Literature DB >> 21578641

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

Li-Cai Zhu1.   

Abstract

In the title three-dimensional heterometallic complex, {[AgEr(C(6)H(4)NO(2))(2)(C(2)H(3)O(2))(H(2)O)]ClO(4)}(n), the eight-coordin-ate Er(III) 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 mol-ecule. The two-coordinate Ag(I) 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 mol-ecule and a carboxyl-ate 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.

Entities:  

Year:  2009        PMID: 21578641      PMCID: PMC2971902          DOI: 10.1107/S1600536809048429

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


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

[AgEr(C6H4NO2)2(C2H3O2)(H2O)]ClO4 M = 695.84 Monoclinic, a = 16.1952 (11) Å b = 14.8673 (11) Å c = 7.8938 (6) Å β = 91.783 (1)° V = 1899.7 (2) Å3 Z = 4 Mo Kα radiation μ = 5.62 mm−1 T = 296 K 0.23 × 0.20 × 0.19 mm

Data collection

Bruker APEXII area-detector diffractometer Absorption correction: multi-scan (; Sheldrick, 1996 ▶) T min = 0.285, T max = 0.344 9611 measured reflections 3423 independent reflections 3009 reflections with I > 2σ(I) R int = 0.030

Refinement

R[F 2 > 2σ(F 2)] = 0.025 wR(F 2) = 0.057 S = 1.05 3423 reflections 320 parameters 158 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.76 e Å−3 Δρmin = −1.04 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/S1600536809048429/wm2280sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809048429/wm2280Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[AgEr(C6H4NO2)2(C2H3O2)(H2O)]ClO4F(000) = 1324
Mr = 695.84Dx = 2.433 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4797 reflections
a = 16.1952 (11) Åθ = 2.5–27.9°
b = 14.8673 (11) ŵ = 5.62 mm1
c = 7.8938 (6) ÅT = 296 K
β = 91.783 (1)°Block, colourless
V = 1899.7 (2) Å30.23 × 0.20 × 0.19 mm
Z = 4
Bruker APEXII area-detector diffractometer3423 independent reflections
Radiation source: fine-focus sealed tube3009 reflections with I > 2σ(I)
graphiteRint = 0.030
φ and ω scanθmax = 25.2°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −19→19
Tmin = 0.285, Tmax = 0.344k = −17→17
9611 measured reflectionsl = −5→9
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.057H atoms treated by a mixture of independent and constrained refinement
S = 1.05w = 1/[σ2(Fo2) + (0.0218P)2 + 3.7155P] where P = (Fo2 + 2Fc2)/3
3423 reflections(Δ/σ)max = 0.002
320 parametersΔρmax = 0.76 e Å3
158 restraintsΔρmin = −1.04 e Å3
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.
xyzUiso*/UeqOcc. (<1)
Er10.955305 (12)0.883792 (13)0.05025 (3)0.01689 (8)
Ag10.47352 (3)0.74056 (4)0.10055 (8)0.06366 (18)
N10.3573 (3)0.6969 (3)0.1973 (7)0.0464 (13)
N20.5953 (3)0.7481 (3)−0.0007 (6)0.0378 (11)
C10.1321 (3)0.5802 (3)0.3629 (7)0.0287 (12)
C20.2108 (3)0.6229 (3)0.3048 (7)0.0273 (11)
C30.2810 (3)0.5718 (4)0.2968 (8)0.0427 (15)
H80.28000.51140.32710.051*
C40.3527 (4)0.6105 (4)0.2436 (9)0.0523 (18)
H70.40000.57530.23970.063*
C50.2890 (3)0.7466 (4)0.2066 (9)0.0455 (16)
H110.29140.80700.17670.055*
C60.2147 (3)0.7121 (4)0.2589 (8)0.0378 (14)
H100.16810.74850.26300.045*
C70.6342 (3)0.6716 (4)−0.0395 (8)0.0438 (15)
H40.60760.6171−0.02210.053*
C80.7122 (3)0.6709 (4)−0.1041 (7)0.0340 (13)
H30.73720.6167−0.13150.041*
C90.7531 (3)0.7512 (3)−0.1281 (6)0.0199 (10)
C100.8387 (3)0.7511 (3)−0.1972 (6)0.0203 (10)
C110.7136 (3)0.8299 (3)−0.0871 (7)0.0309 (12)
H60.73940.8851−0.10180.037*
C120.6349 (3)0.8258 (4)−0.0237 (7)0.0359 (13)
H50.60850.87920.00400.043*
O10.0753 (2)0.6328 (2)0.4074 (5)0.0354 (9)
O20.1298 (2)0.4963 (2)0.3618 (5)0.0369 (9)
O30.85978 (19)0.6842 (2)−0.2806 (4)0.0276 (8)
O40.88366 (18)0.8187 (2)−0.1684 (4)0.0237 (7)
O1W0.9992 (2)0.7323 (2)0.0767 (5)0.0327 (9)
H1W1.017 (3)0.702 (3)0.001 (5)0.049*
H2W0.978 (3)0.697 (3)0.142 (5)0.049*
O61.0346 (2)0.8847 (2)0.3130 (4)0.0324 (8)
O51.0476 (2)1.0034 (2)0.1567 (4)0.0289 (8)
C131.0687 (3)0.9591 (3)0.2875 (6)0.0266 (11)
C141.1431 (13)0.9863 (19)0.395 (3)0.040 (4)0.51 (5)
H14A1.17281.03270.33850.059*0.51 (5)
H14B1.17850.93510.41290.059*0.51 (5)
H14C1.12551.00820.50240.059*0.51 (5)
C14'1.1264 (15)1.0028 (19)0.417 (3)0.040 (4)0.49 (5)
H14D1.11421.06590.42300.059*0.49 (5)
H14E1.18240.99470.38360.059*0.49 (5)
H14F1.11910.97560.52550.059*0.49 (5)
Cl10.58069 (12)0.04095 (12)0.7436 (3)0.0642 (5)0.526 (13)
O70.5433 (10)−0.0457 (8)0.742 (2)0.076 (5)0.526 (13)
O80.5249 (9)0.1082 (9)0.709 (2)0.133 (6)0.526 (13)
O90.6203 (10)0.0528 (9)0.9021 (14)0.109 (6)0.526 (13)
O100.6454 (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)
U11U22U33U12U13U23
Er10.01467 (12)0.01458 (12)0.02167 (13)−0.00074 (8)0.00453 (8)0.00002 (8)
Ag10.0248 (2)0.0863 (4)0.0813 (4)−0.0136 (2)0.0248 (3)0.0023 (3)
N10.025 (2)0.047 (3)0.067 (4)−0.007 (2)0.017 (2)0.000 (3)
N20.021 (2)0.045 (3)0.048 (3)−0.003 (2)0.013 (2)0.000 (2)
C10.028 (3)0.020 (3)0.039 (3)−0.005 (2)0.012 (2)−0.003 (2)
C20.024 (3)0.028 (3)0.031 (3)−0.005 (2)0.009 (2)−0.003 (2)
C30.025 (3)0.029 (3)0.075 (5)0.002 (2)0.015 (3)0.001 (3)
C40.026 (3)0.048 (4)0.084 (5)0.004 (3)0.017 (3)0.000 (3)
C50.031 (3)0.036 (3)0.071 (5)−0.009 (3)0.016 (3)0.009 (3)
C60.027 (3)0.030 (3)0.058 (4)−0.001 (2)0.015 (3)0.005 (3)
C70.035 (3)0.036 (3)0.061 (4)−0.016 (3)0.012 (3)0.002 (3)
C80.029 (3)0.026 (3)0.048 (4)−0.003 (2)0.012 (3)−0.001 (2)
C90.016 (2)0.023 (3)0.020 (3)−0.0031 (19)0.0016 (19)−0.0025 (19)
C100.018 (2)0.023 (3)0.021 (3)0.0015 (19)0.0023 (19)0.002 (2)
C110.021 (2)0.026 (3)0.046 (3)−0.004 (2)0.010 (2)−0.001 (2)
C120.026 (3)0.035 (3)0.047 (4)0.007 (2)0.012 (3)0.002 (3)
O10.0258 (19)0.0208 (19)0.061 (3)−0.0007 (15)0.0249 (19)0.0012 (16)
O20.0296 (19)0.0196 (19)0.063 (3)−0.0016 (15)0.0227 (18)−0.0038 (17)
O30.0246 (17)0.0214 (18)0.037 (2)−0.0021 (14)0.0110 (16)−0.0082 (15)
O40.0179 (16)0.0250 (18)0.0283 (19)−0.0051 (14)0.0042 (14)−0.0058 (14)
O1W0.045 (2)0.0204 (18)0.034 (2)0.0068 (16)0.0164 (18)0.0022 (15)
O60.039 (2)0.033 (2)0.025 (2)−0.0065 (16)−0.0043 (16)0.0089 (15)
O50.0335 (19)0.0248 (18)0.028 (2)−0.0076 (15)−0.0089 (16)0.0043 (15)
C130.030 (3)0.023 (3)0.027 (3)−0.001 (2)−0.001 (2)0.000 (2)
C140.038 (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)
Cl10.0638 (11)0.0528 (10)0.0756 (13)0.0017 (9)−0.0046 (10)−0.0013 (9)
O70.071 (8)0.070 (8)0.089 (9)−0.025 (6)0.001 (6)−0.009 (6)
O80.140 (10)0.104 (9)0.153 (11)0.074 (7)−0.032 (8)−0.019 (7)
O90.134 (10)0.110 (8)0.081 (8)−0.042 (7)−0.036 (7)0.001 (6)
O100.133 (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—O42.266 (3)C11—C121.386 (7)
Er1—O2i2.289 (3)C11—H60.9300
Er1—O1ii2.290 (3)C12—H50.9300
Er1—O3iii2.308 (3)O1—Er1v2.290 (3)
Er1—O5iv2.341 (3)O2—Er1vi2.289 (3)
Er1—O1W2.369 (3)O3—Er1vii2.308 (3)
Er1—O62.405 (3)O1W—H1W0.81 (4)
Er1—O52.454 (3)O1W—H2W0.82 (4)
Ag1—N12.153 (4)O6—C131.256 (6)
Ag1—N22.154 (4)O5—C131.263 (6)
N1—C51.336 (7)O5—Er1iv2.341 (3)
N1—C41.337 (8)C13—C141.507 (9)
N2—C121.335 (7)C13—C14'1.507 (10)
N2—C71.341 (7)C14—H14A0.9600
C1—O21.248 (6)C14—H14B0.9600
C1—O11.266 (6)C14—H14C0.9600
C1—C21.507 (6)C14'—H14D0.9600
C2—C31.370 (7)C14'—H14E0.9600
C2—C61.376 (7)C14'—H14F0.9600
C3—C41.374 (8)Cl1—O81.368 (9)
C3—H80.9300Cl1—O10'1.384 (8)
C4—H70.9300Cl1—O7'1.390 (9)
C5—C61.382 (7)Cl1—O91.399 (9)
C5—H110.9300Cl1—O8'1.414 (10)
C6—H100.9300Cl1—O71.423 (9)
C7—C81.376 (7)Cl1—O101.451 (9)
C7—H40.9300Cl1—O9'1.452 (10)
C8—C91.381 (7)O8—O8'0.988 (19)
C8—H30.9300O8—O9'1.557 (19)
C9—C111.378 (7)O9—O10'1.278 (15)
C9—C101.505 (6)O9—O9'1.307 (17)
C10—O31.246 (5)O10—O10'1.280 (17)
C10—O41.258 (5)O10—O8'1.650 (18)
O4—Er1—O2i104.11 (13)O4—C10—C9117.9 (4)
O4—Er1—O1ii90.06 (13)C9—C11—C12119.1 (5)
O2i—Er1—O1ii139.15 (12)C9—C11—H6120.4
O4—Er1—O3iii85.24 (12)C12—C11—H6120.4
O2i—Er1—O3iii73.96 (11)N2—C12—C11122.5 (5)
O1ii—Er1—O3iii146.30 (12)N2—C12—H5118.7
O4—Er1—O5iv77.04 (11)C11—C12—H5118.7
O2i—Er1—O5iv71.89 (13)C1—O1—Er1v134.9 (3)
O1ii—Er1—O5iv74.47 (12)C1—O2—Er1vi138.3 (3)
O3iii—Er1—O5iv135.93 (12)C10—O3—Er1vii148.8 (3)
O4—Er1—O1W78.85 (13)C10—O4—Er1139.3 (3)
O2i—Er1—O1W148.19 (12)Er1—O1W—H1W125 (4)
O1ii—Er1—O1W71.58 (12)Er1—O1W—H2W122 (4)
O3iii—Er1—O1W74.77 (12)H1W—O1W—H2W106 (4)
O5iv—Er1—O1W137.91 (12)C13—O6—Er195.3 (3)
O4—Er1—O6154.95 (12)C13—O5—Er1iv160.6 (3)
O2i—Er1—O692.59 (14)C13—O5—Er192.8 (3)
O1ii—Er1—O689.25 (14)Er1iv—O5—Er1106.35 (13)
O3iii—Er1—O681.55 (12)O6—C13—O5118.7 (4)
O5iv—Er1—O6126.62 (11)O6—C13—C14119.6 (11)
O1W—Er1—O677.18 (13)O5—C13—C14120.8 (11)
O4—Er1—O5149.53 (11)O6—C13—C14'122.6 (12)
O2i—Er1—O574.51 (12)O5—C13—C14'118.3 (12)
O1ii—Er1—O574.32 (12)O6—C13—Er158.3 (2)
O3iii—Er1—O5122.10 (12)O5—C13—Er160.6 (2)
O5iv—Er1—O573.65 (13)C14—C13—Er1167.2 (12)
O1W—Er1—O5118.73 (13)C14'—C13—Er1177.2 (13)
O6—Er1—O552.98 (11)C13—C14—H14A109.5
O4—Er1—C13169.94 (13)C13—C14—H14B109.5
O2i—Er1—C1383.95 (14)C13—C14—H14C109.5
O1ii—Er1—C1379.88 (14)C13—C14'—H14D109.5
O3iii—Er1—C13102.99 (13)C13—C14'—H14E109.5
O5iv—Er1—C13100.25 (13)H14D—C14'—H14E109.5
O1W—Er1—C1397.55 (14)C13—C14'—H14F109.5
O6—Er1—C1326.38 (13)H14D—C14'—H14F109.5
O5—Er1—C1326.64 (12)H14E—C14'—H14F109.5
O4—Er1—Er1iv114.47 (8)O8—Cl1—O10'140.3 (9)
O2i—Er1—Er1iv68.88 (8)O8—Cl1—O7'104.2 (12)
O1ii—Er1—Er1iv70.37 (8)O10'—Cl1—O7'113.8 (8)
O3iii—Er1—Er1iv141.06 (8)O8—Cl1—O9111.5 (8)
O5iv—Er1—Er1iv37.84 (8)O10'—Cl1—O954.6 (7)
O1W—Er1—Er1iv139.44 (9)O7'—Cl1—O9124.9 (10)
O6—Er1—Er1iv88.78 (8)O10'—Cl1—O8'110.7 (8)
O5—Er1—Er1iv35.81 (8)O7'—Cl1—O8'110.1 (9)
C13—Er1—Er1iv62.42 (10)O9—Cl1—O8'124.5 (9)
N1—Ag1—N2165.44 (19)O8—Cl1—O7112.4 (8)
C5—N1—C4117.6 (5)O10'—Cl1—O7107.3 (10)
C5—N1—Ag1126.0 (4)O9—Cl1—O7107.7 (8)
C4—N1—Ag1116.3 (4)O8'—Cl1—O7126.7 (10)
C12—N2—C7118.2 (4)O8—Cl1—O10111.8 (8)
C12—N2—Ag1123.0 (4)O10'—Cl1—O1053.6 (7)
C7—N2—Ag1118.8 (4)O7'—Cl1—O1097.3 (10)
O2—C1—O1126.7 (4)O9—Cl1—O10106.3 (7)
O2—C1—C2116.4 (4)O8'—Cl1—O1070.3 (8)
O1—C1—C2116.9 (4)O7—Cl1—O10106.7 (8)
C3—C2—C6118.5 (5)O8—Cl1—O9'66.9 (8)
C3—C2—C1119.4 (5)O10'—Cl1—O9'109.0 (8)
C6—C2—C1122.2 (5)O7'—Cl1—O9'108.9 (8)
C2—C3—C4119.5 (5)O9—Cl1—O9'54.5 (7)
C2—C3—H8120.2O8'—Cl1—O9'103.8 (8)
C4—C3—H8120.2O7—Cl1—O9'97.5 (10)
N1—C4—C3122.7 (5)O10—Cl1—O9'153.4 (9)
N1—C4—H7118.6O8'—O8—Cl171.7 (8)
C3—C4—H7118.6O8'—O8—O9'123.3 (13)
N1—C5—C6122.7 (5)Cl1—O8—O9'59.1 (6)
N1—C5—H11118.6O10'—O9—O9'126.6 (10)
C6—C5—H11118.6O10'—O9—Cl162.1 (6)
C2—C6—C5119.0 (5)O9'—O9—Cl164.8 (7)
C2—C6—H10120.5O10'—O10—Cl160.5 (6)
C5—C6—H10120.5O10'—O10—O8'102.8 (9)
N2—C7—C8122.2 (5)Cl1—O10—O8'53.8 (5)
N2—C7—H4118.9O8—O8'—Cl166.8 (8)
C8—C7—H4118.9O8—O8'—O10122.7 (11)
C7—C8—C9119.7 (5)Cl1—O8'—O1055.9 (6)
C7—C8—H3120.2O9—O9'—Cl160.7 (5)
C9—C8—H3120.2O9—O9'—O8105.7 (9)
C11—C9—C8118.2 (4)Cl1—O9'—O854.0 (5)
C11—C9—C10121.7 (4)O9—O10'—O10126.2 (10)
C8—C9—C10120.0 (4)O9—O10'—Cl163.3 (6)
O3—C10—O4124.5 (4)O10—O10'—Cl165.9 (6)
O3—C10—C9117.6 (4)
D—H···AD—HH···AD···AD—H···A
O1W—H2W···O4iii0.82 (4)2.19 (3)2.891 (5)145 (5)
O1W—H1W···O6vii0.81 (4)1.99 (4)2.786 (5)167 (6)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A DA 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) ; (ii) .

  3 in total

1.  Lanthanide-transition-metal sandwich framework comprising {Cu3} cluster pillars and layered networks of {Er36} wheels.

Authors:  Jian-Wen Cheng; Jie Zhang; Shou-Tian Zheng; Man-Bo Zhang; Guo-Yu Yang
Journal:  Angew Chem Int Ed Engl       Date:  2005-12-16       Impact factor: 15.336

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

3.  Poly[[di-μ(3)-nicotinato-μ(3)-oxalato-samarium(III)silver(I)] dihydrate].

Authors:  Li-Cai Zhu; Zhen-Gang Zhao; Shu-Juan Yu
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-08-19
  3 in total

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