Literature DB >> 21589254

Tetra-μ-acetato-κO:O';κO,O':O;κO:O,O'-bis-[(acetato-κO,O')(1,10-phenanthroline-κN,N')europium(III)].

Rui-Qing Fan1, Cun-Fa Sun, Yu-Lin Yang.   

Abstract

In the title centrosymmetric dinuclear complex, [Eu(2)(CHn class="Chemical">(3)CO(2))(6)(C(12)H(8)N(2))(2)], the Eu(III) atom is nine-coordinated by two N atoms from a 1,10-phenanthroline ligand and seven O atoms from five acetate ligands (two bidentate, three monodentate). The crystal structure is stabilized by π-π stacking inter-actions between the pyridine and benzene rings of adjacent mol-ecules, with a centroid-centroid distance of 3.829 (2) Å.

Entities:  

Year:  2010        PMID: 21589254      PMCID: PMC3011772          DOI: 10.1107/S1600536810046131

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


Related literature

For general background to lanthanide complexes based on nitro­gen-containing organic ligands, see: Lima et al. (2009 ▶); Prasad & Rajasekharan (2009 ▶); Xiang et al. (2009 ▶); Yang et al. (2009 ▶).

Experimental

Crystal data

[Eu2(C2H3n class="Chemical">O2)6(C12H8N2)2] M = 1018.59 Monoclinic, a = 9.7249 (19) Å b = 23.670 (5) Å c = 8.2984 (17) Å β = 90.32 (3)° V = 1910.2 (7) Å3 Z = 2 Mo Kα radiation μ = 3.32 mm−1 T = 293 K 0.20 × 0.10 × 0.08 mm

Data collection

Bruker APEX CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.559, T max = 0.789 18210 measured reflections 4324 independent reflections 2668 reflections with I > 2σ(I) R int = 0.125

Refinement

R[F 2 > 2σ(F 2)] = 0.057 wR(F 2) = 0.101 S = 0.99 4324 reflections 244 parameters H-atom parameters constrained Δρmax = 1.02 e Å−3 Δρmin = −0.90 e Å−3 Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶) and Mercury (Macrae et al., 2006 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810046131/hy2358sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810046131/hy2358Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Eu2(C2H3O2)6(C12H8N2)2]F(000) = 1000
Mr = 1018.59Dx = 1.771 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3465 reflections
a = 9.7249 (19) Åθ = 3.3–27.5°
b = 23.670 (5) ŵ = 3.32 mm1
c = 8.2984 (17) ÅT = 293 K
β = 90.32 (3)°Block, colorless
V = 1910.2 (7) Å30.20 × 0.10 × 0.08 mm
Z = 2
Bruker APEX CCD diffractometer4324 independent reflections
Radiation source: fine-focus sealed tube2668 reflections with I > 2σ(I)
graphiteRint = 0.125
φ and ω scansθmax = 27.5°, θmin = 3.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −12→12
Tmin = 0.559, Tmax = 0.789k = −30→30
18210 measured reflectionsl = −9→10
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.101H-atom parameters constrained
S = 0.99w = 1/[σ2(Fo2) + (0.0299P)2] where P = (Fo2 + 2Fc2)/3
4324 reflections(Δ/σ)max < 0.001
244 parametersΔρmax = 1.02 e Å3
0 restraintsΔρmin = −0.90 e Å3
xyzUiso*/Ueq
Eu10.13542 (4)0.060026 (13)0.95103 (4)0.03528 (13)
O10.0766 (5)0.0993 (2)1.2170 (5)0.0495 (14)
O20.1771 (6)0.0886 (2)0.6727 (6)0.0517 (14)
O30.3281 (5)0.0295 (2)0.7710 (6)0.0507 (14)
O4−0.0904 (5)0.08694 (18)0.8702 (6)0.0472 (13)
O5−0.2383 (5)0.01441 (19)0.8964 (6)0.0458 (13)
O60.0405 (5)−0.02279 (18)0.8341 (5)0.0423 (12)
N10.1482 (7)0.1713 (2)0.9431 (8)0.0511 (16)
N20.3590 (6)0.1076 (2)1.0623 (7)0.0408 (14)
C10.4668 (7)0.0771 (3)1.1138 (8)0.0431 (19)
H1A0.46220.03801.10350.052*
C20.5841 (8)0.1002 (3)1.1811 (9)0.053 (2)
H2A0.65660.07721.21330.063*
C30.5921 (9)0.1571 (3)1.1996 (10)0.066 (3)
H3A0.67020.17331.24540.079*
C40.4818 (8)0.1915 (3)1.1492 (10)0.055 (2)
C50.4823 (11)0.2517 (4)1.1624 (12)0.084 (3)
H5A0.55650.26941.21240.101*
C60.3792 (11)0.2832 (4)1.1049 (12)0.086 (3)
H6A0.38300.32221.11620.103*
C70.2628 (9)0.2580 (3)1.0260 (10)0.064 (2)
C80.1551 (10)0.2892 (3)0.9555 (11)0.075 (3)
H8A0.15690.32850.95960.090*
C90.0499 (11)0.2627 (3)0.8825 (12)0.083 (3)
H9A−0.02140.28310.83520.100*
C100.0503 (10)0.2035 (3)0.8793 (10)0.067 (3)
H10A−0.02330.18550.82890.081*
C110.2555 (8)0.1984 (3)1.0144 (9)0.049 (2)
C120.3674 (8)0.1641 (3)1.0785 (8)0.0447 (19)
C13−0.0119 (7)0.0640 (3)1.2593 (8)0.0391 (16)
C14−0.0864 (8)0.0707 (3)1.4136 (8)0.055 (2)
H14A−0.10520.03421.45850.083*
H14B−0.17140.09031.39440.083*
H14C−0.03090.09211.48770.083*
C150.2801 (8)0.0583 (3)0.6569 (9)0.0431 (17)
C160.3468 (9)0.0548 (4)0.4946 (9)0.063 (2)
H16A0.43430.07360.49820.095*
H16B0.28890.07270.41560.095*
H16C0.36000.01590.46610.095*
C17−0.2064 (8)0.0637 (3)0.8529 (8)0.0422 (17)
C18−0.3164 (8)0.0977 (3)0.7682 (9)0.056 (2)
H18A−0.39950.07590.76170.084*
H18B−0.28620.10710.66150.084*
H18C−0.33340.13180.82750.084*
U11U22U33U12U13U23
Eu10.0401 (2)0.02511 (17)0.0406 (2)−0.00140 (19)−0.00452 (14)−0.00032 (19)
O10.061 (4)0.044 (3)0.044 (3)−0.015 (3)0.004 (3)−0.011 (2)
O20.061 (4)0.045 (3)0.049 (3)0.014 (3)−0.002 (3)0.005 (2)
O30.046 (3)0.056 (3)0.049 (3)0.011 (3)−0.004 (3)0.002 (3)
O40.041 (3)0.036 (3)0.064 (3)−0.003 (2)−0.009 (3)0.007 (3)
O50.047 (3)0.030 (3)0.059 (3)0.000 (2)−0.014 (3)0.008 (2)
O60.055 (3)0.027 (3)0.044 (3)−0.005 (2)−0.002 (2)−0.011 (2)
N10.059 (4)0.033 (3)0.061 (4)0.001 (3)−0.008 (3)0.001 (3)
N20.047 (4)0.033 (3)0.042 (3)−0.006 (3)0.001 (3)−0.001 (3)
C10.039 (5)0.035 (4)0.055 (5)0.002 (3)−0.004 (4)0.003 (3)
C20.048 (5)0.049 (5)0.062 (5)−0.003 (4)−0.012 (4)−0.006 (4)
C30.064 (6)0.055 (5)0.077 (6)−0.007 (5)−0.019 (5)−0.014 (5)
C40.051 (5)0.039 (4)0.075 (6)−0.008 (4)−0.007 (4)−0.002 (4)
C50.092 (8)0.046 (5)0.114 (8)−0.016 (5)−0.034 (7)−0.012 (6)
C60.106 (9)0.033 (5)0.118 (9)−0.011 (5)−0.021 (7)−0.015 (5)
C70.075 (7)0.035 (4)0.081 (6)−0.002 (4)−0.008 (5)−0.003 (4)
C80.096 (8)0.031 (4)0.099 (7)0.010 (5)−0.017 (6)0.005 (5)
C90.101 (8)0.038 (5)0.110 (8)0.014 (5)−0.037 (7)0.006 (5)
C100.071 (7)0.045 (5)0.086 (6)−0.002 (4)−0.027 (5)0.006 (5)
C110.057 (5)0.028 (4)0.061 (5)−0.009 (4)0.003 (4)−0.003 (4)
C120.055 (5)0.031 (4)0.048 (4)−0.006 (4)0.002 (4)−0.001 (3)
C130.035 (4)0.037 (4)0.046 (4)0.000 (4)−0.001 (3)0.000 (4)
C140.051 (5)0.073 (6)0.042 (4)−0.006 (4)0.009 (4)−0.015 (4)
C150.040 (4)0.031 (4)0.059 (5)−0.007 (4)−0.007 (4)−0.003 (4)
C160.065 (6)0.074 (6)0.052 (5)−0.001 (5)0.004 (4)−0.001 (4)
C170.043 (4)0.038 (4)0.046 (4)0.009 (4)0.002 (3)−0.001 (4)
C180.052 (6)0.059 (5)0.057 (5)0.003 (4)−0.007 (4)0.011 (4)
Eu1—O12.465 (5)C4—C121.412 (9)
Eu1—O22.443 (5)C4—C51.428 (10)
Eu1—O32.509 (5)C5—C61.335 (11)
Eu1—O42.380 (5)C5—H5A0.9300
Eu1—O5i2.387 (4)C6—C71.434 (11)
Eu1—O62.372 (4)C6—H6A0.9300
Eu1—O6i2.630 (5)C7—C81.407 (10)
Eu1—N12.639 (6)C7—C111.414 (9)
Eu1—N22.613 (6)C8—C91.342 (11)
O1—C131.251 (8)C8—H8A0.9300
O2—C151.240 (8)C9—C101.401 (10)
O3—C151.254 (8)C9—H9A0.9300
O4—C171.262 (8)C10—H10A0.9300
O5—C171.261 (8)C11—C121.456 (10)
O5—Eu1i2.387 (4)C13—O6i1.276 (7)
O6—C13i1.276 (7)C13—C141.484 (10)
O6—Eu1i2.630 (5)C14—H14A0.9600
N1—C101.328 (9)C14—H14B0.9600
N1—C111.358 (8)C14—H14C0.9600
N2—C11.342 (8)C15—C161.501 (11)
N2—C121.346 (8)C16—H16A0.9600
C1—C21.381 (9)C16—H16B0.9600
C1—H1A0.9300C16—H16C0.9600
C2—C31.356 (10)C17—C181.509 (9)
C2—H2A0.9300C18—H18A0.9600
C3—C41.409 (11)C18—H18B0.9600
C3—H3A0.9300C18—H18C0.9600
O6—Eu1—O475.50 (15)C2—C3—H3A120.1
O6—Eu1—O5i76.58 (15)C4—C3—H3A120.1
O4—Eu1—O5i136.96 (17)C3—C4—C12117.0 (7)
O6—Eu1—O284.76 (16)C3—C4—C5123.5 (7)
O4—Eu1—O279.46 (18)C12—C4—C5119.5 (7)
O5i—Eu1—O2129.42 (18)C6—C5—C4121.8 (8)
O6—Eu1—O1125.90 (17)C6—C5—H5A119.1
O4—Eu1—O186.14 (18)C4—C5—H5A119.1
O5i—Eu1—O184.40 (17)C5—C6—C7121.3 (8)
O2—Eu1—O1141.47 (16)C5—C6—H6A119.3
O6—Eu1—O378.98 (17)C7—C6—H6A119.3
O4—Eu1—O3126.90 (16)C8—C7—C11117.3 (8)
O5i—Eu1—O377.95 (17)C8—C7—C6123.7 (8)
O2—Eu1—O352.29 (16)C11—C7—C6119.0 (8)
O1—Eu1—O3145.03 (16)C9—C8—C7120.4 (8)
O6—Eu1—N2145.30 (17)C9—C8—H8A119.8
O4—Eu1—N2138.49 (16)C7—C8—H8A119.8
O5i—Eu1—N277.60 (16)C8—C9—C10118.3 (8)
O2—Eu1—N294.15 (18)C8—C9—H9A120.9
O1—Eu1—N273.60 (18)C10—C9—H9A120.9
O3—Eu1—N273.25 (18)N1—C10—C9124.7 (8)
O6—Eu1—O6i75.36 (17)N1—C10—H10A117.7
O4—Eu1—O6i71.21 (16)C9—C10—H10A117.7
O5i—Eu1—O6i70.45 (16)N1—C11—C7122.6 (7)
O2—Eu1—O6i147.77 (16)N1—C11—C12117.8 (6)
O1—Eu1—O6i50.54 (15)C7—C11—C12119.6 (7)
O3—Eu1—O6i142.95 (15)N2—C12—C4123.0 (7)
N2—Eu1—O6i116.62 (16)N2—C12—C11118.2 (6)
O6—Eu1—N1146.45 (16)C4—C12—C11118.7 (6)
O4—Eu1—N176.66 (18)O1—C13—O6i119.3 (7)
O5i—Eu1—N1136.95 (16)O1—C13—C14120.7 (6)
O2—Eu1—N172.03 (18)O6i—C13—C14120.0 (7)
O1—Eu1—N169.92 (18)C13—C14—H14A109.5
O3—Eu1—N1103.7 (2)C13—C14—H14B109.5
N2—Eu1—N162.53 (18)H14A—C14—H14B109.5
O6i—Eu1—N1112.49 (18)C13—C14—H14C109.5
C13—O1—Eu199.3 (4)H14A—C14—H14C109.5
C15—O2—Eu194.4 (4)H14B—C14—H14C109.5
C15—O3—Eu191.0 (5)O2—C15—O3122.2 (7)
C17—O4—Eu1137.6 (4)O2—C15—C16118.7 (7)
C17—O5—Eu1i137.0 (4)O3—C15—C16119.1 (7)
C13i—O6—Eu1164.5 (5)C15—C16—H16A109.5
C13i—O6—Eu1i90.8 (4)C15—C16—H16B109.5
Eu1—O6—Eu1i104.64 (16)H16A—C16—H16B109.5
C10—N1—C11116.8 (7)C15—C16—H16C109.5
C10—N1—Eu1123.3 (5)H16A—C16—H16C109.5
C11—N1—Eu1119.8 (4)H16B—C16—H16C109.5
C1—N2—C12117.2 (6)O4—C17—O5126.3 (6)
C1—N2—Eu1121.8 (4)O4—C17—C18116.8 (7)
C12—N2—Eu1120.9 (5)O5—C17—C18116.9 (7)
N2—C1—C2123.9 (7)C17—C18—H18A109.5
N2—C1—H1A118.1C17—C18—H18B109.5
C2—C1—H1A118.1H18A—C18—H18B109.5
C3—C2—C1119.1 (7)C17—C18—H18C109.5
C3—C2—H2A120.5H18A—C18—H18C109.5
C1—C2—H2A120.5H18B—C18—H18C109.5
C2—C3—C4119.9 (7)
Table 1

Selected bond lengths (Å)

Eu1—O12.465 (5)
Eu1—O22.443 (5)
Eu1—O32.509 (5)
Eu1—O42.380 (5)
Eu1—O5i2.387 (4)
Eu1—O62.372 (4)
Eu1—O6i2.630 (5)
Eu1—N12.639 (6)
Eu1—N22.613 (6)

Symmetry code: (i) .

  3 in total

1.  A short history of SHELX.

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

2.  Structural diversity of infinite 3d-4f heterometallic cluster compounds driven by various lanthanide radii.

Authors:  Shengchang Xiang; Shengmin Hu; Tianlu Sheng; Jianshan Chen; Xintao Wu
Journal:  Chemistry       Date:  2009-11-16       Impact factor: 5.236

3.  Cerium(IV)-lanthanide(III)-pyridine-2,6-dicarboxylic acid system: coordination salts, chains, and rings.

Authors:  T K Prasad; M V Rajasekharan
Journal:  Inorg Chem       Date:  2009-12-21       Impact factor: 5.165

  3 in total

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