°

V = 1712.7 (6) Å3

Z = 2

Mo Kα radiation

μ = 2.27 mm−1

T = 296 K

0.35 × 0.25 × 0.25 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.504, T max = 0.601

27464 measured reflections

7447 independent reflections

7223 reflections with I > 2σ(I)

R int = 0.022

Refinement

R[F 2 > 2σ(F 2)] = 0.022

wR(F 2) = 0.060

S = 1.10

7447 reflections

505 parameters

3 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.69 e Å−3

Δρmin = −0.77 e Å−3

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810036421/wm2398sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810036421/wm2398Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

(C3H5N2)3[Dy(C7H3NO4)3]·3H2O	Z = 2
Mr = 919.13	F(000) = 918
Triclinic, P1	Dx = 1.782 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.939 (2) Å	Cell parameters from 125 reflections
b = 12.099 (2) Å	θ = 7.5–15°
c = 14.070 (3) Å	µ = 2.27 mm−1
α = 88.57 (3)°	T = 296 K
β = 85.64 (3)°	Block, colourless
γ = 67.28 (3)°	0.35 × 0.25 × 0.25 mm
V = 1712.7 (6) Å3

Bruker APEXII CCD diffractometer	7447 independent reflections
Radiation source: fine-focus sealed tube	7223 reflections with I > 2σ(I)
graphite	Rint = 0.022
φ and ω scans	θmax = 27.0°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −13→13
Tmin = 0.504, Tmax = 0.601	k = −13→15
27464 measured reflections	l = −17→17

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.022	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.060	H atoms treated by a mixture of independent and constrained refinement
S = 1.10	w = 1/[σ2(Fo2) + (0.0314P)2 + 1.7104P] where P = (Fo2 + 2Fc2)/3
7447 reflections	(Δ/σ)max = 0.001
505 parameters	Δρmax = 0.69 e Å−3
3 restraints	Δρmin = −0.77 e Å−3

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

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

	x	y	z	Uiso*/Ueq
Dy2	0.492045 (10)	0.266222 (9)	0.252168 (7)	0.02219 (4)
N1	0.38988 (19)	0.43970 (17)	0.36385 (14)	0.0243 (4)
O11	0.31544 (18)	0.41655 (17)	0.17113 (13)	0.0338 (4)
N2	0.5350 (2)	0.05867 (18)	0.30655 (14)	0.0257 (4)
O3	0.29744 (19)	0.27164 (17)	0.34879 (14)	0.0345 (4)
O9	0.71488 (18)	0.14570 (17)	0.18726 (13)	0.0344 (4)
O7	0.40575 (19)	0.15338 (17)	0.15780 (13)	0.0348 (4)
O1	0.60328 (17)	0.40305 (16)	0.25167 (13)	0.0304 (4)
O5	0.6077 (2)	0.20866 (16)	0.39291 (13)	0.0350 (4)
N3	0.5446 (2)	0.29826 (18)	0.07972 (14)	0.0265 (4)
O10	0.8795 (2)	0.1004 (2)	0.07273 (15)	0.0456 (5)
C6	0.5682 (3)	0.4965 (2)	0.30392 (18)	0.0288 (5)
C14	0.4159 (3)	0.0481 (2)	0.17445 (18)	0.0298 (5)
C13	0.6477 (3)	0.1058 (2)	0.42917 (18)	0.0300 (5)
C5	0.2800 (2)	0.4523 (2)	0.41906 (17)	0.0269 (5)
C1	0.4427 (2)	0.5216 (2)	0.36810 (17)	0.0268 (5)
O8	0.3703 (2)	−0.01097 (19)	0.12661 (15)	0.0432 (5)
C15	0.6663 (2)	0.2410 (2)	0.03876 (18)	0.0290 (5)
C8	0.6011 (2)	0.0175 (2)	0.38414 (17)	0.0270 (5)
C21	0.3162 (3)	0.4294 (3)	0.0813 (2)	0.0388 (6)
O6	0.7192 (2)	0.07182 (19)	0.49629 (16)	0.0475 (5)
C11	0.5093 (3)	−0.1261 (2)	0.2908 (2)	0.0368 (6)
H11	0.4774	−0.1736	0.2576	0.044*
O4	0.1420 (2)	0.34799 (19)	0.46686 (15)	0.0419 (5)
C12	0.4892 (2)	−0.0110 (2)	0.26079 (18)	0.0286 (5)
C20	0.7622 (3)	0.1555 (2)	0.10429 (19)	0.0313 (5)
C7	0.2347 (2)	0.3501 (2)	0.41110 (18)	0.0282 (5)
O2	0.6264 (2)	0.5655 (2)	0.30446 (17)	0.0466 (5)
C2	0.3867 (3)	0.6207 (2)	0.4278 (2)	0.0363 (6)
H2	0.4260	0.6762	0.4306	0.044*
C9	0.6241 (3)	−0.0961 (2)	0.4192 (2)	0.0349 (6)
H9	0.6695	−0.1231	0.4739	0.042*
C4	0.2156 (3)	0.5508 (2)	0.4781 (2)	0.0355 (6)
H4	0.1369	0.5601	0.5135	0.043*
C19	0.4500 (3)	0.3706 (2)	0.02714 (18)	0.0305 (5)
C16	0.6994 (3)	0.2573 (3)	−0.0559 (2)	0.0388 (6)
H16	0.7858	0.2185	−0.0824	0.047*
C17	0.6007 (3)	0.3327 (3)	−0.1099 (2)	0.0445 (7)
H17	0.6199	0.3450	−0.1739	0.053*
C18	0.4737 (3)	0.3896 (3)	−0.0690 (2)	0.0413 (6)
H18	0.4057	0.4393	−0.1047	0.050*
C10	0.5776 (3)	−0.1689 (2)	0.3708 (2)	0.0391 (6)
H10	0.5924	−0.2460	0.3922	0.047*
O12	0.2182 (2)	0.4833 (3)	0.03738 (18)	0.0843 (11)
C3	0.2725 (3)	0.6355 (3)	0.4827 (2)	0.0418 (7)
H3	0.2332	0.7017	0.5229	0.050*
C30	0.2356 (3)	0.1317 (3)	0.9875 (2)	0.0349 (6)
H30	0.2716	0.0773	1.0356	0.042*
C29	0.3007 (4)	0.1858 (4)	0.9312 (3)	0.0565 (9)
H29	0.3893	0.1754	0.9332	0.068*
N9	0.2143 (4)	0.2573 (4)	0.8719 (3)	0.0879 (12)
H9A	0.2305	0.3022	0.8285	0.105*
C28	0.0964 (3)	0.2459 (3)	0.8928 (2)	0.0409 (6)
H28	0.0184	0.2856	0.8628	0.049*
N8	0.1118 (4)	0.1690 (4)	0.9629 (3)	0.0694 (9)
H8A	0.044 (4)	0.144 (4)	0.990 (3)	0.083*
N7	0.0067 (3)	0.9748 (3)	0.22123 (19)	0.0460 (6)
H7A	−0.032 (3)	1.016 (3)	0.172 (2)	0.055*
C25	−0.0575 (3)	0.9456 (4)	0.2928 (3)	0.0577 (9)
H25	−0.1468	0.9570	0.2959	0.069*
C26	0.1345 (3)	0.9451 (3)	0.2428 (2)	0.0461 (7)
H26	0.2019	0.9561	0.2043	0.055*
N6	0.0242 (3)	0.8977 (3)	0.3600 (2)	0.0556 (7)
H6	0.0043	0.8714	0.4138	0.067*
C27	0.1448 (4)	0.8969 (3)	0.3299 (3)	0.0520 (8)
H27	0.2209	0.8682	0.3635	0.062*
C23	0.9146 (3)	0.3939 (4)	0.1412 (2)	0.0529 (8)
H23	0.8654	0.4415	0.0937	0.063*
C24	0.8704 (3)	0.3407 (3)	0.2103 (2)	0.0363 (6)
H24	0.7834	0.3455	0.2205	0.044*
C22	1.0765 (3)	0.2936 (3)	0.2290 (3)	0.0520 (8)
H22	1.1600	0.2603	0.2529	0.062*
N5	1.0434 (3)	0.3669 (4)	0.1519 (3)	0.0713 (10)
H5	1.0957	0.3912	0.1167	0.086*
O13	0.0930 (3)	0.6349 (2)	0.22816 (19)	0.0625 (7)
H2W	0.0469	0.6143	0.2710	0.094*
H1W	0.1609	0.5740	0.2092	0.094*
O14	0.0736 (2)	0.1513 (2)	0.46679 (16)	0.0482 (5)
H3W	0.0936	0.2127	0.4652	0.072*
H4W	0.1461	0.0904	0.4598	0.072*
O15	0.1116 (3)	0.4098 (3)	0.6635 (2)	0.0794 (9)
H5W	0.1782	0.4267	0.6729	0.119*
H6W	0.1159	0.3982	0.6038	0.119*
N4	0.9700 (4)	0.2789 (3)	0.2631 (3)	0.0758 (10)
H4A	0.966 (5)	0.231 (4)	0.316 (3)	0.091*

	U11	U22	U33	U12	U13	U23
Dy2	0.02178 (6)	0.02328 (6)	0.02335 (7)	−0.01066 (4)	−0.00168 (4)	−0.00032 (4)
N1	0.0258 (10)	0.0247 (9)	0.0244 (9)	−0.0116 (8)	−0.0031 (8)	0.0020 (7)
O11	0.0279 (9)	0.0380 (10)	0.0295 (9)	−0.0059 (7)	−0.0021 (7)	0.0010 (7)
N2	0.0259 (10)	0.0265 (9)	0.0266 (10)	−0.0127 (8)	−0.0001 (8)	−0.0016 (8)
O3	0.0353 (10)	0.0355 (9)	0.0383 (10)	−0.0213 (8)	0.0089 (8)	−0.0095 (8)
O9	0.0272 (9)	0.0370 (10)	0.0327 (10)	−0.0062 (7)	0.0007 (7)	0.0046 (8)
O7	0.0442 (11)	0.0354 (9)	0.0324 (9)	−0.0221 (8)	−0.0110 (8)	0.0018 (7)
O1	0.0286 (9)	0.0306 (9)	0.0349 (9)	−0.0156 (7)	0.0033 (7)	−0.0038 (7)
O5	0.0469 (11)	0.0284 (9)	0.0335 (10)	−0.0166 (8)	−0.0143 (8)	0.0015 (7)
N3	0.0265 (10)	0.0279 (10)	0.0261 (10)	−0.0115 (8)	−0.0020 (8)	−0.0001 (8)
O10	0.0290 (10)	0.0535 (13)	0.0418 (11)	−0.0038 (9)	0.0053 (8)	0.0010 (9)
C6	0.0294 (12)	0.0286 (11)	0.0321 (13)	−0.0151 (10)	−0.0045 (10)	0.0031 (9)
C14	0.0282 (12)	0.0353 (13)	0.0298 (12)	−0.0168 (10)	0.0000 (10)	−0.0045 (10)
C13	0.0334 (13)	0.0297 (12)	0.0282 (12)	−0.0133 (10)	−0.0045 (10)	−0.0008 (9)
C5	0.0279 (12)	0.0271 (11)	0.0256 (11)	−0.0108 (9)	−0.0008 (9)	0.0015 (9)
C1	0.0293 (12)	0.0262 (11)	0.0277 (12)	−0.0133 (9)	−0.0045 (9)	0.0019 (9)
O8	0.0535 (12)	0.0449 (11)	0.0446 (11)	−0.0312 (10)	−0.0158 (10)	−0.0016 (9)
C15	0.0276 (12)	0.0324 (12)	0.0278 (12)	−0.0128 (10)	−0.0004 (9)	−0.0022 (9)
C8	0.0271 (12)	0.0279 (11)	0.0264 (12)	−0.0111 (9)	−0.0002 (9)	−0.0005 (9)
C21	0.0306 (13)	0.0470 (16)	0.0327 (14)	−0.0074 (12)	−0.0071 (11)	0.0016 (12)
O6	0.0633 (14)	0.0397 (11)	0.0435 (12)	−0.0200 (10)	−0.0295 (11)	0.0068 (9)
C11	0.0399 (15)	0.0316 (13)	0.0454 (15)	−0.0207 (11)	−0.0034 (12)	−0.0024 (11)
O4	0.0411 (11)	0.0447 (11)	0.0454 (12)	−0.0255 (9)	0.0149 (9)	−0.0085 (9)
C12	0.0286 (12)	0.0300 (12)	0.0312 (12)	−0.0158 (10)	−0.0008 (10)	−0.0025 (10)
C20	0.0256 (12)	0.0313 (12)	0.0350 (14)	−0.0090 (10)	−0.0001 (10)	−0.0028 (10)
C7	0.0269 (12)	0.0307 (12)	0.0290 (12)	−0.0136 (10)	−0.0002 (9)	0.0015 (9)
O2	0.0484 (12)	0.0445 (11)	0.0597 (14)	−0.0336 (10)	0.0092 (10)	−0.0107 (10)
C2	0.0434 (15)	0.0301 (12)	0.0396 (15)	−0.0191 (11)	0.0000 (12)	−0.0049 (11)
C9	0.0339 (13)	0.0321 (13)	0.0399 (14)	−0.0138 (11)	−0.0055 (11)	0.0069 (11)
C4	0.0378 (14)	0.0338 (13)	0.0348 (14)	−0.0154 (11)	0.0080 (11)	−0.0058 (11)
C19	0.0314 (13)	0.0335 (12)	0.0260 (12)	−0.0118 (10)	−0.0035 (10)	0.0020 (10)
C16	0.0351 (14)	0.0504 (16)	0.0304 (13)	−0.0170 (12)	0.0055 (11)	−0.0030 (12)
C17	0.0501 (18)	0.0593 (19)	0.0244 (13)	−0.0221 (15)	0.0007 (12)	0.0048 (12)
C18	0.0438 (16)	0.0486 (16)	0.0296 (14)	−0.0155 (13)	−0.0068 (12)	0.0077 (12)
C10	0.0413 (15)	0.0291 (13)	0.0514 (17)	−0.0186 (11)	−0.0044 (13)	0.0082 (12)
O12	0.0377 (13)	0.131 (3)	0.0416 (14)	0.0155 (15)	−0.0127 (11)	0.0054 (15)
C3	0.0505 (17)	0.0311 (13)	0.0430 (16)	−0.0161 (12)	0.0083 (13)	−0.0122 (12)
C30	0.0391 (14)	0.0399 (14)	0.0301 (13)	−0.0187 (12)	−0.0093 (11)	−0.0013 (11)
C29	0.0447 (18)	0.069 (2)	0.057 (2)	−0.0227 (17)	−0.0042 (16)	0.0032 (17)
N9	0.097 (3)	0.088 (3)	0.072 (2)	−0.031 (2)	0.000 (2)	0.019 (2)
C28	0.0372 (15)	0.0498 (16)	0.0341 (14)	−0.0145 (13)	−0.0077 (12)	0.0051 (12)
N8	0.069 (2)	0.079 (2)	0.068 (2)	−0.0367 (19)	−0.0072 (17)	−0.0045 (18)
N7	0.0380 (13)	0.0514 (15)	0.0421 (14)	−0.0099 (11)	−0.0052 (11)	0.0048 (12)
C25	0.0390 (17)	0.072 (2)	0.056 (2)	−0.0163 (16)	0.0029 (15)	0.0062 (18)
C26	0.0381 (15)	0.0491 (17)	0.0527 (18)	−0.0185 (13)	−0.0025 (13)	−0.0035 (14)
N6	0.0671 (19)	0.0552 (17)	0.0408 (15)	−0.0205 (15)	0.0000 (13)	0.0057 (12)
C27	0.0521 (19)	0.0497 (18)	0.056 (2)	−0.0181 (15)	−0.0202 (16)	−0.0003 (15)
C23	0.0414 (17)	0.073 (2)	0.0451 (18)	−0.0223 (16)	−0.0081 (14)	0.0018 (16)
C24	0.0236 (12)	0.0502 (16)	0.0407 (15)	−0.0206 (11)	0.0011 (10)	−0.0094 (12)
C22	0.0242 (14)	0.061 (2)	0.064 (2)	−0.0068 (13)	−0.0130 (14)	−0.0145 (17)
N5	0.0547 (19)	0.094 (3)	0.079 (2)	−0.0465 (19)	0.0196 (17)	−0.026 (2)
O13	0.0524 (14)	0.0571 (15)	0.0597 (15)	−0.0014 (12)	−0.0012 (12)	−0.0022 (12)
O14	0.0477 (12)	0.0453 (12)	0.0567 (14)	−0.0235 (10)	−0.0070 (10)	0.0091 (10)
O15	0.090 (2)	0.102 (2)	0.0473 (15)	−0.0424 (19)	0.0164 (14)	−0.0014 (15)
N4	0.093 (3)	0.058 (2)	0.071 (2)	−0.023 (2)	−0.009 (2)	0.0016 (17)

Dy2—O5	2.3745 (19)	C4—H4	0.9300
Dy2—O1	2.4032 (17)	C19—C18	1.388 (4)
Dy2—O7	2.4072 (18)	C16—C17	1.381 (4)
Dy2—O3	2.4167 (19)	C16—H16	0.9300
Dy2—O11	2.420 (2)	C17—C18	1.376 (4)
Dy2—O9	2.426 (2)	C17—H17	0.9300
Dy2—N2	2.482 (2)	C18—H18	0.9300
Dy2—N1	2.492 (2)	C10—H10	0.9300
Dy2—N3	2.506 (2)	C3—H3	0.9300
N1—C1	1.331 (3)	C30—N8	1.322 (4)
N1—C5	1.339 (3)	C30—C29	1.345 (5)
O11—C21	1.270 (3)	C30—H30	0.9300
N2—C8	1.333 (3)	C29—N9	1.339 (5)
N2—C12	1.334 (3)	C29—H29	0.9300
O3—C7	1.260 (3)	N9—C28	1.359 (5)
O9—C20	1.262 (3)	N9—H9A	0.8600
O7—C14	1.253 (3)	C28—N8	1.313 (5)
O1—C6	1.277 (3)	C28—H28	0.9300
O5—C13	1.258 (3)	N8—H8A	0.960 (19)
N3—C19	1.330 (3)	N7—C25	1.304 (4)
N3—C15	1.333 (3)	N7—C26	1.359 (4)
O10—C20	1.246 (3)	N7—H7A	0.873 (18)
C6—O2	1.230 (3)	C25—N6	1.315 (5)
C6—C1	1.515 (4)	C25—H25	0.9300
C14—O8	1.250 (3)	C26—C27	1.338 (5)
C14—C12	1.514 (4)	C26—H26	0.9300
C13—O6	1.232 (3)	N6—C27	1.351 (5)
C13—C8	1.518 (3)	N6—H6	0.8600
C5—C4	1.385 (4)	C27—H27	0.9300
C5—C7	1.510 (3)	C23—C24	1.317 (5)
C1—C2	1.387 (4)	C23—N5	1.337 (5)
C15—C16	1.383 (4)	C23—H23	0.9300
C15—C20	1.511 (4)	C24—N4	1.328 (5)
C8—C9	1.384 (3)	C24—H24	0.9300
C21—O12	1.223 (4)	C22—N4	1.301 (5)
C21—C19	1.511 (4)	C22—N5	1.362 (5)
C11—C10	1.375 (4)	C22—H22	0.9300
C11—C12	1.383 (4)	N5—H5	0.8600
C11—H11	0.9300	O13—H2W	0.8499
O4—C7	1.241 (3)	O13—H1W	0.8500
C2—C3	1.369 (4)	O14—H3W	0.8501
C2—H2	0.9300	O14—H4W	0.8500
C9—C10	1.388 (4)	O15—H5W	0.8500
C9—H9	0.9300	O15—H6W	0.8501
C4—C3	1.395 (4)	N4—H4A	0.937 (19)
O5—Dy2—O1	78.70 (7)	O10—C20—O9	125.6 (3)
O5—Dy2—O7	129.04 (6)	O10—C20—C15	118.3 (2)
O1—Dy2—O7	146.45 (6)	O9—C20—C15	116.1 (2)
O5—Dy2—O3	86.53 (7)	O4—C7—O3	125.3 (2)
O1—Dy2—O3	128.79 (6)	O4—C7—C5	118.4 (2)
O7—Dy2—O3	77.27 (7)	O3—C7—C5	116.3 (2)
O5—Dy2—O11	147.58 (7)	C3—C2—C1	119.0 (2)
O1—Dy2—O11	88.66 (7)	C3—C2—H2	120.5
O7—Dy2—O11	75.43 (7)	C1—C2—H2	120.5
O3—Dy2—O11	78.34 (7)	C8—C9—C10	118.3 (3)
O5—Dy2—O9	78.53 (7)	C8—C9—H9	120.8
O1—Dy2—O9	77.03 (7)	C10—C9—H9	120.8
O7—Dy2—O9	89.53 (7)	C5—C4—C3	117.9 (3)
O3—Dy2—O9	147.00 (7)	C5—C4—H4	121.1
O11—Dy2—O9	127.78 (6)	C3—C4—H4	121.1
O5—Dy2—N2	64.77 (7)	N3—C19—C18	122.3 (3)
O1—Dy2—N2	137.08 (6)	N3—C19—C21	114.1 (2)
O7—Dy2—N2	64.30 (7)	C18—C19—C21	123.6 (2)
O3—Dy2—N2	72.61 (7)	C17—C16—C15	118.2 (3)
O11—Dy2—N2	134.24 (7)	C17—C16—H16	120.9
O9—Dy2—N2	74.41 (7)	C15—C16—H16	120.9
O5—Dy2—N1	74.09 (7)	C18—C17—C16	119.8 (3)
O1—Dy2—N1	64.41 (6)	C18—C17—H17	120.1
O7—Dy2—N1	134.39 (7)	C16—C17—H17	120.1
O3—Dy2—N1	64.39 (7)	C17—C18—C19	118.2 (3)
O11—Dy2—N1	73.51 (7)	C17—C18—H18	120.9
O9—Dy2—N1	136.03 (7)	C19—C18—H18	120.9
N2—Dy2—N1	121.12 (7)	C11—C10—C9	119.5 (2)
O5—Dy2—N3	137.66 (7)	C11—C10—H10	120.2
O1—Dy2—N3	74.77 (7)	C9—C10—H10	120.2
O7—Dy2—N3	71.72 (7)	C2—C3—C4	119.6 (3)
O3—Dy2—N3	135.76 (7)	C2—C3—H3	120.2
O11—Dy2—N3	63.97 (7)	C4—C3—H3	120.2
O9—Dy2—N3	63.82 (7)	N8—C30—C29	108.5 (3)
N2—Dy2—N3	118.21 (7)	N8—C30—H30	125.7
N1—Dy2—N3	120.61 (7)	C29—C30—H30	125.7
C1—N1—C5	119.4 (2)	N9—C29—C30	107.2 (3)
C1—N1—Dy2	120.34 (16)	N9—C29—H29	126.4
C5—N1—Dy2	120.26 (15)	C30—C29—H29	126.4
C21—O11—Dy2	124.08 (17)	C29—N9—C28	107.4 (3)
C8—N2—C12	119.5 (2)	C29—N9—H9A	126.3
C8—N2—Dy2	119.67 (16)	C28—N9—H9A	126.3
C12—N2—Dy2	120.78 (16)	N8—C28—N9	108.0 (3)
C7—O3—Dy2	124.83 (16)	N8—C28—H28	126.0
C20—O9—Dy2	125.16 (16)	N9—C28—H28	126.0
C14—O7—Dy2	125.14 (16)	C28—N8—C30	108.8 (3)
C6—O1—Dy2	125.57 (16)	C28—N8—H8A	124 (3)
C13—O5—Dy2	125.83 (16)	C30—N8—H8A	127 (3)
C19—N3—C15	119.0 (2)	C25—N7—C26	108.6 (3)
C19—N3—Dy2	120.24 (17)	C25—N7—H7A	123 (3)
C15—N3—Dy2	120.71 (16)	C26—N7—H7A	128 (3)
O2—C6—O1	125.4 (2)	N7—C25—N6	109.0 (3)
O2—C6—C1	119.6 (2)	N7—C25—H25	125.5
O1—C6—C1	115.0 (2)	N6—C25—H25	125.5
O8—C14—O7	125.7 (2)	C27—C26—N7	106.8 (3)
O8—C14—C12	118.0 (2)	C27—C26—H26	126.6
O7—C14—C12	116.3 (2)	N7—C26—H26	126.6
O6—C13—O5	126.3 (2)	C25—N6—C27	108.3 (3)
O6—C13—C8	118.5 (2)	C25—N6—H6	125.8
O5—C13—C8	115.2 (2)	C27—N6—H6	125.8
N1—C5—C4	122.2 (2)	C26—C27—N6	107.3 (3)
N1—C5—C7	114.0 (2)	C26—C27—H27	126.4
C4—C5—C7	123.8 (2)	N6—C27—H27	126.4
N1—C1—C2	121.8 (2)	C24—C23—N5	107.4 (3)
N1—C1—C6	114.6 (2)	C24—C23—H23	126.3
C2—C1—C6	123.5 (2)	N5—C23—H23	126.3
N3—C15—C16	122.4 (2)	C23—C24—N4	108.9 (3)
N3—C15—C20	113.9 (2)	C23—C24—H24	125.5
C16—C15—C20	123.7 (2)	N4—C24—H24	125.5
N2—C8—C9	122.0 (2)	N4—C22—N5	107.5 (3)
N2—C8—C13	114.1 (2)	N4—C22—H22	126.3
C9—C8—C13	123.9 (2)	N5—C22—H22	126.3
O12—C21—O11	125.0 (3)	C23—N5—C22	107.4 (3)
O12—C21—C19	119.4 (3)	C23—N5—H5	126.3
O11—C21—C19	115.6 (2)	C22—N5—H5	126.3
C10—C11—C12	118.7 (2)	H2W—O13—H1W	109.8
C10—C11—H11	120.6	H3W—O14—H4W	107.0
C12—C11—H11	120.6	H5W—O15—H6W	105.4
N2—C12—C11	121.9 (2)	C22—N4—C24	108.8 (3)
N2—C12—C14	113.5 (2)	C22—N4—H4A	125 (3)
C11—C12—C14	124.6 (2)	C24—N4—H4A	126 (3)
O5—Dy2—N1—C1	85.81 (18)	N1—Dy2—N3—C15	126.34 (18)
O1—Dy2—N1—C1	0.95 (16)	Dy2—O1—C6—O2	178.9 (2)
O7—Dy2—N1—C1	−144.58 (16)	Dy2—O1—C6—C1	−2.1 (3)
O3—Dy2—N1—C1	179.64 (19)	Dy2—O7—C14—O8	179.2 (2)
O11—Dy2—N1—C1	−95.64 (18)	Dy2—O7—C14—C12	−0.3 (3)
O9—Dy2—N1—C1	32.2 (2)	Dy2—O5—C13—O6	172.1 (2)
N2—Dy2—N1—C1	132.20 (17)	Dy2—O5—C13—C8	−8.0 (3)
N3—Dy2—N1—C1	−50.61 (19)	C1—N1—C5—C4	2.7 (4)
O5—Dy2—N1—C5	−95.26 (18)	Dy2—N1—C5—C4	−176.21 (19)
O1—Dy2—N1—C5	179.88 (19)	C1—N1—C5—C7	−177.0 (2)
O7—Dy2—N1—C5	34.4 (2)	Dy2—N1—C5—C7	4.1 (3)
O3—Dy2—N1—C5	−1.43 (16)	C5—N1—C1—C2	−0.4 (4)
O11—Dy2—N1—C5	83.29 (17)	Dy2—N1—C1—C2	178.49 (19)
O9—Dy2—N1—C5	−148.86 (16)	C5—N1—C1—C6	178.8 (2)
N2—Dy2—N1—C5	−48.87 (19)	Dy2—N1—C1—C6	−2.2 (3)
N3—Dy2—N1—C5	128.32 (17)	O2—C6—C1—N1	−178.2 (2)
O5—Dy2—O11—C21	153.0 (2)	O1—C6—C1—N1	2.7 (3)
O1—Dy2—O11—C21	86.7 (2)	O2—C6—C1—C2	1.1 (4)
O7—Dy2—O11—C21	−63.5 (2)	O1—C6—C1—C2	−178.0 (2)
O3—Dy2—O11—C21	−143.2 (2)	C19—N3—C15—C16	2.4 (4)
O9—Dy2—O11—C21	14.3 (3)	Dy2—N3—C15—C16	−179.3 (2)
N2—Dy2—O11—C21	−92.0 (2)	C19—N3—C15—C20	−176.2 (2)
N1—Dy2—O11—C21	150.4 (2)	Dy2—N3—C15—C20	2.1 (3)
N3—Dy2—O11—C21	13.0 (2)	C12—N2—C8—C9	0.0 (4)
O5—Dy2—N2—C8	−1.01 (17)	Dy2—N2—C8—C9	177.92 (19)
O1—Dy2—N2—C8	33.4 (2)	C12—N2—C8—C13	−180.0 (2)
O7—Dy2—N2—C8	−179.4 (2)	Dy2—N2—C8—C13	−2.1 (3)
O3—Dy2—N2—C8	−95.45 (18)	O6—C13—C8—N2	−173.9 (2)
O11—Dy2—N2—C8	−148.54 (16)	O5—C13—C8—N2	6.2 (3)
O9—Dy2—N2—C8	83.44 (18)	O6—C13—C8—C9	6.1 (4)
N1—Dy2—N2—C8	−51.34 (19)	O5—C13—C8—C9	−173.8 (3)
N3—Dy2—N2—C8	131.40 (17)	Dy2—O11—C21—O12	161.7 (3)
O5—Dy2—N2—C12	176.9 (2)	Dy2—O11—C21—C19	−17.3 (4)
O1—Dy2—N2—C12	−148.70 (17)	C8—N2—C12—C11	−0.7 (4)
O7—Dy2—N2—C12	−1.49 (17)	Dy2—N2—C12—C11	−178.6 (2)
O3—Dy2—N2—C12	82.45 (18)	C8—N2—C12—C14	179.8 (2)
O11—Dy2—N2—C12	29.4 (2)	Dy2—N2—C12—C14	1.9 (3)
O9—Dy2—N2—C12	−98.66 (19)	C10—C11—C12—N2	0.7 (4)
N1—Dy2—N2—C12	126.56 (18)	C10—C11—C12—C14	−179.9 (3)
N3—Dy2—N2—C12	−50.7 (2)	O8—C14—C12—N2	179.4 (2)
O5—Dy2—O3—C7	71.8 (2)	O7—C14—C12—N2	−1.0 (3)
O1—Dy2—O3—C7	−0.7 (2)	O8—C14—C12—C11	−0.1 (4)
O7—Dy2—O3—C7	−156.8 (2)	O7—C14—C12—C11	179.5 (3)
O11—Dy2—O3—C7	−79.3 (2)	Dy2—O9—C20—O10	174.2 (2)
O9—Dy2—O3—C7	134.5 (2)	Dy2—O9—C20—C15	−6.4 (3)
N2—Dy2—O3—C7	136.5 (2)	N3—C15—C20—O10	−178.0 (2)
N1—Dy2—O3—C7	−2.17 (19)	C16—C15—C20—O10	3.3 (4)
N3—Dy2—O3—C7	−110.7 (2)	N3—C15—C20—O9	2.5 (3)
O5—Dy2—O9—C20	−154.7 (2)	C16—C15—C20—O9	−176.1 (3)
O1—Dy2—O9—C20	−73.8 (2)	Dy2—O3—C7—O4	−173.2 (2)
O7—Dy2—O9—C20	75.2 (2)	Dy2—O3—C7—C5	5.0 (3)
O3—Dy2—O9—C20	140.5 (2)	N1—C5—C7—O4	172.6 (2)
O11—Dy2—O9—C20	4.1 (2)	C4—C5—C7—O4	−7.1 (4)
N2—Dy2—O9—C20	138.6 (2)	N1—C5—C7—O3	−5.8 (3)
N1—Dy2—O9—C20	−102.5 (2)	C4—C5—C7—O3	174.5 (3)
N3—Dy2—O9—C20	5.4 (2)	N1—C1—C2—C3	−1.1 (4)
O5—Dy2—O7—C14	−1.0 (2)	C6—C1—C2—C3	179.7 (3)
O1—Dy2—O7—C14	139.05 (19)	N2—C8—C9—C10	0.7 (4)
O3—Dy2—O7—C14	−75.7 (2)	C13—C8—C9—C10	−179.3 (3)
O11—Dy2—O7—C14	−156.8 (2)	N1—C5—C4—C3	−3.3 (4)
O9—Dy2—O7—C14	73.8 (2)	C7—C5—C4—C3	176.3 (3)
N2—Dy2—O7—C14	0.9 (2)	C15—N3—C19—C18	−0.6 (4)
N1—Dy2—O7—C14	−108.4 (2)	Dy2—N3—C19—C18	−178.9 (2)
N3—Dy2—O7—C14	136.3 (2)	C15—N3—C19—C21	179.4 (2)
O5—Dy2—O1—C6	−76.9 (2)	Dy2—N3—C19—C21	1.2 (3)
O7—Dy2—O1—C6	133.71 (19)	O12—C21—C19—N3	−169.3 (3)
O3—Dy2—O1—C6	−0.8 (2)	O11—C21—C19—N3	9.8 (4)
O11—Dy2—O1—C6	73.1 (2)	O12—C21—C19—C18	10.8 (5)
O9—Dy2—O1—C6	−157.6 (2)	O11—C21—C19—C18	−170.2 (3)
N2—Dy2—O1—C6	−108.3 (2)	N3—C15—C16—C17	−2.3 (4)
N1—Dy2—O1—C6	0.76 (18)	C20—C15—C16—C17	176.2 (3)
N3—Dy2—O1—C6	136.4 (2)	C15—C16—C17—C18	0.4 (5)
O1—Dy2—O5—C13	−151.7 (2)	C16—C17—C18—C19	1.4 (5)
O7—Dy2—O5—C13	7.1 (3)	N3—C19—C18—C17	−1.3 (4)
O3—Dy2—O5—C13	77.6 (2)	C21—C19—C18—C17	178.7 (3)
O11—Dy2—O5—C13	139.3 (2)	C12—C11—C10—C9	0.1 (4)
O9—Dy2—O5—C13	−72.8 (2)	C8—C9—C10—C11	−0.8 (4)
N2—Dy2—O5—C13	5.2 (2)	C1—C2—C3—C4	0.4 (5)
N1—Dy2—O5—C13	141.9 (2)	C5—C4—C3—C2	1.7 (4)
N3—Dy2—O5—C13	−99.8 (2)	N8—C30—C29—N9	0.2 (4)
O5—Dy2—N3—C19	−155.57 (17)	C30—C29—N9—C28	0.0 (5)
O1—Dy2—N3—C19	−102.47 (19)	C29—N9—C28—N8	−0.2 (5)
O7—Dy2—N3—C19	75.94 (19)	N9—C28—N8—C30	0.4 (4)
O3—Dy2—N3—C19	28.1 (2)	C29—C30—N8—C28	−0.4 (4)
O11—Dy2—N3—C19	−6.39 (18)	C26—N7—C25—N6	−0.2 (4)
O9—Dy2—N3—C19	174.7 (2)	C25—N7—C26—C27	0.1 (4)
N2—Dy2—N3—C19	121.87 (18)	N7—C25—N6—C27	0.3 (4)
N1—Dy2—N3—C19	−55.4 (2)	N7—C26—C27—N6	0.1 (4)
O5—Dy2—N3—C15	26.2 (2)	C25—N6—C27—C26	−0.2 (4)
O1—Dy2—N3—C15	79.27 (18)	N5—C23—C24—N4	−1.1 (4)
O7—Dy2—N3—C15	−102.32 (19)	C24—C23—N5—C22	1.0 (4)
O3—Dy2—N3—C15	−150.11 (17)	N4—C22—N5—C23	−0.6 (4)
O11—Dy2—N3—C15	175.4 (2)	N5—C22—N4—C24	−0.1 (4)
O9—Dy2—N3—C15	−3.53 (17)	C23—C24—N4—C22	0.8 (4)
N2—Dy2—N3—C15	−56.4 (2)

D—H···A	D—H	H···A	D···A	D—H···A
N4—H4A···O14i	0.94 (2)	2.50 (3)	3.286 (4)	141 (4)
N5—H5···O12i	0.86	2.27	3.121 (5)	171
N8—H8A···O10ii	0.96 (2)	2.29 (2)	3.241 (4)	172 (4)
N7—H7A···O10iii	0.87 (2)	1.82 (2)	2.695 (4)	177 (4)
N7—H7A···O9iii	0.87 (2)	2.60 (3)	3.127 (3)	120 (3)
N6—H6···O14iv	0.86	1.89	2.731 (4)	167
O13—H2W···O15iv	0.85	2.02	2.828 (4)	159
O13—H1W···O11	0.85	2.05	2.896 (3)	174
O13—H1W···O12	0.85	2.61	3.192 (4)	127
O14—H3W···O4	0.85	1.91	2.756 (3)	178
O14—H4W···O6v	0.85	2.06	2.842 (3)	153
O15—H5W···O2vi	0.85	2.22	3.061 (4)	169
O15—H6W···O4	0.85	2.00	2.845 (4)	172

Table 1

Selected bond lengths (Å)

Dy2—O5	2.3745 (19)
Dy2—O1	2.4032 (17)
Dy2—O7	2.4072 (18)
Dy2—O3	2.4167 (19)
Dy2—O11	2.420 (2)
Dy2—O9	2.426 (2)
Dy2—N2	2.482 (2)
Dy2—N1	2.492 (2)
Dy2—N3	2.506 (2)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N4—H4A⋯O14i	0.94 (2)	2.50 (3)	3.286 (4)	141 (4)
N5—H5⋯O12i	0.86	2.27	3.121 (5)	171
N8—H8A⋯O10ii	0.96 (2)	2.29 (2)	3.241 (4)	172 (4)
N7—H7A⋯O10iii	0.87 (2)	1.82 (2)	2.695 (4)	177 (4)
N7—H7A⋯O9iii	0.87 (2)	2.60 (3)	3.127 (3)	120 (3)
N6—H6⋯O14iv	0.86	1.89	2.731 (4)	167
O13—H2W⋯O15iv	0.85	2.02	2.828 (4)	159
O13—H1W⋯O11	0.85	2.05	2.896 (3)	174
O13—H1W⋯O12	0.85	2.61	3.192 (4)	127
O14—H3W⋯O4	0.85	1.91	2.756 (3)	178
O14—H4W⋯O6v	0.85	2.06	2.842 (3)	153
O15—H5W⋯O2vi	0.85	2.22	3.061 (4)	169
O15—H6W⋯O4	0.85	2.00	2.845 (4)	172

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .