Bis(μ-3,5-dinitro­benzoato-κ2O1:O1′)bis­(μ-3,5-dinitro­benzoato)-κ3O1,O1′:O1;κ3O1:O1,O1′-bis­[(3,5-dinitro­benzoato-κ2O1,O1′)(1,10-phenanthroline-κ2N,N)dysprosium(III)]

Dong, C.-H.; Zhang, D.-H.; Ren, N.; Xi, G.-Q.; Hao, J.-J.

doi:10.1107/S1600536810052001

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 1| January 2011| Page m102

https://doi.org/10.1107/S1600536810052001

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Bis(μ-3,5-dinitrobenzoato-κ²O¹:O^1′)bis(μ-3,5-dinitrobenzoato)-κ³O¹,O^1′:O¹;κ³O¹:O¹,O^1′-bis[(3,5-dinitrobenzoato-κ²O¹,O^1′)(1,10-phenanthroline-κ²N,N)dysprosium(III)]

Chun-Hua Dong,^a ^* Da-Hai Zhang,^a Ning Ren,^a Gai-Qing Xi ^a and Juan-Juan Hao ^a

^aDepartment of Chemistry, Handan College, Handan, Hebei 056005, People's Republic of China
^*Correspondence e-mail: dong_chunhua@126.com

(Received 16 November 2010; accepted 11 December 2010; online 18 December 2010)

In the binuclear title complex, [Dy₂(C₇H₃N₂O₆)₆(C₁₂H₈N₂)₂], the Dy^III ions exhibit a distorted monocapped square-antiprismatic geometry and are coordinated by seven O atoms of four 3,5-dinitrobenzoate (DNBA) anions and two N atoms of a phenanthroline ligand. The carboxylate groups of the DNBA anions exhibit three coordination modes: bidentate chelating, bidentate chelating–bridging and tridentate chelating–bridging. The center of the molecule is located on a crystallographic center of inversion.

Related literature

For related structures, see: Wang et al. (2004 ); Ren et al. (2006 ); Zhang et al. (2007 ); Xu et al. (2008a ,b ).

Experimental

Crystal data

[Dy₂(C₇H₃N₂O₆)₆(C₁₂H₈N₂)₂]
M_r = 1952.09
Triclinic, $[P \overline 1]$
a = 11.9569 (4) Å
b = 12.8636 (4) Å
c = 13.1187 (4) Å
α = 104.24 (5)°
β = 113.96 (5)°
γ = 100.46 (5)°
V = 1694.6 (12) Å³
Z = 1
Mo Kα radiation
μ = 2.31 mm⁻¹
T = 296 K
0.15 × 0.13 × 0.12 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1997) T_min = 0.724, T_max = 0.769
8296 measured reflections
5771 independent reflections
5624 reflections with I > 2σ(I)
R_int = 0.011

Refinement

R[F² > 2σ(F²)] = 0.016
wR(F²) = 0.041
S = 1.03
5771 reflections
541 parameters
H-atom parameters constrained
Δρ_max = 0.43 e Å⁻³
Δρ_min = −0.78 e Å⁻³

Data collection: APEX2 (Bruker, 2004 ); cell refinement: SAINT (Bruker, 2001 ); 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 and local programs.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810052001/im2251sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810052001/im2251Isup2.hkl

checkCIF report

Comment top

Coordination compounds of rare earth metals with various carboxylic acids are of high interest because of their special structures and fascinating properties. Nowadays, they have wide applications to many fields as e.g. new materials (Wang, et al., 2004). Therefore, benzoic acid derivatives and 1,10-phenanthroline were chosen to prepare complexes with a mixed ligand set. As an extention of our previous studies (Ren, et al., 2006; Zhang, et al., 2007; Xu, et al., 2008a,b), we now report the synthesis and molecular structure of the title dysprosium complex with 3,5-dinitrobenzoic acid and 1,10-phenanthroline.

The binuclear molecular structure of [Dy(3,5-DNBA)₃(phen)]₂ is shown in Fig. 1. Fig.2 shows the coordination geometry about the Dy^III ions. Two Dy^III ions are linked by two bidentate chelating-bridging and tridentate chelating-bridging carboxylate groups. Each Dy^III ion is ninefold coordinated to two nitrogen atoms (N1, N2) from one 1,10-phenanthroline molecule, two oxygen atoms (O1, O2) from one bidentate chelating carboxylate group, two oxygen atoms (O13, O14A) from bidentate chelating-bridging carboxylate groups and three oxygen atoms (O7, O7A, O8) from tridentate chelating-bridging carboxylate groups. The coordination polyhedron adopts a distorted mono-capped square antiprismatic geometry. The oxygen atom (O7) from the tridentate chelating-bridging carboxylate adopts the capped position. The coordination mode is similar to that of [Dy(p-MOBA)₃phen]₂ (Zhang, et al., 2007) but different from that of [Dy(BA)₃phen]₂ (Xu, et al., 2008a) and [Dy(m-MBA)₃phen]₂.H₂O (Xu, et al., 2008b).

In the coordination polyhedron of Dy^III ion, Dy—O distances are in the range of 2.3257 (13) to 2.7576 (14) Å, and the mean bond length of Dy—O is 2.4341 Å. The average Dy—N distance is 2.5242 Å. It can be easily seen that the bond of Dy—O is stronger than that of Dy—N in the complex corresponding to HSAB concept. Since carboxylate units are negatively charged the corresponding oxygen atoms are the by far harder ligands and therefore establish stronger bonds towards the hard Lewis acid Dy(III) as compared to neutral nitrogen donor atoms. At the same time, the average Dy—O distance of the title complex (2.4341 Å) is slightly longer than the corresponding average distances of the complexes [Dy(BA)₃phen]₂ (Xu, et al., 2008a) (2.364 Å); and [Dy(m-MBA)₃phen]₂.H₂O (Xu, et al., 2008b) (2.346 Å). This effect can be explained by electronic effects of different substituents at the benzoate ligands.

Related literature top

For related structures, see: Wang et al. (2004); Ren et al. (2006); Zhang et al. (2007); Xu et al. (2008a,b).

Experimental top

DyCl₃.6H₂O was obtained by a reaction of Dy₂O₃ (99.95%) and HCl (6.0 mol.L^-1) followed by water bath evaporation. DyCl₃.6H₂O (0.06 mmol), 3,5-dinitrobenzoic acid (0.18 mmol), 1,10-phenanthroline(0.06 mmol) and water (1 ml) were mixed in a Parr Teflon-lined stainless vessel (25 ml). After the solution was heated at 150°C for 5 d and cooled to room temperature, yellow block crystals of the title complex were obtained in 30% yield.

Structure description top

For related structures, see: Wang et al. (2004); Ren et al. (2006); Zhang et al. (2007); Xu et al. (2008a,b).

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and local programs.

Figures top

	Fig. 1. Molecular structure of the title compound with the atom-labelling scheme.
	Fig. 2. Coordination environment of Dy^III ions.

Bis(µ-3,5-dinitrobenzoato-κ²O¹:O^1')bis(µ-3,5- dinitrobenzoato)-κ³O¹,O^1':O¹; κ³O¹:O¹,O^1'-bis[(3,5-dinitrobenzoato- κ²O¹,O^1')(1,10-phenanthroline- κ²N,N)dysprosium(III)] top

Crystal data top

[Dy₂(C₇H₃N₂O₆)₆(C₁₂H₈N₂)₂]	Z = 1
M_r = 1952.09	F(000) = 962
Triclinic, P1	D_x = 1.913 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 11.9569 (4) Å	Cell parameters from 9404 reflections
b = 12.8636 (4) Å	θ = 2.9–31.0°
c = 13.1187 (4) Å	µ = 2.31 mm⁻¹
α = 104.24 (5)°	T = 296 K
β = 113.96 (5)°	Block, yellow
γ = 100.46 (5)°	0.15 × 0.13 × 0.12 mm
V = 1694.6 (12) Å³

Data collection top

Bruker APEXII CCD diffractometer	5771 independent reflections
Radiation source: fine-focus sealed tube	5624 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.011
φ and ω scans	θ_max = 25.0°, θ_min = 2.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1997)	h = −14→14
T_min = 0.724, T_max = 0.769	k = −14→15
8296 measured reflections	l = −15→9

Refinement top

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)] = 0.016	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.041	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0218P)² + 1.1919P] where P = (F_o² + 2F_c²)/3
5771 reflections	(Δ/σ)_max = 0.002
541 parameters	Δρ_max = 0.43 e Å⁻³
0 restraints	Δρ_min = −0.78 e Å⁻³

Crystal data top

[Dy₂(C₇H₃N₂O₆)₆(C₁₂H₈N₂)₂]	γ = 100.46 (5)°
M_r = 1952.09	V = 1694.6 (12) Å³
Triclinic, P1	Z = 1
a = 11.9569 (4) Å	Mo Kα radiation
b = 12.8636 (4) Å	µ = 2.31 mm⁻¹
c = 13.1187 (4) Å	T = 296 K
α = 104.24 (5)°	0.15 × 0.13 × 0.12 mm
β = 113.96 (5)°

Data collection top

Bruker APEXII CCD diffractometer	5771 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1997)	5624 reflections with I > 2σ(I)
T_min = 0.724, T_max = 0.769	R_int = 0.011
8296 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.016	0 restraints
wR(F²) = 0.041	H-atom parameters constrained
S = 1.03	Δρ_max = 0.43 e Å⁻³
5771 reflections	Δρ_min = −0.78 e Å⁻³
541 parameters

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

	x	y	z	U_iso*/U_eq
Dy1	0.871683 (8)	−0.052102 (7)	0.823196 (7)	0.01272 (4)
O1	0.74648 (14)	−0.24750 (12)	0.72351 (13)	0.0227 (3)
O2	0.64232 (13)	−0.13350 (11)	0.76732 (12)	0.0191 (3)
O3	0.19645 (18)	−0.30876 (16)	0.6887 (2)	0.0513 (5)
O4	0.11452 (15)	−0.49005 (15)	0.62444 (16)	0.0358 (4)
O5	0.39257 (16)	−0.72017 (13)	0.60925 (18)	0.0385 (4)
O6	0.52990 (16)	−0.65952 (13)	0.55170 (14)	0.0284 (3)
O7	1.11237 (13)	0.08515 (12)	1.00543 (12)	0.0187 (3)
O8	1.03333 (13)	0.09536 (12)	0.82564 (12)	0.0204 (3)
O9	1.31759 (17)	0.43985 (14)	0.83671 (16)	0.0362 (4)
O10	1.51618 (16)	0.44826 (14)	0.88585 (15)	0.0348 (4)
O11	1.67069 (17)	0.15932 (18)	1.0302 (2)	0.0497 (5)
O12	1.57894 (15)	0.08509 (13)	1.11887 (14)	0.0274 (3)
O13	0.85945 (13)	0.11215 (11)	0.93722 (12)	0.0177 (3)
O14	0.97802 (13)	0.14829 (12)	1.13307 (12)	0.0189 (3)
O15	0.71846 (17)	0.41054 (14)	0.80972 (14)	0.0334 (4)
O16	0.79596 (16)	0.58264 (13)	0.93352 (15)	0.0301 (4)
O17	1.09372 (17)	0.66977 (14)	1.34595 (15)	0.0354 (4)
O18	1.17536 (17)	0.54349 (15)	1.39998 (14)	0.0380 (4)
N1	0.88628 (16)	−0.11343 (14)	0.62924 (15)	0.0186 (4)
N2	0.74346 (15)	0.01781 (14)	0.66740 (14)	0.0176 (3)
N3	0.20251 (18)	−0.40429 (16)	0.65720 (17)	0.0270 (4)
N4	0.45681 (17)	−0.64570 (15)	0.59303 (16)	0.0238 (4)
N5	1.41001 (19)	0.40570 (16)	0.87562 (17)	0.0274 (4)
N6	1.58388 (17)	0.14053 (16)	1.05651 (17)	0.0267 (4)
N7	0.78537 (17)	0.48234 (15)	0.90981 (16)	0.0220 (4)
N8	1.10119 (18)	0.57440 (16)	1.32688 (16)	0.0257 (4)
C1	0.83068 (19)	−0.06731 (16)	0.54593 (18)	0.0194 (4)
C2	0.9514 (2)	−0.18157 (18)	0.60723 (19)	0.0230 (4)
H2	0.9890	−0.2142	0.6630	0.028*
C3	0.9665 (2)	−0.20684 (19)	0.5046 (2)	0.0275 (5)
H3A	1.0123	−0.2557	0.4925	0.033*
C4	0.9133 (2)	−0.15888 (19)	0.4223 (2)	0.0279 (5)
H4	0.9241	−0.1735	0.3545	0.034*
C5	0.8422 (2)	−0.08754 (18)	0.44056 (18)	0.0244 (5)
C6	0.7806 (3)	−0.0350 (2)	0.3580 (2)	0.0334 (6)
H6A	0.7886	−0.0474	0.2888	0.040*
C7	0.7115 (3)	0.0315 (2)	0.3782 (2)	0.0340 (6)
H7	0.6727	0.0641	0.3228	0.041*
C8	0.6966 (2)	0.05305 (18)	0.48356 (19)	0.0252 (5)
C9	0.6240 (2)	0.12042 (18)	0.5079 (2)	0.0284 (5)
H9A	0.5856	0.1565	0.4562	0.034*
C10	0.6100 (2)	0.13266 (18)	0.6084 (2)	0.0262 (5)
H10A	0.5612	0.1762	0.6252	0.031*
C11	0.6701 (2)	0.07880 (17)	0.68493 (18)	0.0203 (4)
H11	0.6581	0.0859	0.7518	0.024*
C12	0.75638 (19)	0.00351 (16)	0.56704 (18)	0.0191 (4)
C13	0.53694 (19)	−0.33303 (16)	0.69398 (17)	0.0166 (4)
C14	0.4237 (2)	−0.32036 (17)	0.69359 (17)	0.0184 (4)
H14	0.4158	−0.2488	0.7164	0.022*
C15	0.32329 (19)	−0.41601 (18)	0.65875 (18)	0.0201 (4)
C16	0.3310 (2)	−0.52422 (17)	0.62553 (18)	0.0210 (4)
H16A	0.2631	−0.5878	0.6035	0.025*
C17	0.4446 (2)	−0.53255 (17)	0.62684 (17)	0.0192 (4)
C18	0.54786 (19)	−0.43994 (17)	0.65935 (17)	0.0181 (4)
H18	0.6227	−0.4492	0.6580	0.022*
C19	0.64844 (19)	−0.23132 (17)	0.72999 (17)	0.0174 (4)
C20	1.25799 (19)	0.17446 (16)	0.94754 (17)	0.0160 (4)
C21	1.27380 (19)	0.26101 (17)	0.90393 (17)	0.0183 (4)
H21	1.2048	0.2859	0.8671	0.022*
C22	1.3936 (2)	0.30966 (17)	0.91613 (18)	0.0216 (4)
C23	1.4972 (2)	0.27179 (18)	0.96526 (19)	0.0239 (5)
H23	1.5765	0.3030	0.9700	0.029*
C24	1.4771 (2)	0.18532 (18)	1.00693 (18)	0.0215 (4)
C25	1.36097 (19)	0.13684 (17)	1.00183 (17)	0.0184 (4)
H25	1.3520	0.0807	1.0338	0.022*
C26	1.12560 (19)	0.11572 (16)	0.92589 (18)	0.0155 (4)
C27	0.92602 (18)	0.29805 (17)	1.07147 (17)	0.0167 (4)
C28	0.85225 (18)	0.33263 (17)	0.98083 (18)	0.0175 (4)
H28	0.7983	0.2805	0.9039	0.021*
C29	0.86033 (19)	0.44536 (17)	1.00666 (18)	0.0189 (4)
C30	0.9405 (2)	0.52645 (17)	1.11932 (19)	0.0204 (4)
H30	0.9449	0.6021	1.1355	0.024*
C31	1.01314 (19)	0.48924 (17)	1.20606 (18)	0.0200 (4)
C32	1.00898 (19)	0.37735 (17)	1.18544 (18)	0.0188 (4)
H32	1.0604	0.3557	1.2463	0.023*
C33	0.92031 (18)	0.17556 (17)	1.04534 (17)	0.0161 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy1	0.01184 (6)	0.01290 (6)	0.01367 (6)	0.00395 (4)	0.00583 (4)	0.00544 (4)
O1	0.0192 (7)	0.0182 (7)	0.0302 (8)	0.0036 (6)	0.0139 (7)	0.0055 (6)
O2	0.0177 (7)	0.0146 (7)	0.0228 (7)	0.0037 (6)	0.0084 (6)	0.0061 (6)
O3	0.0317 (10)	0.0325 (10)	0.0843 (16)	0.0094 (8)	0.0328 (11)	0.0032 (10)
O4	0.0200 (8)	0.0350 (9)	0.0456 (10)	−0.0006 (7)	0.0161 (8)	0.0094 (8)
O5	0.0296 (9)	0.0190 (8)	0.0611 (12)	0.0026 (7)	0.0168 (9)	0.0167 (8)
O6	0.0358 (9)	0.0256 (8)	0.0245 (8)	0.0157 (7)	0.0124 (7)	0.0088 (7)
O7	0.0205 (7)	0.0210 (7)	0.0218 (7)	0.0085 (6)	0.0135 (6)	0.0117 (6)
O8	0.0151 (7)	0.0235 (7)	0.0176 (7)	0.0012 (6)	0.0053 (6)	0.0074 (6)
O9	0.0382 (10)	0.0351 (9)	0.0442 (10)	0.0120 (8)	0.0206 (8)	0.0261 (8)
O10	0.0319 (9)	0.0325 (9)	0.0376 (9)	−0.0037 (7)	0.0192 (8)	0.0137 (8)
O11	0.0291 (10)	0.0643 (13)	0.0799 (15)	0.0235 (9)	0.0360 (10)	0.0402 (12)
O12	0.0256 (8)	0.0304 (8)	0.0245 (8)	0.0127 (7)	0.0092 (7)	0.0088 (7)
O13	0.0174 (7)	0.0177 (7)	0.0162 (7)	0.0068 (6)	0.0066 (6)	0.0045 (6)
O14	0.0183 (7)	0.0230 (7)	0.0182 (7)	0.0109 (6)	0.0088 (6)	0.0085 (6)
O15	0.0382 (9)	0.0293 (9)	0.0217 (8)	0.0133 (7)	0.0039 (7)	0.0075 (7)
O16	0.0403 (9)	0.0223 (8)	0.0333 (9)	0.0152 (7)	0.0181 (8)	0.0140 (7)
O17	0.0392 (10)	0.0231 (9)	0.0305 (9)	0.0028 (7)	0.0149 (8)	−0.0042 (7)
O18	0.0345 (10)	0.0388 (10)	0.0200 (8)	0.0059 (8)	0.0005 (7)	0.0031 (7)
N1	0.0192 (8)	0.0160 (8)	0.0184 (8)	0.0026 (7)	0.0084 (7)	0.0057 (7)
N2	0.0145 (8)	0.0154 (8)	0.0168 (8)	0.0014 (7)	0.0037 (7)	0.0053 (7)
N3	0.0202 (9)	0.0280 (10)	0.0295 (10)	0.0046 (8)	0.0123 (8)	0.0062 (8)
N4	0.0210 (9)	0.0167 (9)	0.0221 (9)	0.0027 (7)	0.0015 (8)	0.0059 (7)
N5	0.0306 (11)	0.0232 (9)	0.0257 (10)	0.0001 (8)	0.0144 (8)	0.0088 (8)
N6	0.0174 (9)	0.0303 (10)	0.0314 (10)	0.0075 (8)	0.0118 (8)	0.0089 (9)
N7	0.0239 (9)	0.0215 (9)	0.0241 (10)	0.0103 (8)	0.0119 (8)	0.0103 (8)
N8	0.0242 (10)	0.0245 (10)	0.0209 (9)	0.0006 (8)	0.0112 (8)	0.0003 (8)
C1	0.0193 (10)	0.0136 (9)	0.0166 (10)	−0.0027 (8)	0.0051 (8)	0.0035 (8)
C2	0.0247 (11)	0.0211 (10)	0.0234 (11)	0.0067 (9)	0.0130 (9)	0.0059 (9)
C3	0.0296 (12)	0.0234 (11)	0.0281 (12)	0.0051 (9)	0.0175 (10)	0.0027 (9)
C4	0.0312 (12)	0.0268 (11)	0.0189 (11)	−0.0020 (10)	0.0148 (10)	0.0001 (9)
C5	0.0268 (11)	0.0189 (10)	0.0168 (10)	−0.0047 (9)	0.0082 (9)	0.0020 (8)
C6	0.0458 (15)	0.0292 (12)	0.0175 (11)	0.0011 (11)	0.0128 (11)	0.0074 (9)
C7	0.0452 (15)	0.0291 (12)	0.0204 (11)	0.0062 (11)	0.0088 (11)	0.0131 (10)
C8	0.0275 (11)	0.0185 (10)	0.0194 (10)	0.0012 (9)	0.0039 (9)	0.0075 (8)
C9	0.0309 (12)	0.0205 (11)	0.0255 (11)	0.0068 (9)	0.0035 (10)	0.0128 (9)
C10	0.0229 (11)	0.0187 (10)	0.0280 (12)	0.0073 (9)	0.0039 (9)	0.0076 (9)
C11	0.0167 (10)	0.0182 (10)	0.0189 (10)	0.0038 (8)	0.0039 (8)	0.0047 (8)
C12	0.0173 (10)	0.0144 (9)	0.0162 (10)	−0.0017 (8)	0.0031 (8)	0.0038 (8)
C13	0.0172 (10)	0.0166 (10)	0.0125 (9)	0.0030 (8)	0.0042 (8)	0.0061 (8)
C14	0.0203 (10)	0.0177 (10)	0.0158 (10)	0.0049 (8)	0.0076 (8)	0.0061 (8)
C15	0.0170 (10)	0.0248 (11)	0.0184 (10)	0.0056 (8)	0.0080 (8)	0.0089 (8)
C16	0.0178 (10)	0.0201 (10)	0.0185 (10)	−0.0009 (8)	0.0049 (8)	0.0078 (8)
C17	0.0204 (10)	0.0162 (10)	0.0155 (9)	0.0042 (8)	0.0037 (8)	0.0063 (8)
C18	0.0165 (10)	0.0206 (10)	0.0157 (9)	0.0052 (8)	0.0056 (8)	0.0082 (8)
C19	0.0167 (10)	0.0187 (10)	0.0147 (9)	0.0034 (8)	0.0058 (8)	0.0072 (8)
C20	0.0173 (10)	0.0155 (9)	0.0136 (9)	0.0032 (8)	0.0085 (8)	0.0019 (8)
C21	0.0194 (10)	0.0179 (10)	0.0164 (10)	0.0043 (8)	0.0088 (8)	0.0047 (8)
C22	0.0252 (11)	0.0187 (10)	0.0202 (10)	0.0018 (8)	0.0124 (9)	0.0067 (8)
C23	0.0186 (10)	0.0253 (11)	0.0256 (11)	0.0010 (9)	0.0130 (9)	0.0056 (9)
C24	0.0174 (10)	0.0248 (11)	0.0200 (10)	0.0059 (8)	0.0085 (8)	0.0051 (9)
C25	0.0191 (10)	0.0203 (10)	0.0163 (10)	0.0056 (8)	0.0096 (8)	0.0056 (8)
C26	0.0166 (10)	0.0117 (9)	0.0206 (10)	0.0053 (7)	0.0109 (8)	0.0054 (8)
C27	0.0130 (9)	0.0204 (10)	0.0182 (10)	0.0054 (8)	0.0091 (8)	0.0063 (8)
C28	0.0144 (9)	0.0192 (10)	0.0173 (10)	0.0038 (8)	0.0079 (8)	0.0041 (8)
C29	0.0185 (10)	0.0205 (10)	0.0201 (10)	0.0073 (8)	0.0105 (8)	0.0079 (8)
C30	0.0203 (10)	0.0176 (10)	0.0253 (11)	0.0057 (8)	0.0143 (9)	0.0052 (8)
C31	0.0174 (10)	0.0216 (10)	0.0170 (10)	0.0015 (8)	0.0094 (8)	0.0018 (8)
C32	0.0161 (10)	0.0232 (10)	0.0170 (10)	0.0052 (8)	0.0081 (8)	0.0075 (8)
C33	0.0117 (9)	0.0199 (10)	0.0179 (10)	0.0055 (8)	0.0082 (8)	0.0058 (8)

Geometric parameters (Å, º) top

Dy1—O14ⁱ	2.3257 (13)	C3—H3A	0.9300
Dy1—O7ⁱ	2.3288 (14)	C4—C5	1.400 (3)
Dy1—O13	2.3362 (13)	C4—H4	0.9300
Dy1—O1	2.3865 (14)	C5—C6	1.437 (3)
Dy1—O8	2.4339 (14)	C6—C7	1.345 (4)
Dy1—O2	2.4702 (14)	C6—H6A	0.9300
Dy1—N2	2.4891 (16)	C7—C8	1.430 (3)
Dy1—N1	2.5593 (17)	C7—H7	0.9300
Dy1—O7	2.7576 (14)	C8—C9	1.404 (3)
Dy1—C19	2.768 (2)	C8—C12	1.410 (3)
Dy1—C26	2.9258 (19)	C9—C10	1.370 (3)
O1—C19	1.259 (3)	C9—H9A	0.9300
O2—C19	1.260 (2)	C10—C11	1.394 (3)
O3—N3	1.222 (3)	C10—H10A	0.9300
O4—N3	1.219 (2)	C11—H11	0.9300
O5—N4	1.232 (2)	C13—C18	1.386 (3)
O6—N4	1.218 (3)	C13—C14	1.390 (3)
O7—C26	1.258 (2)	C13—C19	1.504 (3)
O7—Dy1ⁱ	2.3287 (14)	C14—C15	1.381 (3)
O8—C26	1.250 (2)	C14—H14	0.9300
O9—N5	1.226 (3)	C15—C16	1.384 (3)
O10—N5	1.226 (3)	C16—C17	1.376 (3)
O11—N6	1.223 (3)	C16—H16A	0.9300
O12—N6	1.222 (3)	C17—C18	1.383 (3)
O13—C33	1.258 (2)	C18—H18	0.9300
O14—C33	1.251 (2)	C20—C21	1.388 (3)
O14—Dy1ⁱ	2.3256 (13)	C20—C25	1.390 (3)
O15—N7	1.224 (2)	C20—C26	1.501 (3)
O16—N7	1.220 (2)	C21—C22	1.382 (3)
O17—N8	1.218 (3)	C21—H21	0.9300
O18—N8	1.220 (3)	C22—C23	1.383 (3)
N1—C2	1.328 (3)	C23—C24	1.379 (3)
N1—C1	1.364 (3)	C23—H23	0.9300
N2—C11	1.328 (3)	C24—C25	1.383 (3)
N2—C12	1.359 (3)	C25—H25	0.9300
N3—C15	1.472 (3)	C27—C32	1.392 (3)
N4—C17	1.466 (3)	C27—C28	1.393 (3)
N5—C22	1.472 (3)	C27—C33	1.510 (3)
N6—C24	1.470 (3)	C28—C29	1.381 (3)
N7—C29	1.473 (3)	C28—H28	0.9300
N8—C31	1.481 (3)	C29—C30	1.385 (3)
C1—C5	1.410 (3)	C30—C31	1.377 (3)
C1—C12	1.437 (3)	C30—H30	0.9300
C2—C3	1.398 (3)	C31—C32	1.385 (3)
C2—H2	0.9300	C32—H32	0.9300
C3—C4	1.365 (3)

O14ⁱ—Dy1—O7ⁱ	75.04 (5)	C3—C4—C5	119.7 (2)
O14ⁱ—Dy1—O13	132.09 (5)	C3—C4—H4	120.1
O7ⁱ—Dy1—O13	75.54 (5)	C5—C4—H4	120.1
O14ⁱ—Dy1—O1	75.25 (5)	C4—C5—C1	117.5 (2)
O7ⁱ—Dy1—O1	84.47 (5)	C4—C5—C6	123.7 (2)
O13—Dy1—O1	137.40 (5)	C1—C5—C6	118.8 (2)
O14ⁱ—Dy1—O8	87.69 (5)	C7—C6—C5	121.7 (2)
O7ⁱ—Dy1—O8	123.10 (5)	C7—C6—H6A	119.1
O13—Dy1—O8	77.86 (5)	C5—C6—H6A	119.1
O1—Dy1—O8	142.85 (5)	C6—C7—C8	121.1 (2)
O14ⁱ—Dy1—O2	124.20 (5)	C6—C7—H7	119.5
O7ⁱ—Dy1—O2	78.34 (5)	C8—C7—H7	119.5
O13—Dy1—O2	84.98 (5)	C9—C8—C12	117.9 (2)
O1—Dy1—O2	53.97 (5)	C9—C8—C7	123.3 (2)
O8—Dy1—O2	146.92 (5)	C12—C8—C7	118.9 (2)
O14ⁱ—Dy1—N2	142.26 (5)	C10—C9—C8	119.5 (2)
O7ⁱ—Dy1—N2	142.06 (5)	C10—C9—H9A	120.2
O13—Dy1—N2	77.89 (5)	C8—C9—H9A	120.2
O1—Dy1—N2	97.54 (5)	C9—C10—C11	118.9 (2)
O8—Dy1—N2	76.05 (5)	C9—C10—H10A	120.6
O2—Dy1—N2	72.78 (5)	C11—C10—H10A	120.6
O14ⁱ—Dy1—N1	77.58 (5)	N2—C11—C10	123.4 (2)
O7ⁱ—Dy1—N1	148.90 (5)	N2—C11—H11	118.3
O13—Dy1—N1	135.04 (5)	C10—C11—H11	118.3
O1—Dy1—N1	74.49 (5)	N2—C12—C8	122.0 (2)
O8—Dy1—N1	69.67 (5)	N2—C12—C1	117.75 (18)
O2—Dy1—N1	105.85 (5)	C8—C12—C1	120.21 (19)
N2—Dy1—N1	64.90 (6)	C18—C13—C14	120.33 (18)
O14ⁱ—Dy1—O7	67.13 (4)	C18—C13—C19	119.01 (18)
O7ⁱ—Dy1—O7	73.78 (5)	C14—C13—C19	120.65 (18)
O13—Dy1—O7	68.80 (4)	C15—C14—C13	118.76 (19)
O1—Dy1—O7	140.13 (5)	C15—C14—H14	120.6
O8—Dy1—O7	49.78 (4)	C13—C14—H14	120.6
O2—Dy1—O7	145.50 (4)	C14—C15—C16	122.8 (2)
N2—Dy1—O7	120.20 (5)	C14—C15—N3	119.53 (19)
N1—Dy1—O7	108.53 (5)	C16—C15—N3	117.71 (18)
O14ⁱ—Dy1—C19	99.17 (5)	C17—C16—C15	116.38 (19)
O7ⁱ—Dy1—C19	78.59 (5)	C17—C16—H16A	121.8
O13—Dy1—C19	110.97 (5)	C15—C16—H16A	121.8
O1—Dy1—C19	27.00 (6)	C16—C17—C18	123.46 (19)
O8—Dy1—C19	158.31 (5)	C16—C17—N4	117.99 (18)
O2—Dy1—C19	27.08 (5)	C18—C17—N4	118.54 (19)
N2—Dy1—C19	86.28 (5)	C17—C18—C13	118.28 (19)
N1—Dy1—C19	91.60 (6)	C17—C18—H18	120.9
O7—Dy1—C19	151.49 (5)	C13—C18—H18	120.9
O14ⁱ—Dy1—C26	73.35 (5)	O1—C19—O2	122.14 (18)
O7ⁱ—Dy1—C26	99.12 (5)	O1—C19—C13	118.19 (18)
O13—Dy1—C26	75.02 (5)	O2—C19—C13	119.66 (18)
O1—Dy1—C26	146.20 (5)	O1—C19—Dy1	59.36 (10)
O8—Dy1—C26	24.86 (5)	O2—C19—Dy1	63.16 (10)
O2—Dy1—C26	159.78 (5)	C13—C19—Dy1	172.09 (13)
N2—Dy1—C26	99.60 (5)	C21—C20—C25	120.43 (18)
N1—Dy1—C26	86.78 (5)	C21—C20—C26	118.89 (18)
O7—Dy1—C26	25.35 (5)	C25—C20—C26	120.47 (18)
C19—Dy1—C26	172.52 (6)	C22—C21—C20	119.00 (19)
C19—O1—Dy1	93.64 (12)	C22—C21—H21	120.5
C19—O2—Dy1	89.76 (11)	C20—C21—H21	120.5
C26—O7—Dy1ⁱ	168.95 (13)	C21—C22—C23	122.4 (2)
C26—O7—Dy1	84.82 (11)	C21—C22—N5	118.0 (2)
Dy1ⁱ—O7—Dy1	106.22 (5)	C23—C22—N5	119.59 (19)
C26—O8—Dy1	100.17 (12)	C24—C23—C22	116.61 (19)
C33—O13—Dy1	135.20 (12)	C24—C23—H23	121.7
C33—O14—Dy1ⁱ	133.49 (13)	C22—C23—H23	121.7
C2—N1—C1	117.54 (18)	C23—C24—C25	123.4 (2)
C2—N1—Dy1	124.43 (14)	C23—C24—N6	118.17 (19)
C1—N1—Dy1	117.88 (13)	C25—C24—N6	118.37 (19)
C11—N2—C12	118.20 (18)	C24—C25—C20	118.00 (19)
C11—N2—Dy1	120.97 (13)	C24—C25—H25	121.0
C12—N2—Dy1	120.55 (13)	C20—C25—H25	121.0
O4—N3—O3	123.91 (19)	O8—C26—O7	123.07 (18)
O4—N3—C15	118.31 (19)	O8—C26—C20	117.14 (17)
O3—N3—C15	117.78 (18)	O7—C26—C20	119.71 (17)
O6—N4—O5	124.60 (19)	O8—C26—Dy1	54.96 (10)
O6—N4—C17	118.01 (17)	O7—C26—Dy1	69.83 (10)
O5—N4—C17	117.39 (19)	C20—C26—Dy1	161.56 (13)
O9—N5—O10	124.19 (19)	C32—C27—C28	119.90 (18)
O9—N5—C22	117.89 (18)	C32—C27—C33	119.84 (18)
O10—N5—C22	117.9 (2)	C28—C27—C33	120.22 (17)
O12—N6—O11	124.3 (2)	C29—C28—C27	119.12 (18)
O12—N6—C24	118.18 (17)	C29—C28—H28	120.4
O11—N6—C24	117.53 (19)	C27—C28—H28	120.4
O16—N7—O15	124.06 (18)	C28—C29—C30	122.62 (19)
O16—N7—C29	118.20 (17)	C28—C29—N7	119.01 (18)
O15—N7—C29	117.72 (17)	C30—C29—N7	118.31 (18)
O17—N8—O18	124.96 (19)	C31—C30—C29	116.52 (19)
O17—N8—C31	117.57 (19)	C31—C30—H30	121.7
O18—N8—C31	117.47 (18)	C29—C30—H30	121.7
N1—C1—C5	122.7 (2)	C30—C31—C32	123.41 (19)
N1—C1—C12	117.96 (18)	C30—C31—N8	117.68 (19)
C5—C1—C12	119.38 (19)	C32—C31—N8	118.90 (19)
N1—C2—C3	123.4 (2)	C31—C32—C27	118.40 (19)
N1—C2—H2	118.3	C31—C32—H32	120.8
C3—C2—H2	118.3	C27—C32—H32	120.8
C4—C3—C2	119.1 (2)	O14—C33—O13	126.95 (19)
C4—C3—H3A	120.4	O14—C33—C27	116.68 (17)
C2—C3—H3A	120.4	O13—C33—C27	116.36 (17)

O14ⁱ—Dy1—O1—C19	151.62 (13)	C5—C1—C12—C8	−0.6 (3)
O7ⁱ—Dy1—O1—C19	75.66 (12)	C18—C13—C14—C15	0.3 (3)
O13—Dy1—O1—C19	14.09 (15)	C19—C13—C14—C15	179.34 (18)
O8—Dy1—O1—C19	−143.01 (11)	C13—C14—C15—C16	0.8 (3)
O2—Dy1—O1—C19	−3.93 (11)	C13—C14—C15—N3	−179.69 (18)
N2—Dy1—O1—C19	−66.19 (12)	O4—N3—C15—C14	179.0 (2)
N1—Dy1—O1—C19	−127.46 (13)	O3—N3—C15—C14	−0.8 (3)
O7—Dy1—O1—C19	132.03 (11)	O4—N3—C15—C16	−1.6 (3)
C26—Dy1—O1—C19	173.81 (11)	O3—N3—C15—C16	178.6 (2)
O14ⁱ—Dy1—O2—C19	−25.03 (13)	C14—C15—C16—C17	−1.1 (3)
O7ⁱ—Dy1—O2—C19	−87.70 (11)	N3—C15—C16—C17	179.44 (18)
O13—Dy1—O2—C19	−163.95 (12)	C15—C16—C17—C18	0.2 (3)
O1—Dy1—O2—C19	3.92 (11)	C15—C16—C17—N4	179.58 (18)
O8—Dy1—O2—C19	137.48 (12)	O6—N4—C17—C16	153.44 (19)
N2—Dy1—O2—C19	117.20 (12)	O5—N4—C17—C16	−27.0 (3)
N1—Dy1—O2—C19	60.54 (12)	O6—N4—C17—C18	−27.1 (3)
O7—Dy1—O2—C19	−124.20 (11)	O5—N4—C17—C18	152.43 (19)
C26—Dy1—O2—C19	−172.44 (14)	C16—C17—C18—C13	0.9 (3)
O14ⁱ—Dy1—O7—C26	99.42 (11)	N4—C17—C18—C13	−178.48 (17)
O7ⁱ—Dy1—O7—C26	179.69 (13)	C14—C13—C18—C17	−1.2 (3)
O13—Dy1—O7—C26	−99.87 (11)	C19—C13—C18—C17	179.82 (17)
O1—Dy1—O7—C26	120.03 (11)	Dy1—O1—C19—O2	7.4 (2)
O8—Dy1—O7—C26	−7.99 (10)	Dy1—O1—C19—C13	−171.36 (15)
O2—Dy1—O7—C26	−142.97 (11)	Dy1—O2—C19—O1	−7.11 (19)
N2—Dy1—O7—C26	−38.96 (12)	Dy1—O2—C19—C13	171.61 (16)
N1—Dy1—O7—C26	32.23 (12)	C18—C13—C19—O1	2.3 (3)
C19—Dy1—O7—C26	164.97 (12)	C14—C13—C19—O1	−176.74 (18)
O14ⁱ—Dy1—O7—Dy1ⁱ	−80.26 (6)	C18—C13—C19—O2	−176.48 (18)
O7ⁱ—Dy1—O7—Dy1ⁱ	0.0	C14—C13—C19—O2	4.5 (3)
O13—Dy1—O7—Dy1ⁱ	80.44 (6)	O14ⁱ—Dy1—C19—O1	−27.75 (12)
O1—Dy1—O7—Dy1ⁱ	−59.66 (9)	O7ⁱ—Dy1—C19—O1	−100.33 (12)
O8—Dy1—O7—Dy1ⁱ	172.32 (8)	O13—Dy1—C19—O1	−169.84 (11)
O2—Dy1—O7—Dy1ⁱ	37.35 (10)	O8—Dy1—C19—O1	79.41 (19)
N2—Dy1—O7—Dy1ⁱ	141.36 (6)	O2—Dy1—C19—O1	173.01 (19)
N1—Dy1—O7—Dy1ⁱ	−147.46 (5)	N2—Dy1—C19—O1	114.64 (12)
C19—Dy1—O7—Dy1ⁱ	−14.72 (13)	N1—Dy1—C19—O1	49.92 (12)
C26—Dy1—O7—Dy1ⁱ	−179.69 (13)	O7—Dy1—C19—O1	−85.92 (15)
O14ⁱ—Dy1—O8—C26	−53.49 (12)	O14ⁱ—Dy1—C19—O2	159.24 (11)
O7ⁱ—Dy1—O8—C26	16.95 (14)	O7ⁱ—Dy1—C19—O2	86.66 (11)
O13—Dy1—O8—C26	80.52 (12)	O13—Dy1—C19—O2	17.15 (12)
O1—Dy1—O8—C26	−115.11 (13)	O1—Dy1—C19—O2	−173.01 (19)
O2—Dy1—O8—C26	140.91 (12)	O8—Dy1—C19—O2	−93.60 (18)
N2—Dy1—O8—C26	160.86 (13)	N2—Dy1—C19—O2	−58.36 (11)
N1—Dy1—O8—C26	−131.10 (13)	N1—Dy1—C19—O2	−123.08 (11)
O7—Dy1—O8—C26	8.14 (11)	O7—Dy1—C19—O2	101.07 (14)
C19—Dy1—O8—C26	−162.75 (14)	C25—C20—C21—C22	−0.5 (3)
O14ⁱ—Dy1—O13—C33	−8.6 (2)	C26—C20—C21—C22	−175.35 (18)
O7ⁱ—Dy1—O13—C33	45.06 (18)	C20—C21—C22—C23	3.1 (3)
O1—Dy1—O13—C33	109.74 (18)	C20—C21—C22—N5	−176.46 (18)
O8—Dy1—O13—C33	−84.17 (18)	O9—N5—C22—C21	2.3 (3)
O2—Dy1—O13—C33	124.29 (18)	O10—N5—C22—C21	−179.54 (19)
N2—Dy1—O13—C33	−162.27 (19)	O9—N5—C22—C23	−177.3 (2)
N1—Dy1—O13—C33	−128.25 (17)	O10—N5—C22—C23	0.9 (3)
O7—Dy1—O13—C33	−32.85 (17)	C21—C22—C23—C24	−2.8 (3)
C19—Dy1—O13—C33	116.54 (18)	N5—C22—C23—C24	176.79 (19)
C26—Dy1—O13—C33	−58.74 (18)	C22—C23—C24—C25	−0.2 (3)
O14ⁱ—Dy1—N1—C2	7.15 (15)	C22—C23—C24—N6	178.21 (19)
O7ⁱ—Dy1—N1—C2	−21.6 (2)	O12—N6—C24—C23	162.5 (2)
O13—Dy1—N1—C2	145.80 (14)	O11—N6—C24—C23	−19.1 (3)
O1—Dy1—N1—C2	−70.76 (16)	O12—N6—C24—C25	−19.1 (3)
O8—Dy1—N1—C2	99.30 (16)	O11—N6—C24—C25	159.4 (2)
O2—Dy1—N1—C2	−115.25 (16)	C23—C24—C25—C20	2.6 (3)
N2—Dy1—N1—C2	−177.03 (17)	N6—C24—C25—C20	−175.74 (18)
O7—Dy1—N1—C2	67.58 (16)	C21—C20—C25—C24	−2.3 (3)
C19—Dy1—N1—C2	−91.89 (16)	C26—C20—C25—C24	172.53 (18)
C26—Dy1—N1—C2	80.80 (16)	Dy1—O8—C26—O7	−16.4 (2)
O14ⁱ—Dy1—N1—C1	−168.30 (14)	Dy1—O8—C26—C20	160.48 (14)
O7ⁱ—Dy1—N1—C1	162.97 (12)	Dy1ⁱ—O7—C26—O8	−167.3 (5)
O13—Dy1—N1—C1	−29.65 (17)	Dy1—O7—C26—O8	14.28 (18)
O1—Dy1—N1—C1	113.79 (14)	Dy1ⁱ—O7—C26—C20	15.9 (8)
O8—Dy1—N1—C1	−76.15 (14)	Dy1—O7—C26—C20	−162.55 (16)
O2—Dy1—N1—C1	69.30 (14)	Dy1ⁱ—O7—C26—Dy1	178.4 (7)
N2—Dy1—N1—C1	7.52 (13)	C21—C20—C26—O8	40.1 (3)
O7—Dy1—N1—C1	−107.87 (13)	C25—C20—C26—O8	−134.8 (2)
C19—Dy1—N1—C1	92.66 (14)	C21—C20—C26—O7	−142.91 (19)
C26—Dy1—N1—C1	−94.65 (14)	C25—C20—C26—O7	42.2 (3)
O14ⁱ—Dy1—N2—C11	−175.70 (13)	C21—C20—C26—Dy1	99.9 (4)
O7ⁱ—Dy1—N2—C11	18.05 (19)	C25—C20—C26—Dy1	−74.9 (5)
O13—Dy1—N2—C11	−28.27 (14)	O14ⁱ—Dy1—C26—O8	123.04 (12)
O1—Dy1—N2—C11	108.70 (15)	O7ⁱ—Dy1—C26—O8	−165.68 (12)
O8—Dy1—N2—C11	−108.59 (15)	O13—Dy1—C26—O8	−93.42 (12)
O2—Dy1—N2—C11	60.17 (15)	O1—Dy1—C26—O8	100.63 (14)
N1—Dy1—N2—C11	177.62 (16)	O2—Dy1—C26—O8	−84.67 (19)
O7—Dy1—N2—C11	−84.71 (15)	N2—Dy1—C26—O8	−18.82 (13)
C19—Dy1—N2—C11	84.11 (15)	N1—Dy1—C26—O8	45.05 (12)
C26—Dy1—N2—C11	−100.55 (15)	O7—Dy1—C26—O8	−165.38 (19)
O14ⁱ—Dy1—N2—C12	−1.93 (18)	O14ⁱ—Dy1—C26—O7	−71.58 (11)
O7ⁱ—Dy1—N2—C12	−168.19 (12)	O7ⁱ—Dy1—C26—O7	−0.30 (13)
O13—Dy1—N2—C12	145.49 (14)	O13—Dy1—C26—O7	71.95 (11)
O1—Dy1—N2—C12	−77.54 (14)	O1—Dy1—C26—O7	−93.99 (13)
O8—Dy1—N2—C12	65.18 (14)	O8—Dy1—C26—O7	165.38 (19)
O2—Dy1—N2—C12	−126.07 (14)	O2—Dy1—C26—O7	80.71 (18)
N1—Dy1—N2—C12	−8.62 (13)	N2—Dy1—C26—O7	146.55 (11)
O7—Dy1—N2—C12	89.06 (14)	N1—Dy1—C26—O7	−149.57 (11)
C19—Dy1—N2—C12	−102.13 (14)	O14ⁱ—Dy1—C26—C20	53.0 (4)
C26—Dy1—N2—C12	73.21 (14)	O7ⁱ—Dy1—C26—C20	124.3 (4)
C2—N1—C1—C5	−1.3 (3)	O13—Dy1—C26—C20	−163.5 (4)
Dy1—N1—C1—C5	174.49 (14)	O1—Dy1—C26—C20	30.6 (5)
C2—N1—C1—C12	177.97 (18)	O8—Dy1—C26—C20	−70.0 (4)
Dy1—N1—C1—C12	−6.3 (2)	O2—Dy1—C26—C20	−154.7 (4)
C1—N1—C2—C3	0.7 (3)	N2—Dy1—C26—C20	−88.9 (4)
Dy1—N1—C2—C3	−174.77 (15)	N1—Dy1—C26—C20	−25.0 (4)
N1—C2—C3—C4	0.7 (3)	O7—Dy1—C26—C20	124.6 (5)
C2—C3—C4—C5	−1.5 (3)	C32—C27—C28—C29	−1.7 (3)
C3—C4—C5—C1	0.9 (3)	C33—C27—C28—C29	−179.22 (18)
C3—C4—C5—C6	−178.8 (2)	C27—C28—C29—C30	0.9 (3)
N1—C1—C5—C4	0.5 (3)	C27—C28—C29—N7	178.08 (18)
C12—C1—C5—C4	−178.73 (18)	O16—N7—C29—C28	−178.27 (19)
N1—C1—C5—C6	−179.83 (19)	O15—N7—C29—C28	0.1 (3)
C12—C1—C5—C6	0.9 (3)	O16—N7—C29—C30	−0.9 (3)
C4—C5—C6—C7	178.9 (2)	O15—N7—C29—C30	177.42 (19)
C1—C5—C6—C7	−0.7 (3)	C28—C29—C30—C31	0.0 (3)
C5—C6—C7—C8	0.1 (4)	N7—C29—C30—C31	−177.21 (18)
C6—C7—C8—C9	−179.0 (2)	C29—C30—C31—C32	−0.1 (3)
C6—C7—C8—C12	0.2 (3)	C29—C30—C31—N8	179.07 (18)
C12—C8—C9—C10	−2.2 (3)	O17—N8—C31—C30	8.0 (3)
C7—C8—C9—C10	177.1 (2)	O18—N8—C31—C30	−172.3 (2)
C8—C9—C10—C11	0.9 (3)	O17—N8—C31—C32	−172.78 (19)
C12—N2—C11—C10	−2.7 (3)	O18—N8—C31—C32	6.9 (3)
Dy1—N2—C11—C10	171.18 (15)	C30—C31—C32—C27	−0.7 (3)
C9—C10—C11—N2	1.7 (3)	N8—C31—C32—C27	−179.90 (18)
C11—N2—C12—C8	1.3 (3)	C28—C27—C32—C31	1.6 (3)
Dy1—N2—C12—C8	−172.66 (14)	C33—C27—C32—C31	179.17 (18)
C11—N2—C12—C1	−176.93 (17)	Dy1ⁱ—O14—C33—O13	50.0 (3)
Dy1—N2—C12—C1	9.1 (2)	Dy1ⁱ—O14—C33—C27	−128.83 (16)
C9—C8—C12—N2	1.1 (3)	Dy1—O13—C33—O14	−27.4 (3)
C7—C8—C12—N2	−178.17 (19)	Dy1—O13—C33—C27	151.46 (13)
C9—C8—C12—C1	179.28 (18)	C32—C27—C33—O14	9.9 (3)
C7—C8—C12—C1	0.0 (3)	C28—C27—C33—O14	−172.54 (18)
N1—C1—C12—N2	−1.6 (3)	C32—C27—C33—O13	−169.07 (18)
C5—C1—C12—N2	177.65 (17)	C28—C27—C33—O13	8.5 (3)
N1—C1—C12—C8	−179.85 (18)

Symmetry code: (i) −x+2, −y, −z+2.

Experimental details

Crystal data
Chemical formula	[Dy₂(C₇H₃N₂O₆)₆(C₁₂H₈N₂)₂]
M_r	1952.09
Crystal system, space group	Triclinic, P1
Temperature (K)	296
a, b, c (Å)	11.9569 (4), 12.8636 (4), 13.1187 (4)
α, β, γ (°)	104.24 (5), 113.96 (5), 100.46 (5)
V (Å³)	1694.6 (12)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	2.31
Crystal size (mm)	0.15 × 0.13 × 0.12

Data collection
Diffractometer	Bruker APEXII CCD
Absorption correction	Multi-scan (SADABS; Sheldrick, 1997)
T_min, T_max	0.724, 0.769
No. of measured, independent and observed [I > 2σ(I)] reflections	8296, 5771, 5624
R_int	0.011
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.016, 0.041, 1.03
No. of reflections	5771
No. of parameters	541
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.43, −0.78

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and local programs.

Acknowledgements

This work was supported financially by the National Science Foundation of Handan College (No. 10003) and the Scientific Research and Development of Hebei Province (No. 09215135). The authors thank Mr Xiu-Guang Wang (Tianjin Normal University) for help with the structure determination.

References

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