Poly[bis­[diaqua­(isonicotinato-κ2O,O′)dysprosium(III)][bis­(iso­nicotinato-κO)copper(II)]tetra­(μ3-isonicotinato-κ3O:O′:N)]

Kuang, D.-Z.; Feng, Y.-L.; Peng, Y.-L.; Deng, Y.-F.

doi:10.1107/S1600536807043899

Poly[bis[diaqua(isonicotinato-κ²O,O′)dysprosium(III)][bis(isonicotinato-κO)copper(II)]tetra(μ₃-isonicotinato-κ³O:O′:N)]

D.-Z. Kuang, Y.-L. Feng, Y.-L. Peng and Y.-F. Deng

The title compound, {[Dy(C₆H₄NO₂)(H₂O)₂]₂[Cu(C₆H₄NO₂)₂](C₆H₄NO₂)₄}_n, is a three-dimensional coordination polymer. The six-coordinate Cu^II atom, lying on an inversion center, is bonded to two O atoms from two monodentate isonicotinate ligands and four N atoms from four bridging isonicotinate ligands. Two Dy^III atoms form a centrosymmetric dinuclear unit and each Dy^III atom is eight-coordinated by six O atoms from five different isonicotinate ligands and two O atoms from two water molecules. These metal coordination units are connected by the bridging isonicotinate ligands, generating a three-dimensional network. The crystal structure is further stabilized by hydrogen bonds.

Read article Similar articles

Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807043899/hy2080sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807043899/hy2080Isup2.hkl Contains datablock I

CCDC reference: 664949

checkCIF report

Key indicators

Single-crystal X-ray study
T = 294 K
Mean (C-C) = 0.006 Å
R factor = 0.025
wR factor = 0.058
Data-to-parameter ratio = 12.4

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       2.87 Ratio
PLAT220_ALERT_2_C Large Non-Solvent    N     Ueq(max)/Ueq(min) ...       2.83 Ratio
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.08 Ratio
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O1
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O7

Alert level G
PLAT794_ALERT_5_G Check Predicted Bond Valency for Dy          (3)       3.01
PLAT794_ALERT_5_G Check Predicted Bond Valency for Cu          (2)       2.09
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......          4

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

Comment top

In the past few years, more extensive attention had been paid to the research on the chemistry of heterometallic complexes containing simultaneously lanthanide and transition metal ions (Costs et al., 1998; Kahn et al., 1999; Sanz et al., 1996). As an extension of this research, we report here the structure of the title compound, a new heterometallic coordination polymer,

In the title compound (Fig. 1), the Cu^II atom lies on an inversion center and is six-coordinated by two O atoms from two monodentate isonicotinate ligands and four N atoms from the other four isonicotinate ligands. Thus the Cu^II atom has a slight distorted octahedral coordination geometry. The Dy^III atom is eight-coordinated by six O atoms from five different isonicotinate ligands and two O atoms from two water molecules in a square antiprism geometry (Table 1). The adjacent Cu and Dy coordination units are bridged by the tridentate isonicotinate ligands, forming a three-dimensional network structure (Fig. 2).

Related literature top

For related literature, see: Costs et al. (1998); Kahn et al. (1999); Sanz et al. (1996).

Experimental top

A mixture of CuO (0.082 g, 1.0 mmol), Dy₂O₃ (0.181 g, 0.5 mmol), isonicotinic acid (0.248 g, 2.0 mmol), H₂O (10 ml, 0.55 mmol) and two drops of acetic acid, with a pH value about 2.0, was sealed in a 25 ml Teflon-lined reaction vessel at 443 K for 5 d. The reaction mixture was cooled to room temperature over a period of 48 h. The product was collected by filtration, washed with water and air-dried. Blue block crystals suitable for X-ray analysis were obtained. Analysis, calculated for C₄₈H₄₀CuDy₂N₈O₂₀: C 40.11, H 2.80, N 7.80%; found: C 40.05; H 2.59, N 7.97%.

Structure description top

For related literature, see: Costs et al. (1998); Kahn et al. (1999); Sanz et al. (1996).

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL (Bruker, 2001).

Figures top

	Fig. 1. The asymmetric unit of the title compound, together with symmetry-related atoms to complete the coordination units. Displacement ellipsoids are drawn at the 50% probability level. H atoms have been omitted for clarity. [Symmetry codes: (i) -x, -y + 1, -z + 1; (ii) -x + 1, -y, -z + 1; (iii) -x + 1/2, y - 1/2, -z + 3/2; (iv) 1/2 + x, 1/2 - y, -1/2 + z.]
	Fig. 2. A view of the three-dimensional structure of the title compound. Dotted lines denote hydrogen bonds.

Poly[bis[diaqua(isonicotinato-κ2O,O')dysprosium(III)] [bis(isonicotinato-κO)copper(II)]tetra(µ3-isonicotinato-κ3O:O':N)] top

Crystal data top

[Dy₂Cu(C₆H₄NO₂)₈(H₂O)₄]	F(000) = 1410
M_r = 1437.43	D_x = 1.861 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 4174 reflections
a = 9.456 (1) Å	θ = 2.6–14.6°
b = 14.966 (3) Å	µ = 3.38 mm⁻¹
c = 18.166 (4) Å	T = 294 K
β = 93.74 (1)°	Block, blue
V = 2565.4 (8) Å³	0.54 × 0.42 × 0.28 mm
Z = 2

Data collection top

Bruker SMART 1000 CCD area-detector diffractometer	4638 independent reflections
Radiation source: normal-focus sealed tube	3853 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.018
φ and ω scans	θ_max = 25.3°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = 0→11
T_min = 0.199, T_max = 0.391	k = 0→17
5313 measured reflections	l = −21→21

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.026	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.058	w = 1/[σ²(F_o²) + (0.0289P)²] where P = (F_o² + 2F_c²)/3
S = 1.03	(Δ/σ)_max = 0.002
4638 reflections	Δρ_max = 0.61 e Å⁻³
375 parameters	Δρ_min = −0.89 e Å⁻³
4 restraints	Extinction correction: SHELXL97
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00120 (9)

Crystal data top

[Dy₂Cu(C₆H₄NO₂)₈(H₂O)₄]	V = 2565.4 (8) Å³
M_r = 1437.43	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 9.456 (1) Å	µ = 3.38 mm⁻¹
b = 14.966 (3) Å	T = 294 K
c = 18.166 (4) Å	0.54 × 0.42 × 0.28 mm
β = 93.74 (1)°

Data collection top

Bruker SMART 1000 CCD area-detector diffractometer	4638 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	3853 reflections with I > 2σ(I)
T_min = 0.199, T_max = 0.391	R_int = 0.018
5313 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.026	4 restraints
wR(F²) = 0.058	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	Δρ_max = 0.61 e Å⁻³
4638 reflections	Δρ_min = −0.89 e Å⁻³
375 parameters

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

	x	y	z	U_iso*/U_eq
Dy	0.195701 (18)	0.583911 (12)	0.500576 (9)	0.01381 (7)
Cu	0.5000	0.0000	0.5000	0.01940 (16)
O1	0.2280 (3)	0.43001 (18)	0.50421 (17)	0.0337 (8)
O2	0.0274 (3)	0.3543 (2)	0.50973 (19)	0.0402 (8)
O3	0.3581 (3)	−0.05366 (19)	0.42852 (15)	0.0255 (7)
O4	0.1845 (3)	−0.1225 (2)	0.48600 (15)	0.0345 (8)
O5	0.3964 (3)	0.56810 (18)	0.41742 (14)	0.0243 (6)
O6	0.2726 (3)	0.69240 (19)	0.41176 (15)	0.0298 (7)
O7	0.1052 (4)	0.5477 (2)	0.61110 (16)	0.0390 (8)
O8	−0.0907 (3)	0.4660 (2)	0.61044 (16)	0.0398 (8)
O9	0.2216 (3)	0.7219 (2)	0.56835 (17)	0.0281 (7)
O10	0.4068 (3)	0.5705 (2)	0.57715 (16)	0.0272 (7)
N1	0.3863 (3)	0.1131 (2)	0.49738 (16)	0.0168 (7)
N2	0.0145 (4)	−0.1238 (3)	0.2173 (2)	0.0425 (11)
N3	0.5756 (5)	0.7292 (3)	0.1969 (2)	0.0467 (11)
N4	0.0917 (4)	0.4501 (4)	0.8722 (2)	0.0475 (12)
C1	0.4533 (4)	0.1926 (3)	0.4982 (2)	0.0230 (9)
H1	0.5517	0.1933	0.4988	0.028*
C2	0.3828 (4)	0.2722 (3)	0.4983 (2)	0.0215 (9)
H2	0.4329	0.3257	0.4987	0.026*
C3	0.2366 (4)	0.2729 (3)	0.4979 (2)	0.0194 (9)
C4	0.1649 (4)	0.1919 (3)	0.4943 (2)	0.0221 (9)
H4	0.0664	0.1900	0.4919	0.027*
C5	0.2442 (4)	0.1140 (3)	0.4944 (2)	0.0220 (9)
H5	0.1964	0.0597	0.4924	0.026*
C6	0.1574 (4)	0.3599 (3)	0.5038 (2)	0.0220 (9)
C7	0.1288 (6)	−0.0714 (4)	0.2280 (3)	0.0491 (15)
H7	0.1616	−0.0417	0.1875	0.059*
C8	0.2008 (5)	−0.0592 (3)	0.2961 (2)	0.0385 (12)
H8	0.2775	−0.0202	0.3008	0.046*
C9	0.1591 (4)	−0.1045 (3)	0.3564 (2)	0.0227 (9)
C10	0.0435 (4)	−0.1607 (3)	0.3463 (2)	0.0300 (10)
H10	0.0117	−0.1931	0.3857	0.036*
C11	−0.0242 (5)	−0.1681 (3)	0.2768 (3)	0.0374 (12)
H11	−0.1016	−0.2064	0.2709	0.045*
C12	0.2395 (4)	−0.0932 (3)	0.4307 (2)	0.0230 (9)
C13	0.6322 (6)	0.6681 (4)	0.2435 (3)	0.0545 (16)
H13	0.7200	0.6444	0.2337	0.065*
C14	0.5697 (5)	0.6376 (4)	0.3052 (3)	0.0424 (13)
H14	0.6148	0.5950	0.3357	0.051*
C15	0.4397 (4)	0.6712 (3)	0.3210 (2)	0.0255 (9)
C16	0.3780 (5)	0.7340 (3)	0.2730 (2)	0.0397 (12)
H16	0.2901	0.7584	0.2814	0.048*
C17	0.4488 (6)	0.7599 (4)	0.2122 (3)	0.0497 (14)
H17	0.4051	0.8014	0.1801	0.060*
C18	0.3660 (4)	0.6428 (3)	0.3878 (2)	0.0192 (9)
C19	0.1568 (5)	0.5134 (4)	0.8384 (3)	0.0528 (16)
H19	0.2187	0.5495	0.8671	0.063*
C20	0.1418 (5)	0.5311 (4)	0.7644 (2)	0.0373 (12)
H20	0.1930	0.5767	0.7438	0.045*
C21	0.0486 (4)	0.4793 (3)	0.7215 (2)	0.0214 (9)
C22	−0.0190 (4)	0.4097 (3)	0.7547 (2)	0.0292 (10)
H22	−0.0812	0.3723	0.7275	0.035*
C23	0.0088 (5)	0.3974 (4)	0.8296 (3)	0.0418 (13)
H23	−0.0334	0.3490	0.8516	0.050*
C24	0.0185 (4)	0.4987 (3)	0.6407 (2)	0.0210 (9)
H9A	0.223 (5)	0.7683 (18)	0.545 (2)	0.043 (16)*
H9B	0.178 (4)	0.734 (3)	0.6043 (15)	0.033 (13)*
H10A	0.468 (4)	0.533 (2)	0.572 (3)	0.043 (16)*
H10B	0.433 (6)	0.592 (4)	0.6169 (17)	0.08 (2)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy	0.01477 (10)	0.01319 (10)	0.01358 (10)	0.00195 (9)	0.00165 (6)	0.00091 (8)
Cu	0.0195 (3)	0.0130 (3)	0.0247 (4)	0.0058 (3)	−0.0065 (3)	−0.0050 (3)
O1	0.0367 (19)	0.0121 (16)	0.052 (2)	0.0043 (14)	0.0036 (15)	0.0001 (14)
O2	0.0233 (17)	0.0296 (19)	0.068 (2)	0.0145 (15)	0.0071 (16)	0.0005 (17)
O3	0.0259 (16)	0.0243 (16)	0.0250 (15)	0.0031 (13)	−0.0088 (12)	−0.0052 (12)
O4	0.045 (2)	0.0325 (18)	0.0256 (17)	0.0004 (16)	0.0011 (15)	0.0013 (14)
O5	0.0253 (15)	0.0255 (17)	0.0229 (14)	0.0021 (13)	0.0075 (12)	0.0046 (12)
O6	0.0399 (18)	0.0192 (16)	0.0324 (16)	0.0038 (14)	0.0184 (14)	0.0026 (13)
O7	0.054 (2)	0.042 (2)	0.0232 (16)	−0.0082 (18)	0.0164 (15)	0.0048 (15)
O8	0.0355 (18)	0.060 (2)	0.0224 (16)	−0.0039 (18)	−0.0074 (14)	−0.0027 (16)
O9	0.0396 (18)	0.0194 (17)	0.0267 (17)	−0.0007 (15)	0.0140 (14)	−0.0017 (14)
O10	0.0242 (16)	0.0313 (19)	0.0248 (16)	0.0093 (15)	−0.0086 (13)	−0.0053 (14)
N1	0.0174 (16)	0.0169 (17)	0.0158 (15)	0.0039 (14)	−0.0022 (13)	−0.0021 (13)
N2	0.048 (3)	0.041 (2)	0.035 (2)	−0.007 (2)	−0.0195 (19)	0.005 (2)
N3	0.063 (3)	0.040 (3)	0.041 (2)	0.004 (2)	0.029 (2)	0.011 (2)
N4	0.041 (2)	0.082 (4)	0.019 (2)	0.003 (3)	−0.0027 (18)	0.009 (2)
C1	0.016 (2)	0.022 (2)	0.031 (2)	−0.0044 (18)	0.0064 (17)	−0.0001 (18)
C2	0.016 (2)	0.018 (2)	0.030 (2)	−0.0011 (17)	−0.0006 (16)	−0.0022 (18)
C3	0.023 (2)	0.014 (2)	0.022 (2)	0.0114 (17)	0.0023 (17)	0.0010 (16)
C4	0.015 (2)	0.021 (2)	0.030 (2)	0.0027 (17)	0.0022 (17)	−0.0006 (18)
C5	0.028 (2)	0.014 (2)	0.024 (2)	−0.0027 (18)	0.0012 (17)	−0.0031 (16)
C6	0.024 (2)	0.021 (2)	0.021 (2)	0.0081 (18)	−0.0023 (17)	−0.0011 (17)
C7	0.060 (3)	0.052 (4)	0.033 (3)	−0.018 (3)	−0.016 (2)	0.017 (3)
C8	0.042 (3)	0.036 (3)	0.036 (3)	−0.016 (2)	−0.015 (2)	0.013 (2)
C9	0.023 (2)	0.019 (2)	0.025 (2)	0.0030 (18)	−0.0035 (17)	−0.0009 (17)
C10	0.027 (2)	0.030 (3)	0.032 (2)	−0.004 (2)	0.0017 (19)	−0.002 (2)
C11	0.032 (3)	0.036 (3)	0.042 (3)	−0.008 (2)	−0.011 (2)	−0.004 (2)
C12	0.029 (2)	0.014 (2)	0.025 (2)	0.0058 (19)	−0.0040 (17)	−0.0054 (18)
C13	0.051 (3)	0.055 (4)	0.063 (4)	0.017 (3)	0.039 (3)	0.019 (3)
C14	0.036 (3)	0.047 (3)	0.046 (3)	0.011 (2)	0.017 (2)	0.018 (2)
C15	0.027 (2)	0.027 (2)	0.023 (2)	−0.001 (2)	0.0096 (18)	−0.0005 (18)
C16	0.045 (3)	0.038 (3)	0.039 (3)	0.012 (2)	0.018 (2)	0.012 (2)
C17	0.063 (4)	0.044 (3)	0.044 (3)	0.010 (3)	0.020 (3)	0.019 (3)
C18	0.0154 (19)	0.023 (2)	0.019 (2)	−0.0054 (18)	−0.0009 (16)	0.0014 (17)
C19	0.043 (3)	0.093 (5)	0.023 (3)	−0.017 (3)	−0.001 (2)	−0.017 (3)
C20	0.036 (3)	0.053 (3)	0.023 (2)	−0.014 (2)	0.0017 (19)	−0.004 (2)
C21	0.021 (2)	0.029 (2)	0.0154 (19)	0.0051 (19)	0.0068 (16)	−0.0001 (17)
C22	0.030 (2)	0.033 (3)	0.024 (2)	−0.002 (2)	0.0009 (18)	0.000 (2)
C23	0.052 (3)	0.043 (3)	0.031 (3)	0.005 (3)	0.014 (2)	0.014 (2)
C24	0.024 (2)	0.025 (2)	0.0138 (19)	0.0036 (19)	−0.0014 (17)	−0.0001 (17)

Geometric parameters (Å, º) top

Dy—O7	2.298 (3)	C1—C2	1.365 (5)
Dy—O2ⁱ	2.300 (3)	C1—H1	0.9300
Dy—O8ⁱ	2.313 (3)	C2—C3	1.382 (5)
Dy—O1	2.324 (3)	C2—H2	0.9300
Dy—O10	2.366 (3)	C3—C4	1.388 (6)
Dy—O9	2.409 (3)	C3—C6	1.510 (5)
Dy—O6	2.433 (3)	C4—C5	1.386 (6)
Dy—O5	2.513 (3)	C4—H4	0.9300
Dy—C18	2.828 (4)	C5—H5	0.9300
Cu—O3	1.976 (3)	C7—C8	1.385 (6)
Cu—O3ⁱⁱ	1.976 (3)	C7—H7	0.9300
Cu—N1	2.004 (3)	C8—C9	1.369 (6)
Cu—N1ⁱⁱ	2.004 (3)	C8—H8	0.9300
Cu—N4ⁱⁱⁱ	2.639 (4)	C9—C10	1.382 (6)
O1—C6	1.243 (5)	C9—C12	1.515 (5)
O2—C6	1.244 (5)	C10—C11	1.384 (6)
O2—Dyⁱ	2.300 (3)	C10—H10	0.9300
O3—C12	1.271 (5)	C11—H11	0.9300
O4—C12	1.240 (5)	C13—C14	1.378 (6)
O5—C18	1.266 (5)	C13—H13	0.9300
O6—C18	1.253 (5)	C14—C15	1.376 (6)
O7—C24	1.248 (5)	C14—H14	0.9300
O8—C24	1.239 (5)	C15—C16	1.385 (6)
O8—Dyⁱ	2.313 (3)	C15—C18	1.499 (5)
O9—H9A	0.81 (3)	C16—C17	1.384 (6)
O9—H9B	0.82 (3)	C16—H16	0.9300
O10—H10A	0.82 (3)	C17—H17	0.9300
O10—H10B	0.81 (4)	C19—C20	1.368 (6)
N1—C5	1.341 (5)	C19—H19	0.9300
N1—C1	1.348 (5)	C20—C21	1.377 (6)
N2—C11	1.339 (6)	C20—H20	0.9300
N2—C7	1.340 (6)	C21—C22	1.382 (6)
N3—C17	1.331 (6)	C21—C24	1.504 (5)
N3—C13	1.334 (6)	C22—C23	1.381 (6)
N4—C19	1.304 (7)	C22—H22	0.9300
N4—C23	1.325 (7)	C23—H23	0.9300

O7—Dy—O2ⁱ	76.94 (12)	C3—C2—H2	120.2
O7—Dy—O8ⁱ	121.52 (12)	C2—C3—C4	118.6 (4)
O2ⁱ—Dy—O8ⁱ	73.71 (12)	C2—C3—C6	120.4 (4)
O7—Dy—O1	78.31 (12)	C4—C3—C6	120.9 (3)
O2ⁱ—Dy—O1	121.25 (11)	C5—C4—C3	118.1 (3)
O8ⁱ—Dy—O1	75.69 (12)	C5—C4—H4	120.9
O7—Dy—O10	79.29 (11)	C3—C4—H4	120.9
O2ⁱ—Dy—O10	144.72 (12)	N1—C5—C4	123.3 (4)
O8ⁱ—Dy—O10	141.53 (11)	N1—C5—H5	118.3
O1—Dy—O10	78.16 (11)	C4—C5—H5	118.3
O7—Dy—O9	77.68 (11)	O1—C6—O2	126.1 (4)
O2ⁱ—Dy—O9	76.06 (11)	O1—C6—C3	117.4 (4)
O8ⁱ—Dy—O9	138.25 (12)	O2—C6—C3	116.4 (4)
O1—Dy—O9	145.75 (11)	N2—C7—C8	123.5 (5)
O10—Dy—O9	73.66 (11)	N2—C7—H7	118.3
O7—Dy—O6	151.75 (11)	C8—C7—H7	118.3
O2ⁱ—Dy—O6	89.43 (11)	C9—C8—C7	120.0 (4)
O8ⁱ—Dy—O6	76.52 (11)	C9—C8—H8	120.0
O1—Dy—O6	129.48 (10)	C7—C8—H8	120.0
O10—Dy—O6	99.76 (11)	C8—C9—C10	117.5 (4)
O9—Dy—O6	75.05 (10)	C8—C9—C12	120.3 (4)
O7—Dy—O5	147.35 (11)	C10—C9—C12	122.2 (4)
O2ⁱ—Dy—O5	135.54 (10)	C9—C10—C11	119.0 (4)
O8ⁱ—Dy—O5	75.13 (10)	C9—C10—H10	120.5
O1—Dy—O5	79.68 (10)	C11—C10—H10	120.5
O10—Dy—O5	72.79 (10)	N2—C11—C10	124.2 (4)
O9—Dy—O5	109.42 (10)	N2—C11—H11	117.9
O6—Dy—O5	52.71 (9)	C10—C11—H11	117.9
O7—Dy—C18	165.56 (11)	O4—C12—O3	127.4 (4)
O2ⁱ—Dy—C18	112.24 (11)	O4—C12—C9	118.0 (4)
O8ⁱ—Dy—C18	72.62 (11)	O3—C12—C9	114.6 (4)
O1—Dy—C18	104.46 (11)	N3—C13—C14	124.5 (5)
O10—Dy—C18	87.36 (11)	N3—C13—H13	117.7
O9—Dy—C18	93.40 (11)	C14—C13—H13	117.7
O6—Dy—C18	26.21 (10)	C15—C14—C13	119.1 (5)
O5—Dy—C18	26.58 (10)	C15—C14—H14	120.4
O3—Cu—O3ⁱⁱ	180.000 (1)	C13—C14—H14	120.4
O3—Cu—N1	89.27 (12)	C14—C15—C16	117.4 (4)
O3ⁱⁱ—Cu—N1	90.73 (12)	C14—C15—C18	122.3 (4)
O3—Cu—N1ⁱⁱ	90.73 (12)	C16—C15—C18	120.2 (4)
O3ⁱⁱ—Cu—N1ⁱⁱ	89.27 (12)	C17—C16—C15	119.2 (4)
N1—Cu—N1ⁱⁱ	180.00 (17)	C17—C16—H16	120.4
O3—Cu—N4ⁱⁱⁱ	102.43 (12)	C15—C16—H16	120.4
O3ⁱⁱ—Cu—N4ⁱⁱⁱ	77.57 (12)	N3—C17—C16	124.0 (5)
N1—Cu—N4ⁱⁱⁱ	93.04 (14)	N3—C17—H17	118.0
N1ⁱⁱ—Cu—N4ⁱⁱⁱ	86.96 (14)	C16—C17—H17	118.0
C6—O1—Dy	140.1 (3)	O6—C18—O5	121.4 (3)
C6—O2—Dyⁱ	150.7 (3)	O6—C18—C15	119.2 (4)
C12—O3—Cu	137.0 (3)	O5—C18—C15	119.3 (4)
C18—O5—Dy	90.7 (2)	O6—C18—Dy	59.05 (19)
C18—O6—Dy	94.7 (2)	O5—C18—Dy	62.69 (19)
C24—O7—Dy	143.9 (3)	C15—C18—Dy	172.3 (3)
C24—O8—Dyⁱ	144.4 (3)	N4—C19—C20	125.5 (5)
Dy—O9—H9A	118 (3)	N4—C19—H19	117.3
Dy—O9—H9B	124 (3)	C20—C19—H19	117.3
H9A—O9—H9B	105 (5)	C19—C20—C21	118.0 (5)
Dy—O10—H10A	125 (3)	C19—C20—H20	121.0
Dy—O10—H10B	133 (4)	C21—C20—H20	121.0
H10A—O10—H10B	102 (5)	C20—C21—C22	118.3 (4)
C5—N1—C1	117.4 (3)	C20—C21—C24	121.2 (4)
C5—N1—Cu	123.0 (3)	C22—C21—C24	120.5 (4)
C1—N1—Cu	119.6 (3)	C23—C22—C21	117.8 (4)
C11—N2—C7	115.7 (4)	C23—C22—H22	121.1
C17—N3—C13	115.7 (4)	C21—C22—H22	121.1
C19—N4—C23	115.9 (4)	N4—C23—C22	124.3 (5)
N1—C1—C2	122.8 (3)	N4—C23—H23	117.8
N1—C1—H1	118.6	C22—C23—H23	117.8
C2—C1—H1	118.6	O8—C24—O7	126.3 (4)
C1—C2—C3	119.7 (4)	O8—C24—C21	117.1 (4)
C1—C2—H2	120.2	O7—C24—C21	116.5 (4)

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y, −z+1; (iii) −x+1/2, y−1/2, −z+3/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O9—H9A···O4^iv	0.81 (3)	1.98 (3)	2.778 (4)	169 (5)
O9—H9B···N3^v	0.82 (3)	2.07 (3)	2.883 (5)	176 (5)
O10—H10A···O5^vi	0.82 (3)	1.98 (2)	2.784 (4)	166 (5)
O10—H10B···N2^vii	0.81 (4)	1.99 (2)	2.796 (5)	169 (6)

Symmetry codes: (iv) x, y+1, z; (v) x−1/2, −y+3/2, z+1/2; (vi) −x+1, −y+1, −z+1; (vii) x+1/2, −y+1/2, z+1/2.

Experimental details

Crystal data
Chemical formula	[Dy₂Cu(C₆H₄NO₂)₈(H₂O)₄]
M_r	1437.43
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	294
a, b, c (Å)	9.456 (1), 14.966 (3), 18.166 (4)
β (°)	93.74 (1)
V (Å³)	2565.4 (8)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	3.38
Crystal size (mm)	0.54 × 0.42 × 0.28

Data collection
Diffractometer	Bruker SMART 1000 CCD area-detector
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.199, 0.391
No. of measured, independent and observed [I > 2σ(I)] reflections	5313, 4638, 3853
R_int	0.018
(sin θ/λ)_max (Å⁻¹)	0.600

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.026, 0.058, 1.03
No. of reflections	4638
No. of parameters	375
No. of restraints	4
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.61, −0.89

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2001).

Selected bond lengths (Å) top

Dy—O7	2.298 (3)	Dy—O6	2.433 (3)
Dy—O2ⁱ	2.300 (3)	Dy—O5	2.513 (3)
Dy—O8ⁱ	2.313 (3)	Cu—O3	1.976 (3)
Dy—O1	2.324 (3)	Cu—N1	2.004 (3)
Dy—O10	2.366 (3)	Cu—N4ⁱⁱ	2.639 (4)
Dy—O9	2.409 (3)

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1/2, y−1/2, −z+3/2.