Poly[[diaquabis(2,2′-bipyridine-κ2N,N′)(μ3-5-hydroxyisophthalato-κ5O1,O1′:O3,O3′:O3′)(μ3-5-hydroxy­isophthalato-κ4O1,O1′:O3:O3′)(μ2-5-hydroxyisophthalato-κ3O1,O1′:O3)didysprosium(III)] dihydrate]

Zhang, Y.-L.

doi:10.1107/S1600536811039080

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 10| October 2011| Pages m1473-m1474

https://doi.org/10.1107/S1600536811039080

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Poly[[diaquabis(2,2′-bipyridine-κ²N,N′)(μ₃-5-hydroxyisophthalato-κ⁵O¹,O^1′:O³,O^3′:O^3′)(μ₃-5-hydroxyisophthalato-κ⁴O¹,O^1′:O³:O^3′)(μ₂-5-hydroxyisophthalato-κ³O¹,O^1′:O³)didysprosium(III)] dihydrate]

Yan-Lin Zhang ^a ^*

^aSchool of Chemistry and Environment, South China Normal University, Guangzhou 510006, People's Republic of China
^*Correspondence e-mail: zhangyl75@yahoo.com.cn

(Received 22 August 2011; accepted 23 September 2011; online 30 September 2011)

The polymeric title compound, {[Dy₂(C₈H₄O₅)₃(C₁₀H₈N₂)₂(H₂O)₂]·2H₂O}_n, contains two independent Dy^III ions, both of which are nine-coordinated in a distorted tricapped trigonal–prismatic geometry. One Dy^III ion is coordinated by five 5-hydroxyisophthalate (hip) ligands and one 2,2′-bipyridine (bpy) ligand and the other by three hip ligands, one bpy ligand and two water molecules. The Dy^III ions are bridged by the carboxylate groups of the hip ligands, forming a three-dimensional framework. O—H⋯O hydrogen bonds are present in the crystal structure.

Related literature

For related structures, see: Li et al. (2007 ); Plater et al. (2001 ); Zhuo et al. (2006a ,b ).

Experimental

Crystal data

[Dy₂(C₈H₄O₅)₃(C₁₀H₈N₂)₂(H₂O)₂]·2H₂O
M_r = 1249.77
Triclinic, $[P \overline 1]$
a = 11.3736 (5) Å
b = 12.0349 (6) Å
c = 17.8360 (8) Å
α = 91.310 (1)°
β = 103.187 (1)°
γ = 106.505 (1)°
V = 2269.00 (18) Å³
Z = 2
Mo Kα radiation
μ = 3.35 mm⁻¹
T = 298 K
0.25 × 0.24 × 0.21 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ) T_min = 0.488, T_max = 0.540
11732 measured reflections
8024 independent reflections
7052 reflections with I > 2σ(I)
R_int = 0.020

Refinement

R[F² > 2σ(F²)] = 0.035
wR(F²) = 0.094
S = 1.06
8024 reflections
624 parameters
252 restraints
H-atom parameters constrained
Δρ_max = 2.65 e Å⁻³
Δρ_min = −1.25 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5⋯O4Wⁱ	0.82	2.15	2.910 (11)	154
O10—H10A⋯O2ⁱⁱ	0.82	1.95	2.761 (6)	168
O15—H15⋯O1ⁱⁱⁱ	0.82	1.92	2.718 (6)	163
O1W—H1WA⋯O8^iv	0.85	1.84	2.609 (6)	150
O1W—H1WB⋯O3Wⁱⁱⁱ	0.85	2.01	2.717 (7)	141
O2W—H2WA⋯O11	0.85	2.15	2.676 (6)	120
O2W—H2WB⋯O7ⁱⁱ	0.85	1.86	2.689 (6)	164
O3W—H3WA⋯O4Wⁱⁱⁱ	0.85	1.99	2.744 (9)	147
O3W—H3WB⋯O8^v	0.85	2.03	2.832 (9)	156
O4W—H4WA⋯O6^vi	0.85	1.96	2.809 (8)	175
O4W—H4WB⋯O12	0.85	2.20	2.801 (8)	128
Symmetry codes: (i) x, y+1, z; (ii) -x+1, -y+2, -z+1; (iii) -x+1, -y+1, -z+1; (iv) x+1, y, z+1; (v) x+1, y, z; (vi) -x, -y+1, -z+1.

Data collection: APEX2 (Bruker, 2007 ); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999 ) and SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536811039080/hy2467sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811039080/hy2467Isup2.hkl

checkCIF report

Comment top

In recent years, in situ metal/ligand reactions have been widely investigated for the discovery of new organic reactions and the elucidation of reaction mechanism, as well as the generation of novel coordination polymers. There is currently much interest in employing polycarboxylate ligands with O donors and bipyridine ligands with N donors to design metal coordination polymers with intriguing structures and potential applications. Particular attention has been paid to 5-hydroxyisophthalate and 2,2'-bipyridine ligands; they have five O coordination sites and two N coordination sites, respectively, and thus can potentially afford different coordination modes in multicoordinated ways with transition metal ions (Li et al., 2007; Plater et al., 2001; Zhuo et al., 2006a,b) to form new metal coordination polymers with various structures and interesting properties. In this paper, we report the crystal structure of the title compound, which was synthesized under hydrothermal conditions.

As shown in Fig. 1, both Dy^III ions exhibit a distorted tricapped trigonal prismatic geometry. One Dy^III ion is coordinated by five 5-hydroxyisophthalate (hip) ligands and one 2,2'-bipyridine (bpy) ligand and the other is by three hip ligands, one bpy ligand and two water molecules. The Dy—O bond lengths range from 2.287 (4) to 2.818 (4) Å and the Dy—N bond lengths range from 2.545 (5) to 2.628 (5) Å. In the crystal, the Dy^III ions are bridged by the carboxylate groups of the hip ligands, forming a three-dimensional framework (Fig. 2). O—H···O hydrogen bonds are present (Table 1).

Related literature top

For related structures, see: Li et al. (2007); Plater et al. (2001); Zhuo et al. (2006a,b).

Experimental top

A mixture of Dy₂O₃ (0.363 g, 1 mmol), 5-hydroxyisophthalic acid (0.182 g, 1 mmol), 2,2'-bipyridine (0.132 g, 1 mmol) and water (10 ml) in the presence of HClO₄ (0.039 g, 0.385 mmol) was stirred vigorously for 30 min and then sealed in a 20 ml Teflon-lined stainless-steel autoclave. The autoclave was heated and maintained at 433 K for 50 h and then cooled to room temperature at 5 K h^-1. Colorless block crystals were obtained.

Structure description top

For related structures, see: Li et al. (2007); Plater et al. (2001); Zhuo et al. (2006a,b).

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999) and SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The asymmetric unit of the title compound. Displacement ellipsoids are drawn at the 30% probability level. [Symmetry codes: (i) x+1, y, 1+z; (ii) -x, 2-y, 1-z; (iii) -x, 1-y, 1-z; (iv) -x, 1+y, z.]
	Fig. 2. A view of the three-dimensional framework. Hydrogen bonds are shown as dashed lines.

Poly[[diaquabis(2,2'-bipyridine-κ²N,N')(µ₃-5- hydroxyisophthalato- κ⁵O¹,O^1':O³,O^3':O^3')(µ₃- 5-hydroxyisophthalato- κ⁴O¹,O^1':O³:O^3')(µ₂-5- hydroxyisophthalato-κ³O¹,O^1':O³)didysprosium(III)] dihydrate] top

Crystal data top

[Dy₂(C₈H₄O₅)₃(C₁₀H₈N₂)₂(H₂O)₂]·2H₂O	Z = 2
M_r = 1249.77	F(000) = 1224
Triclinic, P1	D_x = 1.829 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 11.3736 (5) Å	Cell parameters from 7036 reflections
b = 12.0349 (6) Å	θ = 2.3–25.2°
c = 17.8360 (8) Å	µ = 3.35 mm⁻¹
α = 91.310 (1)°	T = 298 K
β = 103.187 (1)°	Block, colourless
γ = 106.505 (1)°	0.25 × 0.24 × 0.21 mm
V = 2269.00 (18) Å³

Data collection top

Bruker APEXII CCD diffractometer	8024 independent reflections
Radiation source: fine-focus sealed tube	7052 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.020
φ and ω scans	θ_max = 25.2°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −11→13
T_min = 0.488, T_max = 0.540	k = −14→12
11732 measured reflections	l = −21→14

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)] = 0.035	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.094	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0438P)² + 9.6294P] where P = (F_o² + 2F_c²)/3
8024 reflections	(Δ/σ)_max = 0.001
624 parameters	Δρ_max = 2.65 e Å⁻³
252 restraints	Δρ_min = −1.25 e Å⁻³

Crystal data top

[Dy₂(C₈H₄O₅)₃(C₁₀H₈N₂)₂(H₂O)₂]·2H₂O	γ = 106.505 (1)°
M_r = 1249.77	V = 2269.00 (18) Å³
Triclinic, P1	Z = 2
a = 11.3736 (5) Å	Mo Kα radiation
b = 12.0349 (6) Å	µ = 3.35 mm⁻¹
c = 17.8360 (8) Å	T = 298 K
α = 91.310 (1)°	0.25 × 0.24 × 0.21 mm
β = 103.187 (1)°

Data collection top

Bruker APEXII CCD diffractometer	8024 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2001)	7052 reflections with I > 2σ(I)
T_min = 0.488, T_max = 0.540	R_int = 0.020
11732 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.035	252 restraints
wR(F²) = 0.094	H-atom parameters constrained
S = 1.06	Δρ_max = 2.65 e Å⁻³
8024 reflections	Δρ_min = −1.25 e Å⁻³
624 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
C1	0.4251 (5)	0.8899 (5)	0.7503 (3)	0.0251 (8)
C2	0.3246 (5)	0.8628 (5)	0.6840 (3)	0.0239 (8)
H2	0.3093	0.7969	0.6508	0.029*
C3	0.2482 (5)	0.9350 (5)	0.6685 (3)	0.0244 (8)
C4	0.2704 (5)	1.0328 (5)	0.7175 (3)	0.0293 (9)
H4	0.2188	1.0809	0.7064	0.035*
C5	0.3692 (6)	1.0599 (6)	0.7831 (4)	0.0322 (9)
C6	0.4462 (6)	0.9871 (5)	0.7995 (4)	0.0302 (9)
H6	0.5120	1.0043	0.8440	0.036*
C7	0.5145 (5)	0.8182 (5)	0.7643 (3)	0.0238 (10)
C8	0.1446 (5)	0.9091 (5)	0.5952 (3)	0.0234 (9)
C9	0.0136 (5)	0.8915 (5)	0.1828 (3)	0.0245 (8)
C10	0.1249 (5)	0.9454 (5)	0.1611 (3)	0.0249 (8)
H10	0.1973	0.9860	0.1983	0.030*
C11	0.1270 (5)	0.9381 (5)	0.0836 (3)	0.0249 (8)
C12	0.0188 (5)	0.8775 (5)	0.0280 (3)	0.0249 (8)
H12	0.0204	0.8723	−0.0238	0.030*
C13	−0.0921 (5)	0.8246 (5)	0.0506 (3)	0.0259 (8)
C14	−0.0937 (5)	0.8305 (5)	0.1277 (3)	0.0258 (8)
H14	−0.1673	0.7932	0.1425	0.031*
C15	0.0150 (5)	0.9011 (5)	0.2669 (3)	0.0241 (10)
C16	−0.2103 (5)	0.7609 (5)	−0.0104 (3)	0.0274 (10)
C17	0.5160 (5)	0.4159 (5)	0.6023 (3)	0.0211 (7)
C18	0.3978 (5)	0.3324 (5)	0.5900 (3)	0.0212 (8)
H18	0.3485	0.3307	0.6253	0.025*
C19	0.3540 (5)	0.2526 (5)	0.5257 (3)	0.0201 (7)
C20	0.4278 (5)	0.2559 (5)	0.4717 (3)	0.0216 (8)
H20	0.4007	0.1998	0.4297	0.026*
C21	0.5417 (5)	0.3438 (5)	0.4819 (3)	0.0222 (8)
C22	0.5862 (5)	0.4218 (5)	0.5472 (3)	0.0229 (8)
H22	0.6638	0.4788	0.5544	0.028*
C23	0.2276 (5)	0.1624 (5)	0.5137 (3)	0.0203 (9)
C24	0.5688 (5)	0.4978 (5)	0.6744 (3)	0.0220 (9)
C25	1.0000 (8)	0.7669 (10)	0.8074 (5)	0.0683 (16)
H25	0.9747	0.8291	0.7869	0.082*
C26	1.1267 (8)	0.7756 (10)	0.8224 (6)	0.0719 (14)
H26	1.1856	0.8417	0.8129	0.086*
C27	1.1621 (9)	0.6827 (10)	0.8517 (6)	0.0729 (13)
H27	1.2463	0.6840	0.8608	0.087*
C28	1.0729 (8)	0.5862 (9)	0.8679 (5)	0.0685 (13)
H28	1.0970	0.5233	0.8883	0.082*
C29	0.9474 (8)	0.5858 (8)	0.8531 (5)	0.0610 (12)
C30	0.8518 (8)	0.4909 (8)	0.8756 (5)	0.0602 (12)
C31	0.8801 (9)	0.3964 (8)	0.9129 (5)	0.0648 (12)
H31	0.9610	0.3886	0.9213	0.078*
C32	0.7869 (9)	0.3161 (8)	0.9366 (6)	0.0685 (13)
H32	0.8057	0.2552	0.9631	0.082*
C33	0.6694 (9)	0.3243 (8)	0.9220 (5)	0.0684 (14)
H33	0.6055	0.2697	0.9375	0.082*
C34	0.6460 (9)	0.4171 (8)	0.8831 (5)	0.0661 (16)
H34	0.5638	0.4221	0.8719	0.079*
C35	0.3302 (6)	0.9129 (6)	0.3933 (4)	0.0425 (12)
H35	0.3510	0.9844	0.4219	0.051*
C36	0.4133 (7)	0.8951 (6)	0.3514 (4)	0.0439 (11)
H36	0.4897	0.9515	0.3535	0.053*
C37	0.3786 (7)	0.7913 (6)	0.3068 (4)	0.0416 (10)
H37	0.4285	0.7779	0.2750	0.050*
C38	0.2695 (6)	0.7073 (6)	0.3096 (4)	0.0380 (10)
H38	0.2461	0.6358	0.2807	0.046*
C39	0.1949 (6)	0.7292 (5)	0.3553 (4)	0.0339 (9)
C40	0.0846 (6)	0.6358 (6)	0.3694 (4)	0.0356 (9)
C41	0.0697 (7)	0.5191 (6)	0.3519 (4)	0.0409 (10)
H41	0.1247	0.4972	0.3274	0.049*
C42	−0.0277 (7)	0.4353 (6)	0.3710 (5)	0.0464 (11)
H42	−0.0391	0.3565	0.3601	0.056*
C43	−0.1078 (7)	0.4720 (6)	0.4069 (5)	0.0460 (11)
H43	−0.1743	0.4182	0.4206	0.055*
C44	−0.0871 (6)	0.5902 (6)	0.4219 (4)	0.0422 (12)
H44	−0.1419	0.6141	0.4457	0.051*
Dy1	0.04319 (2)	0.89445 (2)	0.429009 (13)	0.01643 (8)
Dy2	0.67367 (2)	0.67220 (2)	0.800601 (14)	0.01969 (8)
N1	0.9105 (5)	0.6742 (5)	0.8207 (3)	0.0390 (13)
N2	0.7338 (6)	0.4996 (5)	0.8606 (3)	0.0407 (13)
N3	0.0070 (4)	0.6719 (4)	0.4043 (3)	0.0238 (10)
N4	0.2227 (5)	0.8338 (4)	0.3947 (3)	0.0298 (11)
O1	0.4947 (4)	0.7273 (4)	0.7207 (2)	0.0282 (9)
O2	0.6118 (4)	0.8495 (3)	0.8205 (2)	0.0267 (9)
O3	0.0652 (4)	0.9668 (4)	0.5843 (3)	0.0312 (10)
O4	0.1422 (4)	0.8342 (4)	0.5450 (2)	0.0324 (10)
O5	0.3955 (6)	1.1574 (5)	0.8318 (3)	0.072 (2)
H5	0.3461	1.1943	0.8150	0.108*
O6	−0.0618 (4)	0.8244 (4)	0.2938 (2)	0.0256 (9)
O7	0.0951 (4)	0.9848 (4)	0.3114 (2)	0.0307 (9)
O8	−0.3077 (5)	0.7129 (6)	0.0117 (3)	0.0632 (18)
O9	−0.2044 (4)	0.7600 (4)	−0.0800 (2)	0.0281 (9)
O10	0.2343 (4)	0.9872 (4)	0.0599 (2)	0.0352 (10)
H10A	0.2877	1.0299	0.0958	0.053*
O11	0.6748 (4)	0.5741 (4)	0.6827 (2)	0.0324 (10)
O12	0.5103 (4)	0.4909 (4)	0.7272 (2)	0.0283 (9)
O13	0.1492 (3)	0.1884 (3)	0.5452 (2)	0.0263 (9)
O14	0.2080 (3)	0.0689 (3)	0.4735 (2)	0.0247 (8)
O15	0.6135 (4)	0.3572 (4)	0.4296 (2)	0.0368 (11)
H15	0.5706	0.3213	0.3881	0.055*
O1W	0.5317 (4)	0.6243 (4)	0.8801 (2)	0.0377 (11)
H1WA	0.5604	0.6566	0.9261	0.057*
H1WB	0.4515	0.6014	0.8712	0.057*
O2W	0.7608 (4)	0.8059 (4)	0.7123 (2)	0.0337 (10)
H2WA	0.7579	0.7565	0.6765	0.051*
H2WB	0.7932	0.8733	0.6996	0.051*
O3W	0.6892 (5)	0.5249 (5)	0.1047 (4)	0.0671 (17)
H3WA	0.7242	0.5719	0.1452	0.101*
H3WB	0.6780	0.5651	0.0666	0.101*
O4W	0.2982 (7)	0.3417 (7)	0.7652 (4)	0.106 (3)
H4WA	0.2287	0.2884	0.7480	0.160*
H4WB	0.3365	0.3533	0.7291	0.160*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0205 (15)	0.0297 (16)	0.0218 (15)	0.0061 (13)	0.0008 (13)	−0.0021 (14)
C2	0.0201 (16)	0.0278 (17)	0.0217 (16)	0.0068 (14)	0.0016 (14)	−0.0009 (15)
C3	0.0198 (15)	0.0278 (16)	0.0231 (15)	0.0061 (13)	0.0017 (13)	−0.0006 (14)
C4	0.0235 (16)	0.0319 (17)	0.0287 (17)	0.0084 (15)	−0.0007 (15)	−0.0053 (15)
C5	0.0252 (17)	0.0354 (18)	0.0304 (18)	0.0085 (15)	−0.0025 (15)	−0.0083 (16)
C6	0.0234 (16)	0.0344 (18)	0.0274 (17)	0.0074 (15)	−0.0021 (15)	−0.0064 (16)
C7	0.0196 (19)	0.029 (2)	0.0202 (19)	0.0057 (17)	0.0013 (17)	−0.0010 (17)
C8	0.0201 (19)	0.026 (2)	0.021 (2)	0.0038 (17)	0.0030 (17)	0.0034 (17)
C9	0.0239 (15)	0.0292 (16)	0.0168 (15)	0.0044 (13)	0.0027 (13)	−0.0021 (14)
C10	0.0239 (16)	0.0295 (17)	0.0171 (16)	0.0040 (15)	0.0021 (14)	−0.0030 (15)
C11	0.0244 (17)	0.0298 (17)	0.0176 (16)	0.0050 (15)	0.0041 (14)	−0.0023 (15)
C12	0.0256 (16)	0.0295 (17)	0.0171 (16)	0.0057 (14)	0.0040 (14)	−0.0024 (15)
C13	0.0255 (15)	0.0303 (16)	0.0179 (15)	0.0043 (14)	0.0027 (13)	−0.0020 (14)
C14	0.0248 (16)	0.0306 (17)	0.0177 (16)	0.0034 (14)	0.0029 (14)	−0.0013 (15)
C15	0.0237 (19)	0.028 (2)	0.0172 (19)	0.0051 (17)	0.0024 (17)	−0.0017 (17)
C16	0.025 (2)	0.032 (2)	0.020 (2)	0.0041 (17)	0.0021 (17)	−0.0024 (18)
C17	0.0192 (14)	0.0225 (15)	0.0186 (15)	0.0031 (13)	0.0032 (13)	−0.0030 (13)
C18	0.0193 (15)	0.0234 (16)	0.0182 (16)	0.0024 (14)	0.0046 (13)	−0.0039 (14)
C19	0.0180 (14)	0.0230 (15)	0.0169 (14)	0.0032 (13)	0.0033 (12)	−0.0035 (13)
C20	0.0190 (15)	0.0245 (16)	0.0176 (16)	0.0024 (14)	0.0029 (14)	−0.0051 (14)
C21	0.0196 (16)	0.0256 (17)	0.0183 (16)	0.0028 (14)	0.0040 (14)	−0.0030 (14)
C22	0.0199 (16)	0.0253 (17)	0.0193 (16)	0.0013 (14)	0.0036 (14)	−0.0027 (14)
C23	0.0183 (18)	0.0230 (19)	0.0164 (18)	0.0027 (16)	0.0027 (16)	−0.0019 (17)
C24	0.0203 (19)	0.0223 (19)	0.0193 (19)	0.0034 (16)	0.0011 (16)	−0.0022 (17)
C25	0.043 (3)	0.104 (4)	0.063 (3)	0.024 (3)	0.019 (3)	0.021 (3)
C26	0.047 (2)	0.105 (3)	0.067 (3)	0.024 (2)	0.018 (2)	0.020 (3)
C27	0.050 (2)	0.102 (3)	0.070 (3)	0.028 (2)	0.015 (2)	0.017 (2)
C28	0.052 (2)	0.093 (3)	0.068 (3)	0.034 (2)	0.012 (2)	0.015 (2)
C29	0.052 (2)	0.080 (3)	0.061 (2)	0.038 (2)	0.011 (2)	0.010 (2)
C30	0.058 (2)	0.070 (3)	0.061 (2)	0.039 (2)	0.007 (2)	0.007 (2)
C31	0.066 (2)	0.065 (3)	0.067 (3)	0.035 (2)	0.002 (2)	0.008 (2)
C32	0.073 (3)	0.058 (3)	0.070 (3)	0.027 (2)	−0.001 (2)	0.009 (2)
C33	0.074 (3)	0.053 (3)	0.068 (3)	0.020 (2)	−0.003 (2)	0.011 (2)
C34	0.073 (3)	0.050 (3)	0.066 (3)	0.019 (3)	−0.003 (3)	0.010 (3)
C35	0.037 (2)	0.036 (2)	0.060 (3)	0.008 (2)	0.026 (2)	0.004 (2)
C36	0.039 (2)	0.039 (2)	0.058 (2)	0.0082 (18)	0.0248 (19)	0.0066 (19)
C37	0.039 (2)	0.038 (2)	0.054 (2)	0.0111 (17)	0.0248 (18)	0.0069 (18)
C38	0.0384 (19)	0.0341 (19)	0.048 (2)	0.0124 (16)	0.0220 (17)	0.0056 (17)
C39	0.0349 (19)	0.0294 (18)	0.044 (2)	0.0120 (16)	0.0201 (17)	0.0049 (17)
C40	0.0352 (19)	0.0289 (18)	0.047 (2)	0.0100 (16)	0.0192 (17)	0.0001 (17)
C41	0.0390 (19)	0.0305 (19)	0.056 (2)	0.0086 (16)	0.0196 (18)	−0.0044 (18)
C42	0.042 (2)	0.0324 (19)	0.064 (2)	0.0049 (17)	0.0189 (19)	−0.0042 (18)
C43	0.039 (2)	0.032 (2)	0.066 (2)	0.0034 (18)	0.020 (2)	−0.001 (2)
C44	0.035 (2)	0.030 (2)	0.064 (3)	0.005 (2)	0.021 (2)	−0.001 (2)
Dy1	0.01444 (13)	0.01919 (14)	0.01331 (14)	0.00240 (10)	0.00243 (10)	−0.00233 (10)
Dy2	0.01911 (14)	0.02153 (15)	0.01423 (14)	0.00364 (10)	−0.00064 (10)	−0.00393 (10)
N1	0.031 (3)	0.056 (4)	0.028 (3)	0.014 (3)	0.003 (2)	−0.008 (3)
N2	0.047 (3)	0.036 (3)	0.036 (3)	0.015 (3)	−0.002 (3)	0.002 (3)
N3	0.022 (2)	0.021 (2)	0.027 (3)	0.0041 (19)	0.007 (2)	−0.002 (2)
N4	0.025 (3)	0.028 (3)	0.039 (3)	0.007 (2)	0.015 (2)	0.001 (2)
O1	0.028 (2)	0.032 (2)	0.020 (2)	0.0113 (18)	−0.0043 (17)	−0.0067 (17)
O2	0.021 (2)	0.031 (2)	0.023 (2)	0.0085 (17)	−0.0051 (16)	−0.0102 (17)
O3	0.023 (2)	0.033 (2)	0.038 (2)	0.0123 (18)	0.0013 (18)	0.0082 (19)
O4	0.038 (2)	0.034 (2)	0.022 (2)	0.016 (2)	−0.0039 (18)	−0.0002 (18)
O5	0.074 (4)	0.069 (4)	0.063 (4)	0.047 (3)	−0.032 (3)	−0.047 (3)
O6	0.026 (2)	0.033 (2)	0.0132 (19)	0.0030 (17)	0.0032 (16)	0.0001 (16)
O7	0.035 (2)	0.032 (2)	0.015 (2)	−0.0036 (18)	0.0041 (17)	−0.0036 (17)
O8	0.033 (3)	0.103 (5)	0.024 (3)	−0.023 (3)	0.005 (2)	−0.006 (3)
O9	0.028 (2)	0.036 (2)	0.0140 (19)	0.0053 (18)	−0.0009 (16)	−0.0052 (17)
O10	0.027 (2)	0.045 (3)	0.027 (2)	−0.0024 (19)	0.0107 (19)	−0.009 (2)
O11	0.028 (2)	0.031 (2)	0.028 (2)	−0.0036 (18)	0.0046 (18)	−0.0111 (18)
O12	0.030 (2)	0.029 (2)	0.022 (2)	0.0026 (17)	0.0078 (17)	−0.0076 (17)
O13	0.0190 (19)	0.027 (2)	0.030 (2)	0.0000 (16)	0.0095 (17)	−0.0094 (17)
O14	0.0198 (19)	0.023 (2)	0.026 (2)	−0.0008 (16)	0.0057 (16)	−0.0103 (17)
O15	0.024 (2)	0.054 (3)	0.024 (2)	−0.004 (2)	0.0114 (18)	−0.012 (2)
O1W	0.027 (2)	0.049 (3)	0.025 (2)	−0.006 (2)	0.0046 (18)	−0.008 (2)
O2W	0.042 (3)	0.027 (2)	0.028 (2)	0.0007 (19)	0.011 (2)	0.0007 (18)
O3W	0.062 (4)	0.058 (4)	0.064 (4)	−0.007 (3)	0.014 (3)	−0.003 (3)
O4W	0.095 (5)	0.122 (7)	0.056 (4)	−0.047 (5)	0.030 (4)	−0.019 (4)

Geometric parameters (Å, º) top

C1—C6	1.377 (8)	C30—C31	1.409 (12)
C1—C2	1.401 (8)	C31—C32	1.371 (13)
C1—C7	1.494 (8)	C31—H31	0.9300
C2—C3	1.383 (8)	C32—C33	1.334 (13)
C2—H2	0.9300	C32—H32	0.9300
C3—C4	1.377 (8)	C33—C34	1.385 (12)
C3—C8	1.505 (8)	C33—H33	0.9300
C4—C5	1.383 (8)	C34—N2	1.336 (11)
C4—H4	0.9300	C34—H34	0.9300
C5—O5	1.362 (8)	C35—N4	1.325 (8)
C5—C6	1.397 (9)	C35—C36	1.389 (9)
C6—H6	0.9300	C35—H35	0.9300
C7—O1	1.263 (7)	C36—C37	1.371 (10)
C7—O2	1.269 (7)	C36—H36	0.9300
C8—O4	1.246 (7)	C37—C38	1.372 (9)
C8—O3	1.272 (7)	C37—H37	0.9300
C9—C14	1.381 (8)	C38—C39	1.372 (9)
C9—C10	1.393 (8)	C38—H38	0.9300
C9—C15	1.499 (7)	C39—N4	1.345 (8)
C10—C11	1.390 (8)	C39—C40	1.502 (9)
C10—H10	0.9300	C40—N3	1.346 (7)
C11—O10	1.362 (7)	C40—C41	1.386 (9)
C11—C12	1.388 (8)	C41—C42	1.384 (10)
C12—C13	1.396 (8)	C41—H41	0.9300
C12—H12	0.9300	C42—C43	1.383 (10)
C13—C14	1.380 (8)	C42—H42	0.9300
C13—C16	1.511 (8)	C43—C44	1.384 (9)
C14—H14	0.9300	C43—H43	0.9300
C15—O7	1.260 (7)	C44—N3	1.335 (8)
C15—O6	1.265 (7)	C44—H44	0.9300
C16—O8	1.249 (7)	Dy1—O13ⁱ	2.287 (4)
C16—O9	1.260 (7)	Dy1—O3ⁱⁱ	2.328 (4)
C17—C22	1.392 (7)	Dy1—O4	2.355 (4)
C17—C18	1.397 (7)	Dy1—O14ⁱⁱⁱ	2.358 (4)
C17—C24	1.497 (8)	Dy1—O6	2.444 (4)
C18—C19	1.380 (7)	Dy1—O7	2.496 (4)
C18—H18	0.9300	Dy1—N4	2.545 (5)
C19—C20	1.409 (7)	Dy1—N3	2.603 (5)
C19—C23	1.502 (7)	Dy1—O3	2.818 (4)
C20—C21	1.391 (7)	Dy2—O9^iv	2.300 (4)
C20—H20	0.9300	Dy2—O1W	2.346 (4)
C21—O15	1.359 (7)	Dy2—O11	2.393 (4)
C21—C22	1.380 (8)	Dy2—O2W	2.444 (4)
C22—H22	0.9300	Dy2—O1	2.470 (4)
C23—O14	1.257 (6)	Dy2—O2	2.472 (4)
C23—O13	1.260 (6)	Dy2—O12	2.527 (4)
C24—O12	1.262 (7)	Dy2—N2	2.549 (6)
C24—O11	1.266 (7)	Dy2—N1	2.628 (5)
C25—N1	1.346 (11)	O5—H5	0.8200
C25—C26	1.377 (12)	O10—H10A	0.8200
C25—H25	0.9300	O15—H15	0.8200
C26—C27	1.367 (14)	O1W—H1WA	0.8500
C26—H26	0.9300	O1W—H1WB	0.8500
C27—C28	1.394 (14)	O2W—H2WA	0.8501
C27—H27	0.9300	O2W—H2WB	0.8500
C28—C29	1.390 (11)	O3W—H3WA	0.8500
C28—H28	0.9300	O3W—H3WB	0.8501
C29—N1	1.347 (10)	O4W—H4WA	0.8500
C29—C30	1.470 (13)	O4W—H4WB	0.8500
C30—N2	1.343 (10)

C6—C1—C2	119.8 (5)	C42—C41—C40	119.5 (6)
C6—C1—C7	120.1 (5)	C42—C41—H41	120.2
C2—C1—C7	120.0 (5)	C40—C41—H41	120.2
C3—C2—C1	119.5 (5)	C43—C42—C41	118.2 (7)
C3—C2—H2	120.2	C43—C42—H42	120.9
C1—C2—H2	120.2	C41—C42—H42	120.9
C4—C3—C2	120.5 (5)	C42—C43—C44	118.8 (7)
C4—C3—C8	120.1 (5)	C42—C43—H43	120.6
C2—C3—C8	119.3 (5)	C44—C43—H43	120.6
C3—C4—C5	120.4 (6)	N3—C44—C43	123.6 (6)
C3—C4—H4	119.8	N3—C44—H44	118.2
C5—C4—H4	119.8	C43—C44—H44	118.2
O5—C5—C4	121.8 (6)	O13ⁱ—Dy1—O3ⁱⁱ	72.52 (14)
O5—C5—C6	118.7 (5)	O13ⁱ—Dy1—O4	89.48 (15)
C4—C5—C6	119.5 (6)	O3ⁱⁱ—Dy1—O4	127.26 (15)
C1—C6—C5	120.3 (6)	O13ⁱ—Dy1—O14ⁱⁱⁱ	134.77 (13)
C1—C6—H6	119.8	O3ⁱⁱ—Dy1—O14ⁱⁱⁱ	77.83 (14)
C5—C6—H6	119.8	O4—Dy1—O14ⁱⁱⁱ	82.03 (15)
O1—C7—O2	119.7 (5)	O13ⁱ—Dy1—O6	86.34 (13)
O1—C7—C1	120.7 (5)	O3ⁱⁱ—Dy1—O6	87.44 (14)
O2—C7—C1	119.6 (5)	O4—Dy1—O6	141.71 (14)
O4—C8—O3	121.5 (5)	O14ⁱⁱⁱ—Dy1—O6	125.92 (13)
O4—C8—C3	118.6 (5)	O13ⁱ—Dy1—O7	129.91 (14)
O3—C8—C3	119.8 (5)	O3ⁱⁱ—Dy1—O7	77.91 (15)
C14—C9—C10	120.3 (5)	O4—Dy1—O7	140.19 (15)
C14—C9—C15	121.7 (5)	O14ⁱⁱⁱ—Dy1—O7	73.56 (13)
C10—C9—C15	118.1 (5)	O6—Dy1—O7	52.45 (13)
C11—C10—C9	119.6 (5)	O13ⁱ—Dy1—N4	139.44 (15)
C11—C10—H10	120.2	O3ⁱⁱ—Dy1—N4	145.09 (16)
C9—C10—H10	120.2	O4—Dy1—N4	76.16 (16)
O10—C11—C12	118.2 (5)	O14ⁱⁱⁱ—Dy1—N4	81.22 (15)
O10—C11—C10	121.6 (5)	O6—Dy1—N4	82.61 (15)
C12—C11—C10	120.3 (5)	O7—Dy1—N4	69.50 (16)
C11—C12—C13	119.5 (5)	O13ⁱ—Dy1—N3	76.12 (14)
C11—C12—H12	120.2	O3ⁱⁱ—Dy1—N3	141.60 (15)
C13—C12—H12	120.2	O4—Dy1—N3	73.24 (15)
C14—C13—C12	120.2 (5)	O14ⁱⁱⁱ—Dy1—N3	140.54 (14)
C14—C13—C16	120.5 (5)	O6—Dy1—N3	68.80 (14)
C12—C13—C16	119.3 (5)	O7—Dy1—N3	107.11 (14)
C13—C14—C9	120.2 (5)	N4—Dy1—N3	63.48 (15)
C13—C14—H14	119.9	O13ⁱ—Dy1—O3	73.04 (13)
C9—C14—H14	119.9	O3ⁱⁱ—Dy1—O3	78.01 (14)
O7—C15—O6	119.7 (5)	O4—Dy1—O3	49.26 (13)
O7—C15—C9	119.8 (5)	O14ⁱⁱⁱ—Dy1—O3	67.89 (13)
O6—C15—C9	120.4 (5)	O6—Dy1—O3	157.51 (12)
O8—C16—O9	124.3 (5)	O7—Dy1—O3	137.87 (13)
O8—C16—C13	117.8 (5)	N4—Dy1—O3	118.94 (14)
O9—C16—C13	118.0 (5)	N3—Dy1—O3	113.26 (13)
C22—C17—C18	119.5 (5)	O9^iv—Dy2—O1W	76.99 (14)
C22—C17—C24	119.6 (5)	O9^iv—Dy2—O11	144.48 (14)
C18—C17—C24	120.9 (5)	O1W—Dy2—O11	130.31 (14)
C19—C18—C17	120.2 (5)	O9^iv—Dy2—O2W	102.70 (15)
C19—C18—H18	119.9	O1W—Dy2—O2W	147.49 (16)
C17—C18—H18	119.9	O11—Dy2—O2W	67.17 (14)
C18—C19—C20	120.1 (5)	O9^iv—Dy2—O1	126.34 (14)
C18—C19—C23	119.6 (5)	O1W—Dy2—O1	80.60 (15)
C20—C19—C23	120.3 (5)	O11—Dy2—O1	84.89 (14)
C21—C20—C19	119.3 (5)	O2W—Dy2—O1	73.59 (14)
C21—C20—H20	120.4	O9^iv—Dy2—O2	74.47 (14)
C19—C20—H20	120.4	O1W—Dy2—O2	74.31 (15)
O15—C21—C22	117.2 (5)	O11—Dy2—O2	129.29 (14)
O15—C21—C20	122.6 (5)	O2W—Dy2—O2	74.37 (14)
C22—C21—C20	120.3 (5)	O1—Dy2—O2	52.60 (12)
C21—C22—C17	120.5 (5)	O9^iv—Dy2—O12	145.62 (14)
C21—C22—H22	119.8	O1W—Dy2—O12	77.65 (14)
C17—C22—H22	119.8	O11—Dy2—O12	52.71 (13)
O14—C23—O13	125.5 (5)	O2W—Dy2—O12	111.16 (13)
O14—C23—C19	118.4 (5)	O1—Dy2—O12	71.06 (14)
O13—C23—C19	116.1 (5)	O2—Dy2—O12	119.80 (13)
O12—C24—O11	119.8 (5)	O9^iv—Dy2—N2	79.69 (17)
O12—C24—C17	121.1 (5)	O1W—Dy2—N2	80.15 (18)
O11—C24—C17	119.1 (5)	O11—Dy2—N2	83.40 (17)
N1—C25—C26	124.2 (10)	O2W—Dy2—N2	132.21 (18)
N1—C25—H25	117.9	O1—Dy2—N2	142.38 (17)
C26—C25—H25	117.9	O2—Dy2—N2	146.97 (16)
C27—C26—C25	117.1 (10)	O12—Dy2—N2	73.40 (16)
C27—C26—H26	121.5	O9^iv—Dy2—N1	67.91 (15)
C25—C26—H26	121.5	O1W—Dy2—N1	132.17 (17)
C26—C27—C28	120.5 (9)	O11—Dy2—N1	76.59 (15)
C26—C27—H27	119.7	O2W—Dy2—N1	73.89 (17)
C28—C27—H27	119.7	O1—Dy2—N1	146.81 (16)
C29—C28—C27	118.7 (9)	O2—Dy2—N1	122.85 (16)
C29—C28—H28	120.6	O12—Dy2—N1	115.59 (16)
C27—C28—H28	120.6	N2—Dy2—N1	62.81 (19)
N1—C29—C28	121.2 (9)	C25—N1—C29	118.1 (7)
N1—C29—C30	118.0 (7)	C25—N1—Dy2	122.0 (5)
C28—C29—C30	120.8 (8)	C29—N1—Dy2	119.5 (5)
N2—C30—C31	120.4 (9)	C34—N2—C30	117.7 (7)
N2—C30—C29	116.4 (7)	C34—N2—Dy2	118.8 (5)
C31—C30—C29	123.1 (8)	C30—N2—Dy2	123.3 (5)
C32—C31—C30	119.2 (9)	C44—N3—C40	117.4 (5)
C32—C31—H31	120.4	C44—N3—Dy1	123.9 (4)
C30—C31—H31	120.4	C40—N3—Dy1	118.7 (4)
C33—C32—C31	120.7 (9)	C35—N4—C39	118.0 (5)
C33—C32—H32	119.7	C35—N4—Dy1	120.5 (4)
C31—C32—H32	119.7	C39—N4—Dy1	118.3 (4)
C32—C33—C34	117.7 (10)	C7—O1—Dy2	93.8 (3)
C32—C33—H33	121.1	C7—O2—Dy2	93.6 (3)
C34—C33—H33	121.1	C8—O3—Dy1ⁱⁱ	168.2 (4)
N2—C34—C33	124.2 (9)	C8—O3—Dy1	81.1 (3)
N2—C34—H34	117.9	Dy1ⁱⁱ—O3—Dy1	101.99 (14)
C33—C34—H34	117.9	C8—O4—Dy1	103.3 (3)
N4—C35—C36	123.6 (7)	C5—O5—H5	109.5
N4—C35—H35	118.2	C15—O6—Dy1	94.6 (3)
C36—C35—H35	118.2	C15—O7—Dy1	92.3 (3)
C37—C36—C35	117.5 (6)	C16—O9—Dy2^v	139.1 (4)
C37—C36—H36	121.3	C11—O10—H10A	109.5
C35—C36—H36	121.3	C24—O11—Dy2	96.7 (3)
C36—C37—C38	119.3 (6)	C24—O12—Dy2	90.5 (3)
C36—C37—H37	120.4	C23—O13—Dy1ⁱ	140.5 (4)
C38—C37—H37	120.4	C23—O14—Dy1^vi	138.4 (3)
C39—C38—C37	119.8 (7)	C21—O15—H15	109.5
C39—C38—H38	120.1	Dy2—O1W—H1WA	115.0
C37—C38—H38	120.1	Dy2—O1W—H1WB	133.5
N4—C39—C38	121.5 (6)	H1WA—O1W—H1WB	107.7
N4—C39—C40	116.2 (5)	Dy2—O2W—H2WA	99.2
C38—C39—C40	122.2 (6)	Dy2—O2W—H2WB	153.0
N3—C40—C41	122.5 (6)	H2WA—O2W—H2WB	107.7
N3—C40—C39	116.2 (5)	H3WA—O3W—H3WB	107.7
C41—C40—C39	121.2 (6)	H4WA—O4W—H4WB	107.7

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x, −y+2, −z+1; (iii) x, y+1, z; (iv) x+1, y, z+1; (v) x−1, y, z−1; (vi) x, y−1, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5···O4Wⁱⁱⁱ	0.82	2.15	2.910 (11)	154
O10—H10A···O2^vii	0.82	1.95	2.761 (6)	168
O15—H15···O1^viii	0.82	1.92	2.718 (6)	163
O1W—H1WA···O8^iv	0.85	1.84	2.609 (6)	150
O1W—H1WB···O3W^viii	0.85	2.01	2.717 (7)	141
O2W—H2WA···O11	0.85	2.15	2.676 (6)	120
O2W—H2WB···O7^vii	0.85	1.86	2.689 (6)	164
O3W—H3WA···O4W^viii	0.85	1.99	2.744 (9)	147
O3W—H3WB···O8^ix	0.85	2.03	2.832 (9)	156
O4W—H4WA···O6ⁱ	0.85	1.96	2.809 (8)	175
O4W—H4WB···O12	0.85	2.20	2.801 (8)	128

Symmetry codes: (i) −x, −y+1, −z+1; (iii) x, y+1, z; (iv) x+1, y, z+1; (vii) −x+1, −y+2, −z+1; (viii) −x+1, −y+1, −z+1; (ix) x+1, y, z.

Experimental details

Crystal data
Chemical formula	[Dy₂(C₈H₄O₅)₃(C₁₀H₈N₂)₂(H₂O)₂]·2H₂O
M_r	1249.77
Crystal system, space group	Triclinic, P1
Temperature (K)	298
a, b, c (Å)	11.3736 (5), 12.0349 (6), 17.8360 (8)
α, β, γ (°)	91.310 (1), 103.187 (1), 106.505 (1)
V (Å³)	2269.00 (18)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	3.35
Crystal size (mm)	0.25 × 0.24 × 0.21

Data collection
Diffractometer	Bruker APEXII CCD
Absorption correction	Multi-scan (SADABS; Bruker, 2001)
T_min, T_max	0.488, 0.540
No. of measured, independent and observed [I > 2σ(I)] reflections	11732, 8024, 7052
R_int	0.020
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.035, 0.094, 1.06
No. of reflections	8024
No. of parameters	624
No. of restraints	252
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	2.65, −1.25

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999) and SHELXTL (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5···O4Wⁱ	0.82	2.15	2.910 (11)	154
O10—H10A···O2ⁱⁱ	0.82	1.95	2.761 (6)	168
O15—H15···O1ⁱⁱⁱ	0.82	1.92	2.718 (6)	163
O1W—H1WA···O8^iv	0.85	1.84	2.609 (6)	150
O1W—H1WB···O3Wⁱⁱⁱ	0.85	2.01	2.717 (7)	141
O2W—H2WA···O11	0.85	2.15	2.676 (6)	120
O2W—H2WB···O7ⁱⁱ	0.85	1.86	2.689 (6)	164
O3W—H3WA···O4Wⁱⁱⁱ	0.85	1.99	2.744 (9)	147
O3W—H3WB···O8^v	0.85	2.03	2.832 (9)	156
O4W—H4WA···O6^vi	0.85	1.96	2.809 (8)	175
O4W—H4WB···O12	0.85	2.20	2.801 (8)	128

Symmetry codes: (i) x, y+1, z; (ii) −x+1, −y+2, −z+1; (iii) −x+1, −y+1, −z+1; (iv) x+1, y, z+1; (v) x+1, y, z; (vi) −x, −y+1, −z+1.

Acknowledgements

The author acknowledges South China Normal University for supporting this work.

References

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