Poly[[μ2-acetato-aquadi-μ3-isonicotinato-dysprosium(III)silver(I)] perchlorate]

Zhu, L.-C.

doi:10.1107/S1600536809046637

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 12| December 2009| Pages m1595-m1596

doi:10.1107/S1600536809046637

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Poly[[μ₂-acetato-aquadi-μ₃-isonicotinato-dysprosium(III)silver(I)] perchlorate]

Li-Cai Zhu ^a ^*

^aSchool of Chemistry and Environment, South China Normal University, Guangzhou 510631, People's Republic of China
^*Correspondence e-mail: licaizhu1977@yahoo.com.cn

(Received 20 October 2009; accepted 5 November 2009; online 18 November 2009)

In the title three-dimensional heterometallic complex, {[AgDy(C₆H₄NO₂)₂(C₂H₃O₂)(H₂O)]ClO₄}_n, the Dy(III) ion is eight-coordinated by four O atoms from four different isonicotinate ligands, three O atoms from two different acetate ligands and one O atom of water molecule. The two-coordinate Ag^I ion is bonded to two N atoms from two different isonicotinate anions. These metal coordination units are connected by bridging isonicotinate and acetate ligands, generating a three-dimensional network. The coordinated water molecules link the carboxylate group and the acetate ligand by O—H⋯O hydrogen bonding. The perchlorate anion is disordered over two sites with site occupancy factors 0.508 (12) and 0.492 (12) and the methyl group of the acetate ligand is disordered over two positions of equal occupancy.

Related literature

For the applications of lanthanide–transition metal heterometallic complexes with bridging multifunctional organic ligands in ion exchange, magnetism, bimetallic catalysis and as luminescent probes, see: Cheng et al. (2006 ); Kuang et al. (2007 ); Peng et al. (2008 ); Zhu et al. (2009 ).

Experimental

Crystal data

[AgDy(C₆H₄NO₂)₂(C₂H₃O₂)(H₂O)]ClO₄
M_r = 691.08
Monoclinic, P 2₁ /c
a = 16.1682 (15) Å
b = 15.1020 (14) Å
c = 7.9846 (7) Å
β = 92.845 (1)°
V = 1947.2 (3) Å³
Z = 4
Mo Kα radiation
μ = 5.01 mm⁻¹
T = 296 K
0.23 × 0.20 × 0.19 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.328, T_max = 0.386
9904 measured reflections
3486 independent reflections
3112 reflections with I > 2σ(I)
R_int = 0.025

Refinement

R[F² > 2σ(F²)] = 0.023
wR(F²) = 0.056
S = 1.04
3486 reflections
322 parameters
158 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.66 e Å⁻³
Δρ_min = −0.76 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H2W⋯O2ⁱ	0.79 (3)	2.21 (4)	2.925 (4)	150 (5)
O1W—H1W⋯O5ⁱⁱ	0.79 (3)	2.05 (4)	2.813 (4)	161 (5)
Symmetry codes: (i) $[x, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ ; (ii) $[x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ .

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

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809046637/zq2015sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809046637/zq2015Isup2.hkl

checkCIF report

Comment top

In the past few years, lanthanide-transition metal heterometallic complexs with bridging multifunctionnal organic ligands are of increasing interest, not only because of their impressive topological structures, but also due to their versatile applications in ion exchange, magnetism, bimetallic catalysis and luminescent probe(Cheng et al., 2006; Kuang et al., 2007; Peng et al., 2008; Zhu et al., 2009). As an extension of this research, the structure of the title compound, a new heterometallic coordination polymer, (I), has been determined which is presented in this article.

In the title compound (Fig. 1), there are one Dy(III) ion, one Ag(I) ion, two halves of acetate ligand, two isonicotinate ligands, one coordinated water molecule, and one perchlorate anion in the asymmetric unit. Each Dy(III) ion is eight-coordinated by four O atoms from four different isonicotinate ligands [Dy—O distances ranging from 2.297 (3) to 2.348 (3) Å], and three O atoms from two different acetate ligands [Dy—O distances ranging from 2.394 (3) to 2.484 (3) Å], and one O atom of water molecule [Dy—O distances 2.414 (3) Å]. The O—Dy—O bond angles are in the range from 52.70 (10) to 155.05 (10) °. The Dy center can be described as having a bicapped trigonal prism coordination geometry. The two-coordinate Ag(I) ion is bonded to two N atoms from two different isonicotinate anions [Ag—N distances 2.163 (4) Å]. Thus the Ag(I) ion is in a somewhat linear configuration with N1—Ag1—N2 angle 165.40 (17) °. These metal coordination units are connected by bridging isonicotinate and acetate ligands, generating a three-dimensional network (Fig. 2).The coordinated water molecules link the carboxylate group and acetate ligand by O—H···O hydrogen bonding (Table 1). The perchlorate anion is disordered over two sites with site occupancy factors 0.508 (12) and 0.492 (12). The methyl group of the acetate ligand is disordered over two positions of equal occupancy (0.5:0.5).

Related literature top

For the applications of lanthanide–transition metal heterometallic complexes with bridging multifunctional organic ligands in ion exchange, magnetism, bimetallic catalysis and as luminescent probes, see: Cheng et al. (2006); Kuang et al. (2007); Peng et al. (2008); Zhu et al. (2009).

Experimental top

A mixture of AgNO₃(0.057 g, 0.33 mmol), Dy₂O₃(0.116 g, 0.33 mmol), isonicotinic acid (0.164 g, 1.33 mmol), CH₃COONa(0.057 g, 0.7 mmol), H₂O(7 ml), and HClO₄(0.257 mmol)(pH 2) was sealed in a 20 ml Teflon-lined reaction vessel at 443 K for 6 days then slowly cooled to room temperature. The product was collected by filtration, washed with water and air-dried. Colorless block crystals suitable for X-ray analysis were obtained.

Computing details top

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

Figures top

	Fig. 1. The molecular structure showing the atomic-numbering scheme and displacement ellipsoids drawn at the 30% probability level. Symmetry codes: (A) 1 + x, 1.5 - y, -1/2 + z; (B) 1 - x, 1 - y, 2 - z; (C) x, 1.5 - y, 1/2 + z.
	Fig. 2. A view of the three-dimensional structure of the title compound. Hydrogen atoms are omitted for clarity.

Poly[[µ₂-acetato-aquadi-µ₃-isonicotinato-dysprosium(III)silver(I)] perchlorate] top

Crystal data top

[AgDy(C₆H₄NO₂)₂(C₂H₃O₂)(H₂O)]ClO₄	F(000) = 1316
M_r = 691.08	D_x = 2.357 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 5589 reflections
a = 16.1682 (15) Å	θ = 2.7–27.8°
b = 15.1020 (14) Å	µ = 5.01 mm⁻¹
c = 7.9846 (7) Å	T = 296 K
β = 92.845 (1)°	Block, colorless
V = 1947.2 (3) Å³	0.23 × 0.20 × 0.19 mm
Z = 4

Data collection top

Bruker APEXII area-detector diffractometer	3486 independent reflections
Radiation source: fine-focus sealed tube	3112 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.025
ϕ and ω scan	θ_max = 25.2°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −15→19
T_min = 0.328, T_max = 0.386	k = −18→17
9904 measured reflections	l = −8→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)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.056	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ²(F_o²) + (0.0236P)² + 3.5237P] where P = (F_o² + 2F_c²)/3
3486 reflections	(Δ/σ)_max = 0.002
322 parameters	Δρ_max = 0.66 e Å⁻³
158 restraints	Δρ_min = −0.76 e Å⁻³

Crystal data top

[AgDy(C₆H₄NO₂)₂(C₂H₃O₂)(H₂O)]ClO₄	V = 1947.2 (3) Å³
M_r = 691.08	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 16.1682 (15) Å	µ = 5.01 mm⁻¹
b = 15.1020 (14) Å	T = 296 K
c = 7.9846 (7) Å	0.23 × 0.20 × 0.19 mm
β = 92.845 (1)°

Data collection top

Bruker APEXII area-detector diffractometer	3486 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	3112 reflections with I > 2σ(I)
T_min = 0.328, T_max = 0.386	R_int = 0.025
9904 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.023	158 restraints
wR(F²) = 0.056	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	Δρ_max = 0.66 e Å⁻³
3486 reflections	Δρ_min = −0.76 e Å⁻³
322 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	Occ. (<1)
Dy1	0.454540 (11)	0.616178 (12)	1.04948 (2)	0.01852 (7)
Ag1	0.97316 (3)	0.73989 (4)	0.60071 (7)	0.06665 (17)
O1	0.35829 (18)	0.81592 (19)	0.7190 (4)	0.0300 (7)
O2	0.38143 (17)	0.68117 (19)	0.8281 (4)	0.0263 (7)
O3	0.5762 (2)	0.6330 (2)	0.9080 (5)	0.0401 (9)
O4	0.63060 (19)	0.49745 (19)	0.8632 (5)	0.0403 (9)
O5	0.5347 (2)	0.6149 (2)	1.3147 (4)	0.0360 (8)
O6	0.54781 (19)	0.4970 (2)	1.1607 (4)	0.0320 (7)
O1W	0.4979 (2)	0.7687 (2)	1.0758 (4)	0.0358 (8)
H1W	0.518 (3)	0.795 (3)	1.002 (6)	0.054*
H2W	0.475 (3)	0.800 (3)	1.139 (6)	0.054*
N1	0.0943 (2)	0.7527 (3)	0.9981 (6)	0.0404 (10)
N2	0.8576 (3)	0.6967 (3)	0.6991 (6)	0.0500 (12)
C1	0.2516 (3)	0.7494 (3)	0.8695 (5)	0.0231 (9)
C2	0.2116 (3)	0.6710 (3)	0.9112 (6)	0.0312 (11)
H1	0.2372	0.6165	0.8967	0.037*
C3	0.1336 (3)	0.6753 (3)	0.9741 (7)	0.0388 (12)
H2	0.1072	0.6229	1.0008	0.047*
C4	0.1333 (3)	0.8284 (4)	0.9589 (7)	0.0446 (13)
H3	0.1068	0.8821	0.9760	0.054*
C5	0.2109 (3)	0.8294 (3)	0.8945 (6)	0.0335 (11)
H4	0.2358	0.8828	0.8680	0.040*
C6	0.3367 (2)	0.7495 (3)	0.8008 (5)	0.0202 (9)
C7	0.6332 (3)	0.5809 (3)	0.8637 (6)	0.0303 (10)
C8	0.7113 (3)	0.6231 (3)	0.8058 (6)	0.0293 (10)
C9	0.7156 (3)	0.7123 (3)	0.7613 (7)	0.0410 (13)
H7	0.6693	0.7486	0.7668	0.049*
C10	0.7894 (3)	0.7458 (4)	0.7088 (8)	0.0489 (15)
H8	0.7917	0.8053	0.6791	0.059*
C11	0.8533 (3)	0.6108 (4)	0.7457 (9)	0.0568 (17)
H5	0.9009	0.5763	0.7427	0.068*
C12	0.7818 (3)	0.5719 (3)	0.7975 (7)	0.0428 (13)
H6	0.7810	0.5123	0.8264	0.051*
C13	0.5697 (3)	0.5411 (3)	1.2898 (5)	0.0276 (10)
C14	0.6271 (11)	0.5015 (17)	1.421 (3)	0.045 (4)	0.50
H14A	0.6719	0.5418	1.4467	0.068*	0.50
H14B	0.6487	0.4468	1.3804	0.068*	0.50
H14C	0.5976	0.4905	1.5203	0.068*	0.50
C14'	0.6444 (10)	0.5127 (17)	1.393 (3)	0.045 (4)	0.50
H14D	0.6503	0.5488	1.4915	0.068*	0.50
H14E	0.6926	0.5191	1.3282	0.068*	0.50
H14F	0.6385	0.4518	1.4246	0.068*	0.50
Cl1	0.9165 (8)	0.9620 (9)	0.7618 (15)	0.0633 (8)	0.492 (12)
O7	0.9742 (9)	0.8934 (9)	0.785 (2)	0.138 (7)	0.492 (12)
O8	0.8752 (9)	0.9496 (8)	0.6037 (14)	0.105 (5)	0.492 (12)
O9	0.9544 (10)	1.0465 (9)	0.761 (2)	0.074 (5)	0.492 (12)
O10	0.8556 (9)	0.9600 (10)	0.8849 (19)	0.139 (7)	0.492 (12)
Cl1'	0.9216 (7)	0.9553 (8)	0.7502 (15)	0.0633 (8)	0.508 (12)
O7'	0.9307 (9)	0.8895 (9)	0.8748 (17)	0.125 (6)	0.508 (12)
O8'	0.9565 (10)	0.9226 (10)	0.6054 (17)	0.139 (6)	0.508 (12)
O9'	0.9612 (10)	1.0334 (9)	0.809 (2)	0.090 (6)	0.508 (12)
O10'	0.8355 (6)	0.9715 (7)	0.720 (2)	0.101 (5)	0.508 (12)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy1	0.01576 (11)	0.01481 (11)	0.02554 (12)	0.00081 (7)	0.00650 (8)	0.00006 (8)
Ag1	0.0261 (2)	0.0917 (4)	0.0846 (4)	−0.0148 (2)	0.0267 (2)	0.0028 (3)
O1	0.0256 (16)	0.0230 (16)	0.0424 (19)	0.0016 (13)	0.0128 (14)	0.0096 (14)
O2	0.0190 (15)	0.0247 (15)	0.0357 (18)	0.0039 (12)	0.0055 (13)	0.0049 (13)
O3	0.0302 (19)	0.0227 (17)	0.071 (3)	−0.0018 (13)	0.0332 (18)	−0.0015 (16)
O4	0.0337 (18)	0.0193 (16)	0.070 (2)	−0.0035 (14)	0.0288 (17)	−0.0028 (16)
O5	0.044 (2)	0.0315 (18)	0.0319 (18)	0.0101 (15)	−0.0040 (15)	−0.0092 (14)
O6	0.0376 (18)	0.0270 (16)	0.0304 (17)	0.0082 (14)	−0.0078 (14)	−0.0062 (14)
O1W	0.049 (2)	0.0228 (17)	0.038 (2)	−0.0094 (15)	0.0213 (17)	−0.0029 (14)
N1	0.023 (2)	0.049 (3)	0.051 (3)	0.0021 (18)	0.0138 (19)	−0.003 (2)
N2	0.028 (2)	0.050 (3)	0.074 (3)	−0.009 (2)	0.022 (2)	−0.002 (2)
C1	0.017 (2)	0.028 (2)	0.024 (2)	0.0005 (17)	0.0038 (17)	0.0033 (17)
C2	0.020 (2)	0.026 (2)	0.049 (3)	−0.0004 (18)	0.011 (2)	0.000 (2)
C3	0.025 (2)	0.037 (3)	0.056 (3)	−0.006 (2)	0.017 (2)	−0.001 (2)
C4	0.033 (3)	0.040 (3)	0.062 (4)	0.013 (2)	0.014 (3)	−0.002 (3)
C5	0.027 (2)	0.025 (2)	0.050 (3)	0.0046 (19)	0.012 (2)	0.004 (2)
C6	0.016 (2)	0.020 (2)	0.024 (2)	−0.0002 (16)	0.0040 (17)	0.0002 (17)
C7	0.023 (2)	0.028 (2)	0.041 (3)	−0.0069 (19)	0.016 (2)	−0.001 (2)
C8	0.023 (2)	0.026 (2)	0.041 (3)	−0.0048 (18)	0.014 (2)	−0.003 (2)
C9	0.025 (3)	0.029 (3)	0.070 (4)	0.000 (2)	0.017 (2)	0.004 (2)
C10	0.032 (3)	0.036 (3)	0.081 (4)	−0.010 (2)	0.021 (3)	0.007 (3)
C11	0.026 (3)	0.047 (3)	0.100 (5)	0.000 (2)	0.019 (3)	−0.004 (3)
C12	0.027 (3)	0.031 (3)	0.073 (4)	0.001 (2)	0.017 (3)	−0.001 (3)
C13	0.026 (2)	0.032 (2)	0.025 (2)	0.0036 (19)	−0.0008 (19)	−0.0022 (19)
C14	0.046 (6)	0.045 (5)	0.044 (6)	0.006 (5)	−0.012 (5)	−0.003 (4)
C14'	0.046 (6)	0.045 (5)	0.044 (6)	0.006 (5)	−0.012 (5)	−0.003 (4)
Cl1	0.0616 (15)	0.0502 (16)	0.0776 (16)	0.0036 (11)	−0.0019 (11)	−0.0024 (12)
O7	0.145 (10)	0.105 (8)	0.162 (11)	0.076 (7)	−0.030 (8)	−0.017 (7)
O8	0.132 (10)	0.108 (8)	0.072 (7)	−0.039 (7)	−0.042 (7)	0.005 (6)
O9	0.068 (8)	0.060 (7)	0.094 (8)	−0.011 (6)	0.012 (6)	−0.003 (6)
O10	0.135 (10)	0.151 (10)	0.136 (10)	−0.038 (8)	0.054 (8)	−0.009 (8)
Cl1'	0.0616 (15)	0.0502 (16)	0.0776 (16)	0.0036 (11)	−0.0019 (11)	−0.0024 (12)
O7'	0.140 (10)	0.120 (9)	0.112 (8)	−0.019 (7)	−0.017 (7)	0.066 (7)
O8'	0.163 (10)	0.142 (9)	0.119 (9)	0.012 (8)	0.063 (8)	−0.035 (7)
O9'	0.074 (8)	0.082 (9)	0.115 (10)	−0.034 (7)	0.006 (7)	−0.038 (7)
O10'	0.055 (6)	0.088 (7)	0.160 (10)	0.004 (5)	−0.008 (6)	0.008 (7)

Geometric parameters (Å, º) top

Dy1—O2	2.297 (3)	C2—C3	1.382 (6)
Dy1—O4ⁱ	2.328 (3)	C2—H1	0.9300
Dy1—O3	2.330 (3)	C3—H2	0.9300
Dy1—O1ⁱⁱ	2.348 (3)	C4—C5	1.380 (6)
Dy1—O6ⁱ	2.394 (3)	C4—H3	0.9300
Dy1—O1W	2.414 (3)	C5—H4	0.9300
Dy1—O5	2.428 (3)	C7—C8	1.509 (6)
Dy1—O6	2.484 (3)	C8—C12	1.381 (6)
Dy1—C13	2.842 (4)	C8—C9	1.395 (6)
Dy1—Dy1ⁱ	3.9005 (5)	C9—C10	1.381 (6)
Ag1—N2	2.163 (4)	C9—H7	0.9300
Ag1—N1ⁱⁱⁱ	2.163 (4)	C10—H8	0.9300
O1—C6	1.256 (5)	C11—C12	1.379 (7)
O1—Dy1^iv	2.348 (3)	C11—H5	0.9300
O2—C6	1.272 (5)	C12—H6	0.9300
O3—C7	1.275 (5)	C13—C14	1.490 (9)
O4—C7	1.261 (5)	C13—C14'	1.490 (9)
O4—Dy1ⁱ	2.328 (3)	C14—H14A	0.9600
O5—C13	1.269 (5)	C14—H14B	0.9600
O6—C13	1.263 (5)	C14—H14C	0.9600
O6—Dy1ⁱ	2.394 (3)	C14'—H14D	0.9600
O1W—H1W	0.79 (3)	C14'—H14E	0.9600
O1W—H2W	0.79 (3)	C14'—H14F	0.9600
N1—C3	1.348 (6)	Cl1—O7	1.399 (12)
N1—C4	1.350 (7)	Cl1—O8	1.411 (12)
N1—Ag1^v	2.163 (4)	Cl1—O9	1.416 (11)
N2—C10	1.335 (7)	Cl1—O10	1.426 (12)
N2—C11	1.351 (7)	Cl1'—O8'	1.401 (12)
C1—C5	1.394 (6)	Cl1'—O7'	1.408 (12)
C1—C2	1.398 (6)	Cl1'—O9'	1.411 (11)
C1—C6	1.506 (5)	Cl1'—O10'	1.420 (11)

O2—Dy1—O4ⁱ	104.83 (12)	C2—C1—C6	121.9 (4)
O2—Dy1—O3	89.71 (12)	C3—C2—C1	119.1 (4)
O4ⁱ—Dy1—O3	138.72 (10)	C3—C2—H1	120.4
O2—Dy1—O1ⁱⁱ	85.79 (11)	C1—C2—H1	120.4
O4ⁱ—Dy1—O1ⁱⁱ	74.38 (10)	N1—C3—C2	122.6 (4)
O3—Dy1—O1ⁱⁱ	146.22 (10)	N1—C3—H2	118.7
O2—Dy1—O6ⁱ	77.05 (10)	C2—C3—H2	118.7
O4ⁱ—Dy1—O6ⁱ	72.23 (11)	N1—C4—C5	122.6 (4)
O3—Dy1—O6ⁱ	73.89 (11)	N1—C4—H3	118.7
O1ⁱⁱ—Dy1—O6ⁱ	136.70 (11)	C5—C4—H3	118.7
O2—Dy1—O1W	78.20 (12)	C4—C5—C1	119.2 (4)
O4ⁱ—Dy1—O1W	148.29 (11)	C4—C5—H4	120.4
O3—Dy1—O1W	71.91 (11)	C1—C5—H4	120.4
O1ⁱⁱ—Dy1—O1W	74.40 (11)	O1—C6—O2	124.5 (4)
O6ⁱ—Dy1—O1W	137.44 (11)	O1—C6—C1	118.2 (3)
O2—Dy1—O5	155.05 (10)	O2—C6—C1	117.3 (3)
O4ⁱ—Dy1—O5	91.77 (13)	O4—C7—O3	126.4 (4)
O3—Dy1—O5	89.81 (13)	O4—C7—C8	116.7 (4)
O1ⁱⁱ—Dy1—O5	80.85 (11)	O3—C7—C8	116.9 (4)
O6ⁱ—Dy1—O5	126.52 (10)	C12—C8—C9	118.5 (4)
O1W—Dy1—O5	77.96 (12)	C12—C8—C7	119.0 (4)
O2—Dy1—O6	149.85 (10)	C9—C8—C7	122.5 (4)
O4ⁱ—Dy1—O6	73.52 (11)	C10—C9—C8	119.0 (5)
O3—Dy1—O6	74.95 (11)	C10—C9—H7	120.5
O1ⁱⁱ—Dy1—O6	121.22 (11)	C8—C9—H7	120.5
O6ⁱ—Dy1—O6	73.84 (12)	N2—C10—C9	122.8 (5)
O1W—Dy1—O6	119.46 (12)	N2—C10—H8	118.6
O5—Dy1—O6	52.70 (10)	C9—C10—H8	118.6
O2—Dy1—C13	169.94 (11)	N2—C11—C12	123.1 (5)
O4ⁱ—Dy1—C13	83.17 (13)	N2—C11—H5	118.4
O3—Dy1—C13	80.23 (13)	C12—C11—H5	118.4
O1ⁱⁱ—Dy1—C13	102.45 (12)	C11—C12—C8	118.8 (5)
O6ⁱ—Dy1—C13	100.12 (12)	C11—C12—H6	120.6
O1W—Dy1—C13	98.28 (13)	C8—C12—H6	120.6
O5—Dy1—C13	26.41 (11)	O6—C13—O5	118.8 (4)
O6—Dy1—C13	26.36 (11)	O6—C13—C14	120.1 (11)
O2—Dy1—Dy1ⁱ	114.40 (7)	O5—C13—C14	120.6 (11)
O4ⁱ—Dy1—Dy1ⁱ	68.41 (7)	O6—C13—C14'	119.0 (11)
O3—Dy1—Dy1ⁱ	70.39 (7)	O5—C13—C14'	121.4 (12)
O1ⁱⁱ—Dy1—Dy1ⁱ	140.97 (7)	C14—C13—C14'	15.6 (17)
O6ⁱ—Dy1—Dy1ⁱ	37.71 (7)	O6—C13—Dy1	60.8 (2)
O1W—Dy1—Dy1ⁱ	139.94 (8)	O5—C13—Dy1	58.3 (2)
O5—Dy1—Dy1ⁱ	88.82 (7)	C14—C13—Dy1	177.5 (10)
O6—Dy1—Dy1ⁱ	36.13 (7)	C14'—C13—Dy1	166.7 (9)
C13—Dy1—Dy1ⁱ	62.43 (9)	C13—C14—H14A	109.5
N2—Ag1—N1ⁱⁱⁱ	165.40 (17)	C13—C14—H14B	109.5
C6—O1—Dy1^iv	149.1 (3)	C13—C14—H14C	109.5
C6—O2—Dy1	138.1 (3)	C13—C14'—H14D	109.5
C7—O3—Dy1	134.9 (3)	C13—C14'—H14E	109.5
C7—O4—Dy1ⁱ	139.1 (3)	H14D—C14'—H14E	109.5
C13—O5—Dy1	95.3 (3)	C13—C14'—H14F	109.5
C13—O6—Dy1ⁱ	160.5 (3)	H14D—C14'—H14F	109.5
C13—O6—Dy1	92.8 (3)	H14E—C14'—H14F	109.5
Dy1ⁱ—O6—Dy1	106.16 (12)	O7—Cl1—O8	107.5 (10)
Dy1—O1W—H1W	123 (4)	O7—Cl1—O9	112.5 (10)
Dy1—O1W—H2W	119 (4)	O8—Cl1—O9	107.4 (10)
H1W—O1W—H2W	113 (5)	O7—Cl1—O10	111.9 (11)
C3—N1—C4	118.2 (4)	O8—Cl1—O10	107.5 (10)
C3—N1—Ag1^v	122.7 (3)	O9—Cl1—O10	109.7 (10)
C4—N1—Ag1^v	119.1 (3)	O8'—Cl1'—O7'	107.6 (10)
C10—N2—C11	117.6 (4)	O8'—Cl1'—O9'	111.8 (10)
C10—N2—Ag1	125.7 (4)	O7'—Cl1'—O9'	109.0 (10)
C11—N2—Ag1	116.5 (3)	O8'—Cl1'—O10'	110.8 (10)
C5—C1—C2	118.3 (4)	O7'—Cl1'—O10'	107.9 (10)
C5—C1—C6	119.8 (4)	O9'—Cl1'—O10'	109.6 (10)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H2W···O2ⁱⁱ	0.79 (3)	2.21 (4)	2.925 (4)	150 (5)
O1W—H1W···O5^iv	0.79 (3)	2.05 (4)	2.813 (4)	161 (5)

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

Experimental details

Crystal data
Chemical formula	[AgDy(C₆H₄NO₂)₂(C₂H₃O₂)(H₂O)]ClO₄
M_r	691.08
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	296
a, b, c (Å)	16.1682 (15), 15.1020 (14), 7.9846 (7)
β (°)	92.845 (1)
V (Å³)	1947.2 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	5.01
Crystal size (mm)	0.23 × 0.20 × 0.19

Data collection
Diffractometer	Bruker APEXII area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.328, 0.386
No. of measured, independent and observed [I > 2σ(I)] reflections	9904, 3486, 3112
R_int	0.025
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.023, 0.056, 1.04
No. of reflections	3486
No. of parameters	322
No. of restraints	158
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.66, −0.76

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H2W···O2ⁱ	0.79 (3)	2.21 (4)	2.925 (4)	150 (5)
O1W—H1W···O5ⁱⁱ	0.79 (3)	2.05 (4)	2.813 (4)	161 (5)

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

Acknowledgements

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

References

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