Poly[[μ(2)-acetato-aquadi-μ(3)-isonicotinato-dysprosium(III)silver(I)] perchlorate].

In the title three-dimensional heterometallic complex, {[AgDy(C(6)H(4)NO(2))(2)(C(2)H(3)O(2))(H(2)O)]ClO(4)}(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 mol-ecule. 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 mol-ecules link the carboxyl-ate 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 = 691.08

Monoclinic,

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[F 2 > 2σ(F 2)] = 0.023

wR(F 2) = 0.056

S = 1.04

3486 reflections

322 parameters

158 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.66 e Å−3

Δρmin = −0.76 e Å−3

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.

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

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

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

[AgDy(C6H4NO2)2(C2H3O2)(H2O)]ClO4	F(000) = 1316
Mr = 691.08	Dx = 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

Bruker APEXII area-detector diffractometer	3486 independent reflections
Radiation source: fine-focus sealed tube	3112 reflections with I > 2σ(I)
graphite	Rint = 0.025
φ and ω scan	θmax = 25.2°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −15→19
Tmin = 0.328, Tmax = 0.386	k = −18→17
9904 measured reflections	l = −8→9

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 = 1.03	w = 1/[σ2(Fo2) + (0.0236P)2 + 3.5237P] where P = (Fo2 + 2Fc2)/3
3486 reflections	(Δ/σ)max = 0.002
322 parameters	Δρmax = 0.66 e Å−3
158 restraints	Δρmin = −0.76 e Å−3

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

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

	x	y	z	Uiso*/Ueq	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)

	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)

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—Dy1iv	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—Ag1v	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—Dy1iv	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—Ag1v	122.7 (3)	O9—Cl1—O10	109.7 (10)
C4—N1—Ag1v	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)

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···O5iv	0.79 (3)	2.05 (4)	2.813 (4)	161 (5)

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) ; (ii) .