Literature DB >> 21200648

{μ-6,6'-Dimeth-oxy-2,2'-[ethane-1,2-diylbis(nitrilo-methyl-idyne)]diphenolato}-μ-nitrato-dinitratoeuropium(III)zinc(II).

Rong-Hua Hu, Yan Sui, Li Chen, Chun-Mei He.   

Abstract

In the title heteronuclear Zn(II)-Eu(III) complex [systematic name: {6,6'-dimeth-oxy-2,2'-[ethane-1,2-diylbis(nitrilo-methyl-idyne)]diphenolato-κ(4)O(1),O(1'),O(6),O(6'):2κ(4)O(1),N,N',O(1')}-μ-nitrato-1:2κ(2)O:O'-dini-trato-1κ(4)O,O'-europium(III)zinc(II)], [EuZn(C(18)H(18)N(2)O(4))(NO(3))(3)], with the hexa-dentate Schiff base compartmental ligand N,N'-bis-(3-methoxy-salicyl-idene)ethyl-enediamine (H(2)L), the Eu and Zn atoms are triply bridged by two phenolate O atoms of the Schiff base ligand and one nitrate ion. The five-coordinate Zn atom is in a square-pyramidal geometry with the donor centers of two imine N atoms, two phenolate O atoms and one of the bridging nitrate O atoms. The Eu(III) center has a ninefold coordination environment of O atoms, involving the phenol-ate O atoms, two meth-oxy O atoms, two O atoms from two nitrate ions and one from the bridging nitrate ion. Weak inter-molecular C-H⋯O inter-actions generate a two-dimensional double-layer structure.

Entities:  

Year:  2007        PMID: 21200648      PMCID: PMC2914891          DOI: 10.1107/S160053680706151X

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


Related literature

For related literature, see: Baggio et al. (2000 ▶); Caravan et al. (1999 ▶); Edder et al. (2000 ▶); Knoer et al. (2005 ▶); Sui et al. (2006 ▶, 2007 ▶).

Experimental

Crystal data

[EuZn(C18H18N2O4)(NO3)3] M = 729.70 Monoclinic, a = 10.6576 (13) Å b = 16.460 (2) Å c = 14.8760 (18) Å β = 99.253 (2)° V = 2575.7 (5) Å3 Z = 4 Mo Kα radiation μ = 3.42 mm−1 T = 293 (2) K 0.22 × 0.21 × 0.13 mm

Data collection

Bruker APEXII area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2004 ▶) T min = 0.520, T max = 0.665 19080 measured reflections 6166 independent reflections 4469 reflections with I > 2σ(I) R int = 0.029

Refinement

R[F 2 > 2σ(F 2)] = 0.041 wR(F 2) = 0.137 S = 1.00 6166 reflections 346 parameters 1 restraint H-atom parameters constrained Δρmax = 1.01 e Å−3 Δρmin = −1.34 e Å−3 Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: APEX2; software used to prepare material for publication: APEX2 and publCIF (Westrip, 2007 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680706151X/at2500sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S160053680706151X/at2500Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[EuZn(C18H18N2O4)(NO3)3]F000 = 1432
Mr = 729.70Dx = 1.882 Mg m3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 7701 reflections
a = 10.6576 (13) Åθ = 1.9–28.2º
b = 16.460 (2) ŵ = 3.42 mm1
c = 14.8760 (18) ÅT = 293 (2) K
β = 99.253 (2)ºBlock, yellow
V = 2575.7 (5) Å30.22 × 0.21 × 0.13 mm
Z = 4
Bruker APEXII area-detector diffractometer6166 independent reflections
Radiation source: fine-focus sealed tube4469 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.029
T = 293(2) Kθmax = 28.2º
φ and ω scanθmin = 1.9º
Absorption correction: multi-scan(SADABS; Bruker, 2004)h = −14→13
Tmin = 0.520, Tmax = 0.665k = −21→21
19080 measured reflectionsl = −19→19
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.041H-atom parameters constrained
wR(F2) = 0.137  w = 1/[σ2(Fo2) + (0.095P)2] where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
6166 reflectionsΔρmax = 1.01 e Å3
346 parametersΔρmin = −1.34 e Å3
1 restraintExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0023 (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.
xyzUiso*/Ueq
Eu10.63900 (2)0.108878 (15)0.274156 (15)0.04120 (12)
Zn10.78031 (6)0.03491 (4)0.11111 (4)0.05380 (19)
N10.7500 (5)−0.0694 (3)0.0378 (3)0.0606 (12)
O120.4368 (5)0.1271 (3)0.1789 (3)0.0741 (13)
O10.6479 (4)−0.0006 (2)0.1867 (3)0.0622 (10)
O30.5081 (4)−0.0172 (3)0.3054 (3)0.0632 (11)
O90.7155 (4)0.1980 (3)0.3991 (3)0.0705 (12)
O80.6712 (5)0.0748 (3)0.4353 (3)0.0741 (13)
N40.7205 (6)0.1408 (4)0.4622 (4)0.0751 (16)
C10.5860 (5)−0.0710 (3)0.1821 (4)0.0532 (13)
C40.4554 (7)−0.2156 (5)0.1893 (6)0.088 (2)
H40.4132−0.26470.19270.105*
C20.5091 (6)−0.0829 (4)0.2476 (4)0.0569 (13)
N30.3827 (5)0.1566 (4)0.2423 (4)0.0778 (17)
C60.5955 (6)−0.1324 (4)0.1176 (5)0.0616 (15)
C180.4310 (7)−0.0261 (5)0.3785 (4)0.079 (2)
H18A0.3462−0.04200.35270.118*
H18B0.42840.02480.40970.118*
H18C0.4681−0.06680.42080.118*
O100.7682 (7)0.1548 (4)0.5388 (3)0.128 (3)
C30.4432 (6)−0.1548 (4)0.2542 (5)0.0734 (18)
H30.3932−0.16260.29930.088*
C70.6722 (6)−0.1262 (4)0.0438 (4)0.0611 (15)
H70.6627−0.1663−0.00080.073*
O110.4523 (4)0.1616 (3)0.3198 (3)0.0737 (13)
C50.5259 (7)−0.2051 (4)0.1224 (5)0.0748 (18)
H50.5289−0.24590.07950.090*
O60.9413 (4)0.0296 (3)0.1972 (3)0.0668 (11)
O40.6363 (4)0.2606 (3)0.2286 (3)0.0646 (11)
O20.7090 (4)0.1414 (2)0.1447 (3)0.0608 (10)
O50.8463 (4)0.0763 (4)0.3096 (3)0.0778 (13)
N20.8025 (5)0.0827 (4)−0.0125 (3)0.0618 (12)
N50.9391 (6)0.0506 (4)0.2778 (4)0.0844 (17)
C80.8228 (6)−0.0642 (5)−0.0385 (4)0.0700 (17)
H8A0.7942−0.1060−0.08310.084*
H8B0.9124−0.0728−0.01630.084*
C150.6903 (6)0.2813 (4)0.1541 (4)0.0577 (14)
C160.7293 (5)0.2124 (4)0.1086 (4)0.0535 (13)
C100.8045 (6)0.1575 (4)−0.0319 (4)0.0660 (16)
H100.82430.1710−0.08870.079*
O130.2748 (6)0.1790 (6)0.2304 (5)0.141 (3)
C110.7783 (6)0.2248 (4)0.0271 (4)0.0625 (15)
C90.8027 (7)0.0198 (5)−0.0826 (4)0.0754 (19)
H9A0.87000.0308−0.11770.090*
H9B0.72230.0208−0.12390.090*
C170.5747 (8)0.3264 (4)0.2710 (5)0.083 (2)
H17A0.63290.37100.28410.125*
H17B0.54990.30730.32650.125*
H17C0.50070.34430.23010.125*
C140.7069 (7)0.3593 (4)0.1239 (4)0.0667 (16)
H140.68400.40430.15550.080*
C120.7926 (7)0.3043 (4)−0.0030 (4)0.0739 (19)
H120.82540.3128−0.05650.089*
C130.7599 (8)0.3683 (5)0.0435 (5)0.079 (2)
H130.77240.42030.02210.095*
O71.0692 (8)0.0412 (5)0.3486 (5)0.156 (3)
U11U22U33U12U13U23
Eu10.04652 (18)0.04350 (18)0.03697 (16)−0.00126 (10)0.01698 (11)−0.00322 (9)
Zn10.0580 (4)0.0561 (4)0.0510 (4)0.0004 (3)0.0200 (3)−0.0042 (3)
N10.061 (3)0.067 (3)0.057 (3)−0.003 (3)0.018 (2)−0.017 (2)
O120.065 (3)0.099 (4)0.061 (3)0.004 (2)0.017 (2)−0.013 (2)
O10.073 (3)0.055 (2)0.066 (2)−0.014 (2)0.033 (2)−0.0140 (19)
O30.071 (3)0.066 (3)0.059 (2)−0.010 (2)0.029 (2)−0.001 (2)
O90.088 (3)0.063 (3)0.062 (3)−0.012 (2)0.018 (2)−0.002 (2)
O80.100 (4)0.070 (3)0.055 (2)−0.023 (3)0.021 (2)−0.002 (2)
N40.098 (4)0.083 (4)0.048 (3)−0.029 (4)0.026 (3)−0.009 (3)
C10.052 (3)0.046 (3)0.063 (3)0.000 (2)0.013 (3)0.000 (3)
C40.076 (5)0.068 (5)0.125 (7)−0.027 (4)0.034 (5)−0.017 (4)
C20.055 (3)0.055 (3)0.061 (3)−0.001 (3)0.009 (3)−0.001 (3)
N30.058 (3)0.104 (5)0.075 (4)0.007 (3)0.022 (3)−0.022 (3)
C60.061 (4)0.053 (3)0.072 (4)0.005 (3)0.013 (3)−0.005 (3)
C180.088 (5)0.092 (5)0.067 (4)−0.013 (4)0.043 (4)0.004 (3)
O100.178 (7)0.145 (6)0.054 (3)−0.071 (5)−0.007 (4)0.002 (3)
C30.062 (4)0.072 (5)0.090 (5)−0.010 (3)0.024 (4)0.008 (4)
C70.061 (4)0.062 (4)0.060 (4)0.004 (3)0.010 (3)−0.015 (3)
O110.073 (3)0.097 (4)0.055 (2)0.000 (2)0.022 (2)−0.020 (2)
C50.075 (4)0.054 (4)0.098 (5)−0.009 (3)0.019 (4)−0.018 (3)
O60.060 (2)0.074 (3)0.067 (2)0.002 (2)0.010 (2)−0.005 (2)
O40.088 (3)0.054 (2)0.058 (2)0.008 (2)0.029 (2)0.0014 (18)
O20.079 (3)0.050 (2)0.060 (2)0.008 (2)0.034 (2)0.0059 (18)
O50.058 (3)0.116 (4)0.061 (3)0.007 (3)0.012 (2)−0.015 (3)
N20.061 (3)0.076 (4)0.053 (3)0.002 (3)0.019 (2)0.003 (2)
N50.082 (4)0.091 (5)0.081 (3)−0.001 (3)0.014 (3)−0.018 (3)
C80.065 (4)0.087 (5)0.064 (4)0.002 (3)0.028 (3)−0.017 (3)
C150.064 (3)0.050 (3)0.060 (3)−0.003 (3)0.012 (3)0.003 (3)
C160.057 (3)0.053 (3)0.053 (3)−0.003 (3)0.013 (2)0.006 (2)
C100.067 (4)0.077 (5)0.059 (3)−0.002 (3)0.027 (3)0.011 (3)
O130.070 (4)0.221 (9)0.131 (5)0.045 (4)0.010 (4)−0.060 (5)
C110.062 (4)0.064 (4)0.065 (4)−0.007 (3)0.019 (3)0.001 (3)
C90.076 (4)0.100 (5)0.053 (3)0.013 (4)0.018 (3)−0.009 (3)
C170.108 (6)0.059 (4)0.088 (5)0.013 (4)0.030 (4)−0.009 (3)
C140.080 (4)0.047 (3)0.072 (4)−0.001 (3)0.008 (3)0.008 (3)
C120.089 (5)0.075 (5)0.061 (4)−0.012 (4)0.022 (3)0.019 (3)
C130.102 (6)0.067 (4)0.065 (4)−0.007 (4)0.006 (4)0.019 (3)
O70.124 (6)0.179 (9)0.149 (6)0.008 (5)−0.029 (5)−0.024 (5)
Eu1—O12.234 (4)C18—H18A0.9600
Eu1—O22.239 (4)C18—H18B0.9600
Eu1—O32.584 (4)C18—H18C0.9600
Eu1—O42.587 (4)C3—H30.9300
Eu1—O52.252 (5)C7—H70.9300
Eu1—O82.432 (4)C5—H50.9300
Eu1—O92.405 (4)O6—N51.251 (7)
Eu1—O112.368 (4)O4—C151.371 (7)
Eu1—O122.400 (5)O4—C171.462 (7)
Zn1—O12.027 (4)O2—C161.319 (7)
Zn1—O22.005 (4)O5—N51.238 (7)
Zn1—O61.971 (4)N2—C101.265 (9)
Zn1—N12.032 (5)N2—C91.471 (8)
Zn1—N22.048 (5)N5—O71.607 (9)
N1—C71.262 (8)C8—C91.531 (10)
N1—C81.477 (7)C8—H8A0.9700
O12—N31.278 (6)C8—H8B0.9700
O1—C11.329 (7)C15—C141.381 (8)
O3—C21.383 (7)C15—C161.417 (8)
O3—C181.472 (6)C16—C111.409 (8)
O9—N41.324 (7)C10—C111.468 (9)
O8—N41.245 (7)C10—H100.9300
N4—O101.194 (7)C11—C121.399 (9)
C1—C21.385 (8)C9—H9A0.9700
C1—C61.408 (8)C9—H9B0.9700
C4—C51.351 (10)C17—H17A0.9600
C4—C31.410 (10)C17—H17B0.9600
C4—H40.9300C17—H17C0.9600
C2—C31.388 (9)C14—C131.411 (10)
N3—O131.194 (7)C14—H140.9300
N3—O111.269 (7)C12—C131.336 (10)
C6—C51.416 (9)C12—H120.9300
C6—C71.475 (9)C13—H130.9300
O1—Eu1—O268.93 (14)C1—C6—C5118.5 (6)
O1—Eu1—O579.18 (17)C1—C6—C7124.5 (6)
O2—Eu1—O578.96 (16)C5—C6—C7117.0 (6)
O1—Eu1—O11125.39 (15)O3—C18—H18A109.5
O2—Eu1—O11124.77 (16)O3—C18—H18B109.5
O5—Eu1—O11149.10 (15)H18A—C18—H18B109.5
O1—Eu1—O1282.82 (16)O3—C18—H18C109.5
O2—Eu1—O1281.57 (16)H18A—C18—H18C109.5
O5—Eu1—O12157.19 (16)H18B—C18—H18C109.5
O11—Eu1—O1253.67 (15)C2—C3—C4117.0 (6)
O1—Eu1—O9154.35 (16)C2—C3—H3121.5
O2—Eu1—O9113.64 (16)C4—C3—H3121.5
O5—Eu1—O976.50 (17)N1—C7—C6123.6 (5)
O11—Eu1—O975.57 (15)N1—C7—H7118.2
O12—Eu1—O9122.73 (16)C6—C7—H7118.2
O1—Eu1—O8112.04 (16)N3—O11—Eu196.3 (3)
O2—Eu1—O8152.78 (17)C4—C5—C6120.2 (6)
O5—Eu1—O874.72 (17)C4—C5—H5119.9
O11—Eu1—O878.12 (17)C6—C5—H5119.9
O12—Eu1—O8125.60 (17)N5—O6—Zn1117.6 (4)
O9—Eu1—O853.30 (15)C15—O4—C17116.1 (5)
O1—Eu1—O362.07 (13)C15—O4—Eu1117.6 (3)
O2—Eu1—O3127.64 (14)C17—O4—Eu1126.1 (4)
O5—Eu1—O3107.70 (18)C16—O2—Zn1125.4 (3)
O11—Eu1—O374.94 (15)C16—O2—Eu1131.4 (4)
O12—Eu1—O375.38 (16)Zn1—O2—Eu1101.39 (17)
O9—Eu1—O3118.44 (13)N5—O5—Eu1143.8 (4)
O8—Eu1—O368.39 (14)C10—N2—C9121.4 (5)
O1—Eu1—O4128.75 (13)C10—N2—Zn1126.0 (4)
O2—Eu1—O462.29 (14)C9—N2—Zn1112.3 (4)
O5—Eu1—O4105.10 (18)O5—N5—O6126.8 (6)
O11—Eu1—O475.33 (16)O5—N5—O7116.2 (6)
O12—Eu1—O475.71 (16)O6—N5—O7117.0 (6)
O9—Eu1—O466.55 (14)N1—C8—C9109.1 (5)
O8—Eu1—O4118.38 (15)N1—C8—H8A109.9
O3—Eu1—O4147.03 (14)C9—C8—H8A109.9
O6—Zn1—O2101.66 (18)N1—C8—H8B109.9
O6—Zn1—O1103.73 (18)C9—C8—H8B109.9
O2—Zn1—O177.77 (16)H8A—C8—H8B108.3
O6—Zn1—N1111.0 (2)O4—C15—C14125.9 (6)
O2—Zn1—N1147.0 (2)O4—C15—C16112.4 (5)
O1—Zn1—N189.38 (18)C14—C15—C16121.7 (6)
O6—Zn1—N2112.73 (19)O2—C16—C11125.9 (5)
O2—Zn1—N289.48 (19)O2—C16—C15115.8 (5)
O1—Zn1—N2143.1 (2)C11—C16—C15118.2 (5)
N1—Zn1—N282.8 (2)N2—C10—C11125.9 (5)
C7—N1—C8121.9 (5)N2—C10—H10117.1
C7—N1—Zn1129.6 (4)C11—C10—H10117.1
C8—N1—Zn1107.8 (4)C12—C11—C16119.1 (6)
N3—O12—Eu194.6 (4)C12—C11—C10118.2 (6)
C1—O1—Zn1127.4 (3)C16—C11—C10122.5 (6)
C1—O1—Eu1131.8 (3)N2—C9—C8110.4 (5)
Zn1—O1—Eu1100.89 (16)N2—C9—H9A109.6
C2—O3—C18116.3 (5)C8—C9—H9A109.6
C2—O3—Eu1117.2 (3)N2—C9—H9B109.6
C18—O3—Eu1126.5 (4)C8—C9—H9B109.6
N4—O9—Eu194.8 (3)H9A—C9—H9B108.1
N4—O8—Eu195.7 (4)O4—C17—H17A109.5
O10—N4—O8124.6 (6)O4—C17—H17B109.5
O10—N4—O9120.1 (6)H17A—C17—H17B109.5
O8—N4—O9115.3 (5)O4—C17—H17C109.5
O1—C1—C2115.6 (5)H17A—C17—H17C109.5
O1—C1—C6124.8 (5)H17B—C17—H17C109.5
C2—C1—C6119.5 (6)C15—C14—C13117.6 (6)
C5—C4—C3122.5 (7)C15—C14—H14121.2
C5—C4—H4118.8C13—C14—H14121.2
C3—C4—H4118.8C13—C12—C11121.3 (6)
O3—C2—C1113.1 (5)C13—C12—H12119.3
O3—C2—C3124.6 (6)C11—C12—H12119.3
C1—C2—C3122.3 (6)C12—C13—C14122.0 (7)
O13—N3—O11121.4 (6)C12—C13—H13119.0
O13—N3—O12123.2 (7)C14—C13—H13119.0
O11—N3—O12115.4 (5)
D—H···AD—HH···AD···AD—H···A
C12—H12···O11i0.932.493.406 (8)169
C8—H8A···O13ii0.972.503.442 (9)163
Table 1

Selected bond lengths (Å)

Eu1—O12.234 (4)
Eu1—O22.239 (4)
Eu1—O32.584 (4)
Eu1—O42.587 (4)
Eu1—O52.252 (5)
Eu1—O82.432 (4)
Eu1—O92.405 (4)
Eu1—O112.368 (4)
Eu1—O122.400 (5)
Zn1—O12.027 (4)
Zn1—O22.005 (4)
Zn1—O61.971 (4)
Zn1—N12.032 (5)
Zn1—N22.048 (5)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
C12—H12⋯O11i0.932.493.406 (8)169
C8—H8A⋯O13ii0.972.503.442 (9)163

Symmetry codes: (i) ; (ii) .

  3 in total

1.  Unusual electronic effects of electron-withdrawing sulfonamide groups in optically and magnetically active self-assembled noncovalent heterodimetallic d-f podates.

Authors:  C Edder; C Piguet; G Bernardinelli; J Mareda; C G Bochet; J C Bünzli; G Hopfgartner
Journal:  Inorg Chem       Date:  2000-10-30       Impact factor: 5.165

2.  Gadolinium(III) Chelates as MRI Contrast Agents: Structure, Dynamics, and Applications.

Authors:  P Caravan; J J Ellison; T J McMurry; R B Lauffer
Journal:  Chem Rev       Date:  1999-09-08       Impact factor: 60.622

3.  Syntheses, structures, and magnetic properties of diphenoxo-bridged M(II)Ln(III) complexes derived from N,N'-ethylenebis(3-ethoxysalicylaldiimine) (M = Cu or Ni; Ln = Ce-Yb): observation of surprisingly strong exchange interactions.

Authors:  Rajesh Koner; Hsin-Huang Lin; Ho-Hsiang Wei; Sasankasekhar Mohanta
Journal:  Inorg Chem       Date:  2005-05-16       Impact factor: 5.165

  3 in total
  1 in total

1.  Retraction of articles.

Authors: 
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-03-17
  1 in total

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