metal-organic compounds
Poly[[μ2-acetato-aquadi-μ3-isonicotinato-erbium(III)silver(I)] perchlorate]
aSchool of Chemistry and Environment, South China Normal University, Guangzhou 510631, People's Republic of China
*Correspondence e-mail: licaizhu1977@yahoo.com.cn
In the title three-dimensional heterometallic complex, {[AgEr(C6H4NO2)2(C2H3O2)(H2O)]ClO4}n, the eight-coordinate ErIII ion adopts a distorted bicapped trigonal-prismatic geometry, being coordinated by four O atoms from four different isonicotinate ligands, three O atoms from two different acetate ligands and one O atom of the water molecule. The two-coordinate AgI ion is surrounded by two N atoms from two different isonicotinate anions in a slightly bent configuration. These building blocks are connected by bridging isonicotinate and acetate ligands, generating a three-dimensional network. Ths structure is consolidated by O—H⋯O hydrogen bonding between the coordinated water molecule and a carboxylate group of the acetate ligand. The perchlorate anion is disordered over two sites with site-occupancy factors of 0.526 (13) and 0.474 (13), while the methyl group of the acetate ligand is equally disordered over two sites.
Related literature
For background to lanthanide–transition metal heterometallic complexes, see: Cheng et al. (2006); Kuang et al. (2007); Peng et al. (2008); Zhu et al. (2009).
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2004); cell 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
10.1107/S1600536809048429/wm2280sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536809048429/wm2280Isup2.hkl
A mixture of AgNO3 (0.057 g, 0.33 mmol), Er2O3 (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 and then slowly cooled to room temperature. The product was collected by filtration, washed with water and was air-dried. Colorless block-shaped crystals suitable for X-ray analysis were obtained.
H atoms bonded to C atoms were positioned geometrically and refined as riding, with C—H = 0.93 or 0.96 Å and Uiso(H) = 1.2 or 1.5 Ueq(C). H atoms of water molecules were found from difference Fourier maps and refined isotropically with a restraint of O—H = 0.81 - 0.82 Å. The perchlorate anion is disordered over two sites with site occupancy factors 0.526 (13) and 0.474 (13), whereas the methyl group of the acetate ligand is disordered over two sites with site occupancy factors 0.51 (5) and 0.49 (5).
Data collection: APEX2 (Bruker, 2004); cell
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).[AgEr(C6H4NO2)2(C2H3O2)(H2O)]ClO4 | F(000) = 1324 |
Mr = 695.84 | Dx = 2.433 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 4797 reflections |
a = 16.1952 (11) Å | θ = 2.5–27.9° |
b = 14.8673 (11) Å | µ = 5.62 mm−1 |
c = 7.8938 (6) Å | T = 296 K |
β = 91.783 (1)° | Block, colourless |
V = 1899.7 (2) Å3 | 0.23 × 0.20 × 0.19 mm |
Z = 4 |
Bruker APEXII area-detector diffractometer | 3423 independent reflections |
Radiation source: fine-focus sealed tube | 3009 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
ϕ and ω scan | θmax = 25.2°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −19→19 |
Tmin = 0.285, Tmax = 0.344 | k = −17→17 |
9611 measured reflections | l = −5→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)] = 0.025 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.057 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0218P)2 + 3.7155P] where P = (Fo2 + 2Fc2)/3 |
3423 reflections | (Δ/σ)max = 0.002 |
320 parameters | Δρmax = 0.76 e Å−3 |
158 restraints | Δρmin = −1.04 e Å−3 |
[AgEr(C6H4NO2)2(C2H3O2)(H2O)]ClO4 | V = 1899.7 (2) Å3 |
Mr = 695.84 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 16.1952 (11) Å | µ = 5.62 mm−1 |
b = 14.8673 (11) Å | T = 296 K |
c = 7.8938 (6) Å | 0.23 × 0.20 × 0.19 mm |
β = 91.783 (1)° |
Bruker APEXII area-detector diffractometer | 3423 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3009 reflections with I > 2σ(I) |
Tmin = 0.285, Tmax = 0.344 | Rint = 0.030 |
9611 measured reflections |
R[F2 > 2σ(F2)] = 0.025 | 158 restraints |
wR(F2) = 0.057 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | Δρmax = 0.76 e Å−3 |
3423 reflections | Δρmin = −1.04 e Å−3 |
320 parameters |
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) | |
Er1 | 0.955305 (12) | 0.883792 (13) | 0.05025 (3) | 0.01689 (8) | |
Ag1 | 0.47352 (3) | 0.74056 (4) | 0.10055 (8) | 0.06366 (18) | |
N1 | 0.3573 (3) | 0.6969 (3) | 0.1973 (7) | 0.0464 (13) | |
N2 | 0.5953 (3) | 0.7481 (3) | −0.0007 (6) | 0.0378 (11) | |
C1 | 0.1321 (3) | 0.5802 (3) | 0.3629 (7) | 0.0287 (12) | |
C2 | 0.2108 (3) | 0.6229 (3) | 0.3048 (7) | 0.0273 (11) | |
C3 | 0.2810 (3) | 0.5718 (4) | 0.2968 (8) | 0.0427 (15) | |
H8 | 0.2800 | 0.5114 | 0.3271 | 0.051* | |
C4 | 0.3527 (4) | 0.6105 (4) | 0.2436 (9) | 0.0523 (18) | |
H7 | 0.4000 | 0.5753 | 0.2397 | 0.063* | |
C5 | 0.2890 (3) | 0.7466 (4) | 0.2066 (9) | 0.0455 (16) | |
H11 | 0.2914 | 0.8070 | 0.1767 | 0.055* | |
C6 | 0.2147 (3) | 0.7121 (4) | 0.2589 (8) | 0.0378 (14) | |
H10 | 0.1681 | 0.7485 | 0.2630 | 0.045* | |
C7 | 0.6342 (3) | 0.6716 (4) | −0.0395 (8) | 0.0438 (15) | |
H4 | 0.6076 | 0.6171 | −0.0221 | 0.053* | |
C8 | 0.7122 (3) | 0.6709 (4) | −0.1041 (7) | 0.0340 (13) | |
H3 | 0.7372 | 0.6167 | −0.1315 | 0.041* | |
C9 | 0.7531 (3) | 0.7512 (3) | −0.1281 (6) | 0.0199 (10) | |
C10 | 0.8387 (3) | 0.7511 (3) | −0.1972 (6) | 0.0203 (10) | |
C11 | 0.7136 (3) | 0.8299 (3) | −0.0871 (7) | 0.0309 (12) | |
H6 | 0.7394 | 0.8851 | −0.1018 | 0.037* | |
C12 | 0.6349 (3) | 0.8258 (4) | −0.0237 (7) | 0.0359 (13) | |
H5 | 0.6085 | 0.8792 | 0.0040 | 0.043* | |
O1 | 0.0753 (2) | 0.6328 (2) | 0.4074 (5) | 0.0354 (9) | |
O2 | 0.1298 (2) | 0.4963 (2) | 0.3618 (5) | 0.0369 (9) | |
O3 | 0.85978 (19) | 0.6842 (2) | −0.2806 (4) | 0.0276 (8) | |
O4 | 0.88366 (18) | 0.8187 (2) | −0.1684 (4) | 0.0237 (7) | |
O1W | 0.9992 (2) | 0.7323 (2) | 0.0767 (5) | 0.0327 (9) | |
H1W | 1.017 (3) | 0.702 (3) | 0.001 (5) | 0.049* | |
H2W | 0.978 (3) | 0.697 (3) | 0.142 (5) | 0.049* | |
O6 | 1.0346 (2) | 0.8847 (2) | 0.3130 (4) | 0.0324 (8) | |
O5 | 1.0476 (2) | 1.0034 (2) | 0.1567 (4) | 0.0289 (8) | |
C13 | 1.0687 (3) | 0.9591 (3) | 0.2875 (6) | 0.0266 (11) | |
C14 | 1.1431 (13) | 0.9863 (19) | 0.395 (3) | 0.040 (4) | 0.51 (5) |
H14A | 1.1728 | 1.0327 | 0.3385 | 0.059* | 0.51 (5) |
H14B | 1.1785 | 0.9351 | 0.4129 | 0.059* | 0.51 (5) |
H14C | 1.1255 | 1.0082 | 0.5024 | 0.059* | 0.51 (5) |
C14' | 1.1264 (15) | 1.0028 (19) | 0.417 (3) | 0.040 (4) | 0.49 (5) |
H14D | 1.1142 | 1.0659 | 0.4230 | 0.059* | 0.49 (5) |
H14E | 1.1824 | 0.9947 | 0.3836 | 0.059* | 0.49 (5) |
H14F | 1.1191 | 0.9756 | 0.5255 | 0.059* | 0.49 (5) |
Cl1 | 0.58069 (12) | 0.04095 (12) | 0.7436 (3) | 0.0642 (5) | 0.526 (13) |
O7 | 0.5433 (10) | −0.0457 (8) | 0.742 (2) | 0.076 (5) | 0.526 (13) |
O8 | 0.5249 (9) | 0.1082 (9) | 0.709 (2) | 0.133 (6) | 0.526 (13) |
O9 | 0.6203 (10) | 0.0528 (9) | 0.9021 (14) | 0.109 (6) | 0.526 (13) |
O10 | 0.6454 (9) | 0.0386 (10) | 0.6206 (19) | 0.134 (7) | 0.526 (13) |
Cl1' | 0.58069 (12) | 0.04095 (12) | 0.7436 (3) | 0.0642 (5) | 0.474 (13) |
O7' | 0.5399 (11) | −0.0369 (9) | 0.691 (2) | 0.083 (7) | 0.474 (13) |
O8' | 0.5676 (11) | 0.1101 (10) | 0.6227 (19) | 0.124 (7) | 0.474 (13) |
O9' | 0.5422 (11) | 0.0751 (11) | 0.8943 (18) | 0.134 (7) | 0.474 (13) |
O10' | 0.6643 (6) | 0.0289 (8) | 0.778 (2) | 0.092 (5) | 0.474 (13) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Er1 | 0.01467 (12) | 0.01458 (12) | 0.02167 (13) | −0.00074 (8) | 0.00453 (8) | 0.00002 (8) |
Ag1 | 0.0248 (2) | 0.0863 (4) | 0.0813 (4) | −0.0136 (2) | 0.0248 (3) | 0.0023 (3) |
N1 | 0.025 (2) | 0.047 (3) | 0.067 (4) | −0.007 (2) | 0.017 (2) | 0.000 (3) |
N2 | 0.021 (2) | 0.045 (3) | 0.048 (3) | −0.003 (2) | 0.013 (2) | 0.000 (2) |
C1 | 0.028 (3) | 0.020 (3) | 0.039 (3) | −0.005 (2) | 0.012 (2) | −0.003 (2) |
C2 | 0.024 (3) | 0.028 (3) | 0.031 (3) | −0.005 (2) | 0.009 (2) | −0.003 (2) |
C3 | 0.025 (3) | 0.029 (3) | 0.075 (5) | 0.002 (2) | 0.015 (3) | 0.001 (3) |
C4 | 0.026 (3) | 0.048 (4) | 0.084 (5) | 0.004 (3) | 0.017 (3) | 0.000 (3) |
C5 | 0.031 (3) | 0.036 (3) | 0.071 (5) | −0.009 (3) | 0.016 (3) | 0.009 (3) |
C6 | 0.027 (3) | 0.030 (3) | 0.058 (4) | −0.001 (2) | 0.015 (3) | 0.005 (3) |
C7 | 0.035 (3) | 0.036 (3) | 0.061 (4) | −0.016 (3) | 0.012 (3) | 0.002 (3) |
C8 | 0.029 (3) | 0.026 (3) | 0.048 (4) | −0.003 (2) | 0.012 (3) | −0.001 (2) |
C9 | 0.016 (2) | 0.023 (3) | 0.020 (3) | −0.0031 (19) | 0.0016 (19) | −0.0025 (19) |
C10 | 0.018 (2) | 0.023 (3) | 0.021 (3) | 0.0015 (19) | 0.0023 (19) | 0.002 (2) |
C11 | 0.021 (2) | 0.026 (3) | 0.046 (3) | −0.004 (2) | 0.010 (2) | −0.001 (2) |
C12 | 0.026 (3) | 0.035 (3) | 0.047 (4) | 0.007 (2) | 0.012 (3) | 0.002 (3) |
O1 | 0.0258 (19) | 0.0208 (19) | 0.061 (3) | −0.0007 (15) | 0.0249 (19) | 0.0012 (16) |
O2 | 0.0296 (19) | 0.0196 (19) | 0.063 (3) | −0.0016 (15) | 0.0227 (18) | −0.0038 (17) |
O3 | 0.0246 (17) | 0.0214 (18) | 0.037 (2) | −0.0021 (14) | 0.0110 (16) | −0.0082 (15) |
O4 | 0.0179 (16) | 0.0250 (18) | 0.0283 (19) | −0.0051 (14) | 0.0042 (14) | −0.0058 (14) |
O1W | 0.045 (2) | 0.0204 (18) | 0.034 (2) | 0.0068 (16) | 0.0164 (18) | 0.0022 (15) |
O6 | 0.039 (2) | 0.033 (2) | 0.025 (2) | −0.0065 (16) | −0.0043 (16) | 0.0089 (15) |
O5 | 0.0335 (19) | 0.0248 (18) | 0.028 (2) | −0.0076 (15) | −0.0089 (16) | 0.0043 (15) |
C13 | 0.030 (3) | 0.023 (3) | 0.027 (3) | −0.001 (2) | −0.001 (2) | 0.000 (2) |
C14 | 0.038 (6) | 0.042 (6) | 0.037 (5) | −0.003 (5) | −0.011 (5) | 0.000 (4) |
C14' | 0.038 (6) | 0.042 (6) | 0.037 (5) | −0.003 (5) | −0.011 (5) | 0.000 (4) |
Cl1 | 0.0638 (11) | 0.0528 (10) | 0.0756 (13) | 0.0017 (9) | −0.0046 (10) | −0.0013 (9) |
O7 | 0.071 (8) | 0.070 (8) | 0.089 (9) | −0.025 (6) | 0.001 (6) | −0.009 (6) |
O8 | 0.140 (10) | 0.104 (9) | 0.153 (11) | 0.074 (7) | −0.032 (8) | −0.019 (7) |
O9 | 0.134 (10) | 0.110 (8) | 0.081 (8) | −0.042 (7) | −0.036 (7) | 0.001 (6) |
O10 | 0.133 (10) | 0.143 (10) | 0.130 (10) | −0.033 (8) | 0.052 (8) | −0.008 (8) |
Cl1' | 0.0638 (11) | 0.0528 (10) | 0.0756 (13) | 0.0017 (9) | −0.0046 (10) | −0.0013 (9) |
O7' | 0.073 (9) | 0.081 (9) | 0.096 (10) | −0.033 (7) | 0.011 (7) | −0.034 (7) |
O8' | 0.137 (11) | 0.121 (10) | 0.113 (10) | −0.009 (8) | −0.012 (8) | 0.056 (8) |
O9' | 0.150 (11) | 0.138 (10) | 0.118 (10) | 0.017 (8) | 0.064 (8) | −0.032 (8) |
O10' | 0.054 (6) | 0.077 (7) | 0.144 (11) | 0.004 (5) | −0.023 (7) | 0.009 (7) |
Er1—O4 | 2.266 (3) | C11—C12 | 1.386 (7) |
Er1—O2i | 2.289 (3) | C11—H6 | 0.9300 |
Er1—O1ii | 2.290 (3) | C12—H5 | 0.9300 |
Er1—O3iii | 2.308 (3) | O1—Er1v | 2.290 (3) |
Er1—O5iv | 2.341 (3) | O2—Er1vi | 2.289 (3) |
Er1—O1W | 2.369 (3) | O3—Er1vii | 2.308 (3) |
Er1—O6 | 2.405 (3) | O1W—H1W | 0.81 (4) |
Er1—O5 | 2.454 (3) | O1W—H2W | 0.82 (4) |
Ag1—N1 | 2.153 (4) | O6—C13 | 1.256 (6) |
Ag1—N2 | 2.154 (4) | O5—C13 | 1.263 (6) |
N1—C5 | 1.336 (7) | O5—Er1iv | 2.341 (3) |
N1—C4 | 1.337 (8) | C13—C14 | 1.507 (9) |
N2—C12 | 1.335 (7) | C13—C14' | 1.507 (10) |
N2—C7 | 1.341 (7) | C14—H14A | 0.9600 |
C1—O2 | 1.248 (6) | C14—H14B | 0.9600 |
C1—O1 | 1.266 (6) | C14—H14C | 0.9600 |
C1—C2 | 1.507 (6) | C14'—H14D | 0.9600 |
C2—C3 | 1.370 (7) | C14'—H14E | 0.9600 |
C2—C6 | 1.376 (7) | C14'—H14F | 0.9600 |
C3—C4 | 1.374 (8) | Cl1—O8 | 1.368 (9) |
C3—H8 | 0.9300 | Cl1—O10' | 1.384 (8) |
C4—H7 | 0.9300 | Cl1—O7' | 1.390 (9) |
C5—C6 | 1.382 (7) | Cl1—O9 | 1.399 (9) |
C5—H11 | 0.9300 | Cl1—O8' | 1.414 (10) |
C6—H10 | 0.9300 | Cl1—O7 | 1.423 (9) |
C7—C8 | 1.376 (7) | Cl1—O10 | 1.451 (9) |
C7—H4 | 0.9300 | Cl1—O9' | 1.452 (10) |
C8—C9 | 1.381 (7) | O8—O8' | 0.988 (19) |
C8—H3 | 0.9300 | O8—O9' | 1.557 (19) |
C9—C11 | 1.378 (7) | O9—O10' | 1.278 (15) |
C9—C10 | 1.505 (6) | O9—O9' | 1.307 (17) |
C10—O3 | 1.246 (5) | O10—O10' | 1.280 (17) |
C10—O4 | 1.258 (5) | O10—O8' | 1.650 (18) |
O4—Er1—O2i | 104.11 (13) | O4—C10—C9 | 117.9 (4) |
O4—Er1—O1ii | 90.06 (13) | C9—C11—C12 | 119.1 (5) |
O2i—Er1—O1ii | 139.15 (12) | C9—C11—H6 | 120.4 |
O4—Er1—O3iii | 85.24 (12) | C12—C11—H6 | 120.4 |
O2i—Er1—O3iii | 73.96 (11) | N2—C12—C11 | 122.5 (5) |
O1ii—Er1—O3iii | 146.30 (12) | N2—C12—H5 | 118.7 |
O4—Er1—O5iv | 77.04 (11) | C11—C12—H5 | 118.7 |
O2i—Er1—O5iv | 71.89 (13) | C1—O1—Er1v | 134.9 (3) |
O1ii—Er1—O5iv | 74.47 (12) | C1—O2—Er1vi | 138.3 (3) |
O3iii—Er1—O5iv | 135.93 (12) | C10—O3—Er1vii | 148.8 (3) |
O4—Er1—O1W | 78.85 (13) | C10—O4—Er1 | 139.3 (3) |
O2i—Er1—O1W | 148.19 (12) | Er1—O1W—H1W | 125 (4) |
O1ii—Er1—O1W | 71.58 (12) | Er1—O1W—H2W | 122 (4) |
O3iii—Er1—O1W | 74.77 (12) | H1W—O1W—H2W | 106 (4) |
O5iv—Er1—O1W | 137.91 (12) | C13—O6—Er1 | 95.3 (3) |
O4—Er1—O6 | 154.95 (12) | C13—O5—Er1iv | 160.6 (3) |
O2i—Er1—O6 | 92.59 (14) | C13—O5—Er1 | 92.8 (3) |
O1ii—Er1—O6 | 89.25 (14) | Er1iv—O5—Er1 | 106.35 (13) |
O3iii—Er1—O6 | 81.55 (12) | O6—C13—O5 | 118.7 (4) |
O5iv—Er1—O6 | 126.62 (11) | O6—C13—C14 | 119.6 (11) |
O1W—Er1—O6 | 77.18 (13) | O5—C13—C14 | 120.8 (11) |
O4—Er1—O5 | 149.53 (11) | O6—C13—C14' | 122.6 (12) |
O2i—Er1—O5 | 74.51 (12) | O5—C13—C14' | 118.3 (12) |
O1ii—Er1—O5 | 74.32 (12) | O6—C13—Er1 | 58.3 (2) |
O3iii—Er1—O5 | 122.10 (12) | O5—C13—Er1 | 60.6 (2) |
O5iv—Er1—O5 | 73.65 (13) | C14—C13—Er1 | 167.2 (12) |
O1W—Er1—O5 | 118.73 (13) | C14'—C13—Er1 | 177.2 (13) |
O6—Er1—O5 | 52.98 (11) | C13—C14—H14A | 109.5 |
O4—Er1—C13 | 169.94 (13) | C13—C14—H14B | 109.5 |
O2i—Er1—C13 | 83.95 (14) | C13—C14—H14C | 109.5 |
O1ii—Er1—C13 | 79.88 (14) | C13—C14'—H14D | 109.5 |
O3iii—Er1—C13 | 102.99 (13) | C13—C14'—H14E | 109.5 |
O5iv—Er1—C13 | 100.25 (13) | H14D—C14'—H14E | 109.5 |
O1W—Er1—C13 | 97.55 (14) | C13—C14'—H14F | 109.5 |
O6—Er1—C13 | 26.38 (13) | H14D—C14'—H14F | 109.5 |
O5—Er1—C13 | 26.64 (12) | H14E—C14'—H14F | 109.5 |
O4—Er1—Er1iv | 114.47 (8) | O8—Cl1—O10' | 140.3 (9) |
O2i—Er1—Er1iv | 68.88 (8) | O8—Cl1—O7' | 104.2 (12) |
O1ii—Er1—Er1iv | 70.37 (8) | O10'—Cl1—O7' | 113.8 (8) |
O3iii—Er1—Er1iv | 141.06 (8) | O8—Cl1—O9 | 111.5 (8) |
O5iv—Er1—Er1iv | 37.84 (8) | O10'—Cl1—O9 | 54.6 (7) |
O1W—Er1—Er1iv | 139.44 (9) | O7'—Cl1—O9 | 124.9 (10) |
O6—Er1—Er1iv | 88.78 (8) | O10'—Cl1—O8' | 110.7 (8) |
O5—Er1—Er1iv | 35.81 (8) | O7'—Cl1—O8' | 110.1 (9) |
C13—Er1—Er1iv | 62.42 (10) | O9—Cl1—O8' | 124.5 (9) |
N1—Ag1—N2 | 165.44 (19) | O8—Cl1—O7 | 112.4 (8) |
C5—N1—C4 | 117.6 (5) | O10'—Cl1—O7 | 107.3 (10) |
C5—N1—Ag1 | 126.0 (4) | O9—Cl1—O7 | 107.7 (8) |
C4—N1—Ag1 | 116.3 (4) | O8'—Cl1—O7 | 126.7 (10) |
C12—N2—C7 | 118.2 (4) | O8—Cl1—O10 | 111.8 (8) |
C12—N2—Ag1 | 123.0 (4) | O10'—Cl1—O10 | 53.6 (7) |
C7—N2—Ag1 | 118.8 (4) | O7'—Cl1—O10 | 97.3 (10) |
O2—C1—O1 | 126.7 (4) | O9—Cl1—O10 | 106.3 (7) |
O2—C1—C2 | 116.4 (4) | O8'—Cl1—O10 | 70.3 (8) |
O1—C1—C2 | 116.9 (4) | O7—Cl1—O10 | 106.7 (8) |
C3—C2—C6 | 118.5 (5) | O8—Cl1—O9' | 66.9 (8) |
C3—C2—C1 | 119.4 (5) | O10'—Cl1—O9' | 109.0 (8) |
C6—C2—C1 | 122.2 (5) | O7'—Cl1—O9' | 108.9 (8) |
C2—C3—C4 | 119.5 (5) | O9—Cl1—O9' | 54.5 (7) |
C2—C3—H8 | 120.2 | O8'—Cl1—O9' | 103.8 (8) |
C4—C3—H8 | 120.2 | O7—Cl1—O9' | 97.5 (10) |
N1—C4—C3 | 122.7 (5) | O10—Cl1—O9' | 153.4 (9) |
N1—C4—H7 | 118.6 | O8'—O8—Cl1 | 71.7 (8) |
C3—C4—H7 | 118.6 | O8'—O8—O9' | 123.3 (13) |
N1—C5—C6 | 122.7 (5) | Cl1—O8—O9' | 59.1 (6) |
N1—C5—H11 | 118.6 | O10'—O9—O9' | 126.6 (10) |
C6—C5—H11 | 118.6 | O10'—O9—Cl1 | 62.1 (6) |
C2—C6—C5 | 119.0 (5) | O9'—O9—Cl1 | 64.8 (7) |
C2—C6—H10 | 120.5 | O10'—O10—Cl1 | 60.5 (6) |
C5—C6—H10 | 120.5 | O10'—O10—O8' | 102.8 (9) |
N2—C7—C8 | 122.2 (5) | Cl1—O10—O8' | 53.8 (5) |
N2—C7—H4 | 118.9 | O8—O8'—Cl1 | 66.8 (8) |
C8—C7—H4 | 118.9 | O8—O8'—O10 | 122.7 (11) |
C7—C8—C9 | 119.7 (5) | Cl1—O8'—O10 | 55.9 (6) |
C7—C8—H3 | 120.2 | O9—O9'—Cl1 | 60.7 (5) |
C9—C8—H3 | 120.2 | O9—O9'—O8 | 105.7 (9) |
C11—C9—C8 | 118.2 (4) | Cl1—O9'—O8 | 54.0 (5) |
C11—C9—C10 | 121.7 (4) | O9—O10'—O10 | 126.2 (10) |
C8—C9—C10 | 120.0 (4) | O9—O10'—Cl1 | 63.3 (6) |
O3—C10—O4 | 124.5 (4) | O10—O10'—Cl1 | 65.9 (6) |
O3—C10—C9 | 117.6 (4) |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) x+1, −y+3/2, z−1/2; (iii) x, −y+3/2, z+1/2; (iv) −x+2, −y+2, −z; (v) x−1, −y+3/2, z+1/2; (vi) −x+1, y−1/2, −z+1/2; (vii) x, −y+3/2, z−1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H2W···O4iii | 0.82 (4) | 2.19 (3) | 2.891 (5) | 145 (5) |
O1W—H1W···O6vii | 0.81 (4) | 1.99 (4) | 2.786 (5) | 167 (6) |
Symmetry codes: (iii) x, −y+3/2, z+1/2; (vii) x, −y+3/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [AgEr(C6H4NO2)2(C2H3O2)(H2O)]ClO4 |
Mr | 695.84 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 296 |
a, b, c (Å) | 16.1952 (11), 14.8673 (11), 7.8938 (6) |
β (°) | 91.783 (1) |
V (Å3) | 1899.7 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 5.62 |
Crystal size (mm) | 0.23 × 0.20 × 0.19 |
Data collection | |
Diffractometer | Bruker APEXII area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.285, 0.344 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 9611, 3423, 3009 |
Rint | 0.030 |
(sin θ/λ)max (Å−1) | 0.599 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.025, 0.057, 1.05 |
No. of reflections | 3423 |
No. of parameters | 320 |
No. of restraints | 158 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.76, −1.04 |
Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H2W···O4i | 0.82 (4) | 2.19 (3) | 2.891 (5) | 145 (5) |
O1W—H1W···O6ii | 0.81 (4) | 1.99 (4) | 2.786 (5) | 167 (6) |
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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This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
In the past few years, lanthanide-transition metal heterometallic complexes with bridging multifunctional organic ligands gained increasing interest, not only because of their crystal structures, but also due to their applications in ion exchange, magnetism, catalysis and as luminescent material (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 and is presented in this article.
In the title compound (Fig. 1), there are one ErIII ion, one AgI ion, two halves of an acetate ligand, two isonicotinate ligands, one coordinated water molecule, and one perchlorate anion in the asymmetric unit. Each ErIII ion is eight-coordinated by four O atoms from four different isonicotinate ligands [Er—O distances ranging from 2.266 (3) to 2.308 (3) Å], three O atoms from two different acetate ligands [Er—O distances ranging from 2.341 (3) to 2.454 (3) Å], and one O atom of water molecule [Er—O distance 2.369 (3) Å]. The Er center can be described as having a distorted bicapped trigonal-prismatic coordination geometry. The two-coordinated AgI ion is bonded to two N atoms from two different isonicotinate anions [Ag—N distances 2.153 (4) and 2.154 (4) Å] and adopts a slight distortion from linearity with an N1—Ag1—N2 angle of 165.44 (19) °. These metal coordination units are connected by bridging isonicotinate and acetate ligands, generating a three-dimensional network (Fig. 2). The coordinated water molecules exhibit O—H···O hydrogen bonding to the uncoordinated O atom of a carboxylate group and to the acetate ligand (Table 1).