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Acta Cryst. (2007). E63, m1694    [ doi:10.1107/S160053680702497X ]

Di-[mu]2-acetato-bis{[mu]2-1,1'-[propane-1,3-diylbis(nitrilomethylidyne)]di-2-naphtholato}tricobalt(II)

Y.-P. Diao, S.-S. Huang, H.-L. Zhang, S. Deng and K.-X. Liu

Abstract top

The title compound, [Co3(C25H20N2O2)2(C2H3O2)2], is an acetate- and phenolate-bridged trinuclear cobalt(II) complex. The central Co atom, lying on an inversion centre, is in an octahedral geometry. Each terminal Co atom is in a square-pyramidal geometry.

Comment top

Polynuclear complexes play an important role in the development of coordination chemistry related to magnetism and molecular architectures (Eshel et al., 2000; Jiang et al., 2005; Escuer et al., 2000; El-Behairy et al., 1997; Manhas et al., 2005). The prime strategy for designing these molecular materials is to use suitable bridging ligands that determine the nature of the magnetic interactions (Salem, 2005; Dohlakiya & Patel, 2005). We have recently reported a few polynuclear transition metal complexes (Diao, 2007a,b). As an extension of the work on the polynuclear complexes, we report herein the crystal structure of the title complex, (I).

Compound (I) is an acetate and phenolate bridged trinuclear cobalt(II) complex. The central Co atom, lying on the inversion centre, is coordinated by four O atoms from two Schiff base ligands and two O atoms from two acetate groups, forming an octahedral geometry. Each terminal Co atom is coordinated by two O and two N atoms from one Schiff base ligand and one O atom of an acetate group, forming a square pyramidal geometry.

Related literature top

For related literature, see: Diao (2007a, 2007b); Dohlakiya & Patel (2005); El-Behairy, Khalil, Ishak & Abd El-Halim (1997); Escuer et al. (2000); Eshel et al. (2000); Jiang et al. (2005); Manhas et al. (2005); Salem (2005).

Experimental top

N,N'-1,3-Propanediamine (0.1 mmol, 7.5 mg), 2-hydroxy-1-naphthaldehyde (0.2 mmol, 34.3 mg), and cobalt acetate (0.2 mmol, 50.0 mg) were dissolved in a methanol solution (20 ml). The mixture was stirred for half an hour at room temperature, giving a red solution. After allowing the solution to stand in dark for a week, brown block-like crystals were formed.

Refinement top

All H atoms were placed in idealized positions and constrained to ride on their parent atoms, with C—H = 0.93–0.96 Å, and with Uiso(H) values were fixed at 0.08 Å2.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. Molecular structure of (I). Displacement ellipsoids are drawn at the 30% probability level. Symmetry operator (A): 2 - x,-y,-z.
Di-µ2-acetato-bis{µ2-1,1'-[propane-1,3-diylbis(nitrilomethylidyne)]di- 2-naphtholato}tricobalt(II) top
Crystal data top
[Co3(C25H20N2O2)2(C2H3O2)2]F(000) = 1086
Mr = 1055.74Dx = 1.569 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 11.770 (3) ÅCell parameters from 2321 reflections
b = 11.765 (4) Åθ = 2.2–25.0°
c = 16.137 (3) ŵ = 1.17 mm−1
β = 90.61 (2)°T = 293 K
V = 2234.4 (10) Å3Block, brown
Z = 20.37 × 0.33 × 0.32 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer		3927 independent reflections
Radiation source: fine-focus sealed tube2604 reflections with I > 2σ(I)
graphiteRint = 0.032
ω scansθmax = 25.5°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		h = −14→11
Tmin = 0.672, Tmax = 0.707k = −14→12
7988 measured reflectionsl = −18→16
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.083H-atom parameters constrained
S = 0.86 w = 1/[σ2(Fo2) + (0.0348P)2]
where P = (Fo2 + 2Fc2)/3
3927 reflections(Δ/σ)max < 0.001
313 parametersΔρmax = 0.45 e Å−3
0 restraintsΔρmin = −0.24 e Å−3
Crystal data top
[Co3(C25H20N2O2)2(C2H3O2)2]V = 2234.4 (10) Å3
Mr = 1055.74Z = 2
Monoclinic, P21/nMo Kα radiation
a = 11.770 (3) ŵ = 1.17 mm−1
b = 11.765 (4) ÅT = 293 K
c = 16.137 (3) Å0.37 × 0.33 × 0.32 mm
β = 90.61 (2)°
Data collection top
Bruker SMART CCD area-detector
diffractometer		3927 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		2604 reflections with I > 2σ(I)
Tmin = 0.672, Tmax = 0.707Rint = 0.032
7988 measured reflectionsθmax = 25.5°
Refinement top
R[F2 > 2σ(F2)] = 0.041H-atom parameters constrained
wR(F2) = 0.083Δρmax = 0.45 e Å−3
S = 0.86Δρmin = −0.24 e Å−3
3927 reflectionsAbsolute structure: ?
313 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Co10.98733 (4)0.16208 (3)0.14688 (3)0.04044 (15)
Co21.00000.00000.00000.03656 (18)
O10.94380 (18)0.00047 (16)0.12547 (12)0.0409 (6)
O20.96231 (18)0.17133 (16)0.02205 (12)0.0397 (6)
O31.16502 (19)0.03277 (18)0.03765 (13)0.0451 (6)
O41.15744 (19)0.14127 (18)0.15148 (13)0.0455 (6)
N10.9624 (2)0.1354 (2)0.27103 (16)0.0404 (7)
N20.9711 (2)0.3328 (2)0.15027 (16)0.0388 (7)
C10.9099 (3)−0.0671 (3)0.2633 (2)0.0367 (8)
C20.9091 (3)−0.0797 (3)0.1763 (2)0.0354 (8)
C30.8677 (3)−0.1826 (3)0.1412 (2)0.0418 (9)
H3A0.8624−0.18890.08190.080*
C40.8370 (3)−0.2703 (3)0.1894 (2)0.0459 (9)
H4A0.8077−0.33790.16370.080*
C50.8134 (3)−0.3600 (3)0.3257 (2)0.0491 (10)
H5A0.7868−0.42760.29850.080*
C60.8199 (3)−0.3570 (3)0.4096 (2)0.0544 (10)
H6A0.7960−0.42110.44190.080*
C70.8608 (3)−0.2584 (3)0.4477 (2)0.0568 (11)
H7A0.8680−0.25650.50700.080*
C80.8907 (3)−0.1649 (3)0.4025 (2)0.0488 (9)
H8A0.9195−0.09880.43050.080*
C90.8441 (3)−0.2658 (3)0.2771 (2)0.0391 (8)
C100.8816 (3)−0.1639 (3)0.3151 (2)0.0388 (8)
C110.9360 (3)0.0383 (3)0.3032 (2)0.0419 (9)
H110.93360.03690.36080.050*
C120.9865 (3)0.2281 (3)0.3306 (2)0.0497 (10)
H12A1.06750.23220.33740.080*
H12B0.95460.20950.38350.080*
C130.9476 (3)0.3436 (3)0.3019 (2)0.0488 (9)
H13A0.95460.39650.34690.080*
H13B0.86850.33710.28760.080*
C141.0077 (3)0.3899 (3)0.2268 (2)0.0473 (9)
H14A0.99520.47020.22170.080*
H14B1.08760.37730.23470.080*
C150.9328 (3)0.3953 (3)0.0914 (2)0.0410 (9)
H150.93180.47300.10190.049*
C160.8909 (3)0.3609 (2)0.0109 (2)0.0366 (8)
C170.9088 (3)0.2510 (3)−0.0204 (2)0.0368 (8)
C180.8683 (3)0.2252 (3)−0.10198 (19)0.0415 (9)
H18A0.88320.1512−0.12440.080*
C190.8109 (3)0.3032 (3)−0.1478 (2)0.0445 (9)
H19A0.78520.2833−0.20260.080*
C200.7206 (3)0.4910 (3)−0.1634 (2)0.0497 (9)
H20A0.69390.4688−0.21740.080*
C210.6942 (3)0.5958 (3)−0.1325 (2)0.0557 (10)
H21A0.64910.6481−0.16450.080*
C220.7337 (3)0.6249 (3)−0.0535 (2)0.0604 (11)
H22A0.71500.6982−0.03120.080*
C230.7984 (3)0.5520 (3)−0.0082 (2)0.0554 (11)
H23A0.82600.57570.04530.080*
C240.8269 (3)0.4429 (3)−0.0374 (2)0.0398 (8)
C250.7865 (3)0.4134 (3)−0.1165 (2)0.0390 (8)
C261.3363 (3)0.0714 (3)0.1094 (2)0.0684 (12)
H26A1.37010.05660.05660.080*
H26B1.35290.00970.14650.080*
H26C1.36660.14070.13180.080*
C271.2099 (3)0.0826 (3)0.0986 (2)0.0417 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0557 (3)0.0357 (3)0.0299 (3)0.0030 (2)0.0046 (2)−0.0040 (2)
Co20.0490 (4)0.0338 (3)0.0270 (4)0.0048 (3)0.0043 (3)−0.0027 (3)
O10.0589 (16)0.0341 (12)0.0299 (14)0.0000 (11)0.0084 (11)−0.0010 (11)
O20.0565 (16)0.0313 (11)0.0313 (14)0.0058 (11)0.0013 (11)−0.0032 (10)
O30.0463 (16)0.0503 (14)0.0387 (15)0.0043 (11)0.0018 (12)−0.0072 (12)
O40.0517 (16)0.0486 (14)0.0362 (15)0.0058 (11)−0.0015 (12)−0.0063 (11)
N10.0506 (19)0.0381 (16)0.0324 (18)0.0000 (13)0.0027 (14)−0.0056 (13)
N20.0478 (19)0.0343 (14)0.0343 (17)0.0022 (13)−0.0016 (14)−0.0033 (14)
C10.042 (2)0.0394 (19)0.029 (2)0.0004 (15)0.0037 (16)−0.0009 (16)
C20.039 (2)0.0370 (19)0.030 (2)0.0047 (15)0.0035 (16)−0.0010 (16)
C30.052 (2)0.0390 (19)0.034 (2)−0.0020 (16)0.0086 (17)−0.0056 (16)
C40.053 (3)0.041 (2)0.043 (3)−0.0027 (17)0.0077 (18)−0.0085 (18)
C50.054 (3)0.044 (2)0.049 (3)−0.0059 (17)0.0082 (19)0.0035 (18)
C60.057 (3)0.057 (2)0.049 (3)−0.0078 (19)0.012 (2)0.014 (2)
C70.065 (3)0.070 (3)0.036 (2)−0.004 (2)0.005 (2)0.008 (2)
C80.057 (3)0.055 (2)0.035 (2)−0.0049 (19)0.0078 (18)0.0027 (19)
C90.041 (2)0.0382 (19)0.038 (2)0.0007 (15)0.0070 (17)−0.0005 (17)
C100.039 (2)0.045 (2)0.033 (2)0.0039 (16)0.0063 (16)0.0028 (17)
C110.051 (2)0.050 (2)0.025 (2)−0.0043 (17)0.0029 (16)0.0012 (17)
C120.071 (3)0.046 (2)0.032 (2)−0.0096 (18)0.0030 (19)−0.0083 (17)
C130.062 (3)0.043 (2)0.042 (2)−0.0078 (18)0.0055 (19)−0.0175 (18)
C140.059 (3)0.044 (2)0.038 (2)−0.0038 (17)−0.0046 (19)−0.0080 (17)
C150.052 (2)0.0312 (18)0.040 (2)0.0012 (16)0.0055 (18)−0.0044 (17)
C160.046 (2)0.0338 (18)0.030 (2)0.0008 (15)0.0029 (16)−0.0014 (15)
C170.041 (2)0.0379 (18)0.031 (2)−0.0001 (16)0.0045 (16)0.0031 (16)
C180.055 (2)0.0402 (19)0.029 (2)0.0029 (16)0.0049 (18)−0.0025 (16)
C190.052 (2)0.046 (2)0.036 (2)−0.0022 (17)−0.0017 (18)−0.0021 (17)
C200.053 (2)0.049 (2)0.047 (2)−0.0042 (18)−0.0040 (18)0.0018 (19)
C210.060 (3)0.048 (2)0.059 (3)0.0060 (19)−0.003 (2)0.012 (2)
C220.084 (3)0.042 (2)0.056 (3)0.015 (2)0.000 (2)−0.001 (2)
C230.081 (3)0.040 (2)0.044 (2)0.013 (2)−0.006 (2)−0.0053 (18)
C240.048 (2)0.0349 (18)0.036 (2)−0.0028 (16)0.0049 (17)0.0029 (16)
C250.047 (2)0.0387 (19)0.032 (2)−0.0002 (16)−0.0004 (17)0.0019 (16)
C260.057 (3)0.079 (3)0.069 (3)0.016 (2)−0.011 (2)−0.012 (2)
C270.048 (3)0.0341 (19)0.043 (3)0.0043 (17)0.0031 (19)0.0078 (18)
Geometric parameters (Å, °) top
Co1—O11.998 (2)C8—H8A0.9597
Co1—O42.018 (2)C9—C101.415 (4)
Co1—N22.019 (3)C11—H110.9300
Co1—O22.036 (2)C12—C131.506 (4)
Co1—N12.052 (3)C12—H12A0.9597
Co2—O32.065 (2)C12—H12B0.9603
Co2—O3i2.065 (2)C13—C141.510 (4)
Co2—O2i2.095 (2)C13—H13A0.9599
Co2—O22.095 (2)C13—H13B0.9597
Co2—O1i2.137 (2)C14—H14A0.9598
Co2—O12.137 (2)C14—H14B0.9597
O1—C21.318 (3)C15—C161.442 (4)
O2—C171.317 (3)C15—H150.9300
O3—C271.257 (4)C16—C171.406 (4)
O4—C271.263 (4)C16—C241.446 (4)
N1—C111.294 (4)C17—C181.428 (4)
N1—C121.479 (4)C18—C191.356 (4)
N2—C151.279 (3)C18—H18A0.9599
N2—C141.467 (4)C19—C251.421 (4)
C1—C21.412 (4)C19—H19A0.9600
C1—C111.429 (4)C20—C211.366 (4)
C1—C101.453 (4)C20—C251.413 (4)
C2—C31.421 (4)C20—H20A0.9600
C3—C41.344 (4)C21—C221.396 (5)
C3—H3A0.9602C21—H21A0.9599
C4—C91.418 (4)C22—C231.355 (4)
C4—H4A0.9599C22—H22A0.9599
C5—C61.356 (4)C23—C241.409 (4)
C5—C91.408 (4)C23—H23A0.9600
C5—H5A0.9598C24—C251.402 (4)
C6—C71.396 (5)C26—C271.502 (5)
C6—H6A0.9600C26—H26A0.9600
C7—C81.367 (4)C26—H26B0.9600
C7—H7A0.9602C26—H26C0.9600
C8—C101.413 (4)
O1—Co1—O498.24 (9)C8—C10—C9116.5 (3)
O1—Co1—N2158.02 (10)C8—C10—C1124.4 (3)
O4—Co1—N2102.36 (10)C9—C10—C1119.1 (3)
O1—Co1—O281.12 (8)N1—C11—C1129.6 (3)
O4—Co1—O2100.13 (9)N1—C11—H11115.2
N2—Co1—O287.76 (9)C1—C11—H11115.2
O1—Co1—N189.09 (9)N1—C12—C13114.2 (3)
O4—Co1—N195.61 (10)N1—C12—H12A107.2
N2—Co1—N196.38 (10)C13—C12—H12A106.7
O2—Co1—N1162.48 (10)N1—C12—H12B109.6
O3—Co2—O3i180.00 (17)C13—C12—H12B111.0
O3—Co2—O2i91.69 (8)H12A—C12—H12B107.9
O3i—Co2—O2i88.31 (8)C12—C13—C14115.4 (3)
O3—Co2—O288.31 (8)C12—C13—H13A109.2
O3i—Co2—O291.69 (8)C14—C13—H13A109.7
O2i—Co2—O2180.00 (15)C12—C13—H13B107.0
O3—Co2—O1i88.83 (9)C14—C13—H13B107.4
O3i—Co2—O1i91.17 (9)H13A—C13—H13B107.9
O2i—Co2—O1i76.60 (7)N2—C14—C13112.0 (3)
O2—Co2—O1i103.40 (7)N2—C14—H14A109.6
O3—Co2—O191.17 (9)C13—C14—H14A110.6
O3i—Co2—O188.83 (9)N2—C14—H14B108.7
O2i—Co2—O1103.40 (7)C13—C14—H14B107.7
O2—Co2—O176.60 (7)H14A—C14—H14B108.2
O1i—Co2—O1180.00 (15)N2—C15—C16128.5 (3)
C2—O1—Co1130.82 (19)N2—C15—H15115.8
C2—O1—Co2133.59 (18)C16—C15—H15115.8
Co1—O1—Co294.87 (8)C17—C16—C15122.1 (3)
C17—O2—Co1128.05 (19)C17—C16—C24119.9 (3)
C17—O2—Co2134.18 (19)C15—C16—C24118.0 (3)
Co1—O2—Co295.05 (8)O2—C17—C16122.7 (3)
C27—O3—Co2134.7 (2)O2—C17—C18118.8 (3)
C27—O4—Co1122.2 (2)C16—C17—C18118.5 (3)
C11—N1—C12115.8 (3)C19—C18—C17121.3 (3)
C11—N1—Co1124.3 (2)C19—C18—H18A120.0
C12—N1—Co1119.57 (19)C17—C18—H18A118.7
C15—N2—C14117.4 (3)C18—C19—C25121.7 (3)
C15—N2—Co1125.8 (2)C18—C19—H19A119.2
C14—N2—Co1116.8 (2)C25—C19—H19A119.2
C2—C1—C11122.5 (3)C21—C20—C25120.9 (3)
C2—C1—C10119.4 (3)C21—C20—H20A120.3
C11—C1—C10118.1 (3)C25—C20—H20A118.8
O1—C2—C1123.1 (3)C20—C21—C22118.7 (3)
O1—C2—C3117.9 (3)C20—C21—H21A120.6
C1—C2—C3119.0 (3)C22—C21—H21A120.7
C4—C3—C2121.1 (3)C23—C22—C21121.1 (3)
C4—C3—H3A120.1C23—C22—H22A119.8
C2—C3—H3A118.8C21—C22—H22A119.1
C3—C4—C9122.4 (3)C22—C23—C24122.1 (3)
C3—C4—H4A118.9C22—C23—H23A118.9
C9—C4—H4A118.6C24—C23—H23A119.0
C6—C5—C9121.6 (3)C25—C24—C23116.7 (3)
C6—C5—H5A119.6C25—C24—C16119.7 (3)
C9—C5—H5A118.8C23—C24—C16123.5 (3)
C5—C6—C7118.4 (3)C24—C25—C20120.4 (3)
C5—C6—H6A120.4C24—C25—C19118.8 (3)
C7—C6—H6A121.1C20—C25—C19120.7 (3)
C8—C7—C6121.6 (3)C27—C26—H26A109.5
C8—C7—H7A119.5C27—C26—H26B109.5
C6—C7—H7A118.9H26A—C26—H26B109.5
C7—C8—C10121.4 (3)C27—C26—H26C109.5
C7—C8—H8A119.5H26A—C26—H26C109.5
C10—C8—H8A119.1H26B—C26—H26C109.5
C5—C9—C10120.4 (3)O3—C27—O4125.4 (3)
C5—C9—C4121.0 (3)O3—C27—C26117.2 (3)
C10—C9—C4118.6 (3)O4—C27—C26117.4 (3)
Symmetry codes: (i) −x+2, −y, −z.
Acknowledgements top

This project was financially supported by a research grant from Dalian Medical University.

references
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