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The title linear trinuclear complex, di-μ-acetato-1:2κ2O,O′;2:3κ2O,O′-bis{2,2′-[1,4-butane­diyl­bis­(nitrilo­methyl­idyne)]­diphenolato}-1:2κ6O,N,N,O′:O,O′;2,3κ6O,O′:O,N,N,O′-tricobalt(II), [Co3(C18H18N2O2)2(C2H3O2)2], was prepared by the reaction of the tetradentate Schiff base ligand bis­(salicyl­idene)-1,4-di­amino­butane and Co(CH3COO)2·2H2O in a methanol solution. The central CoII ion, which is located on an inversion center, has a distorted octahedral coordination involving four bridging O atoms from two Schiff base ligands in the equatorial plane and one O atom from each bridging acetate group in the axial positions. The coordination around the terminal CoII ion is irregular square pyramidal, with two O and two N atoms of the ligand in the basal plane and one O atom from an acetate group in the apical position. The acetate bridges linking the central and terminal CoII ions are mutually trans. The closest Co...Co separation is 3.125 (4) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804029605/lh6297sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804029605/lh6297Isup2.hkl
Contains datablock I

CCDC reference: 227248

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.069
  • wR factor = 0.171
  • Data-to-parameter ratio = 13.4

checkCIF/PLATON results

No syntax errors found



Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.137 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.14 PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co2 - O1 .. 5.46 su PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

di-µ-acetato-1:2κ2O:O';2:3κ2O:O'-bis{2,2'-[1,4- butanediylbis(nitrilomethylidyne)]diphenolato}- 1:2κ6O,N,N,O':O,O';2,3κ6O,O':O,N,N,O'-tricobalt(II) top
Crystal data top
[Co3(C18H18N2O2)2(C2H3O2)2]F(000) = 910
Mr = 883.57Dx = 1.506 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2101 reflections
a = 9.193 (9) Åθ = 2.5–22.7°
b = 16.726 (17) ŵ = 1.32 mm1
c = 12.729 (13) ÅT = 298 K
β = 95.314 (18)°Block, red
V = 1949 (3) Å30.38 × 0.32 × 0.22 mm
Z = 2
Data collection top
Bruker SMART CCD area-detector
diffractometer
3360 independent reflections
Radiation source: fine-focus sealed tube1992 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.137
ω scansθmax = 25.0°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 910
Tmin = 0.621, Tmax = 0.745k = 1917
9778 measured reflectionsl = 1514
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)] = 0.070Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.171H-atom parameters constrained
S = 0.91 w = 1/[σ2(Fo2) + (0.0878P)2]
where P = (Fo2 + 2Fc2)/3
3360 reflections(Δ/σ)max < 0.001
251 parametersΔρmax = 1.04 e Å3
0 restraintsΔρmin = 0.69 e Å3
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
Co10.29424 (8)0.13802 (5)0.91226 (6)0.0451 (3)
Co20.50000.00001.00000.0421 (3)
N10.0665 (5)0.1565 (3)0.9367 (4)0.0417 (11)
N20.2732 (5)0.1890 (3)0.7536 (4)0.0446 (11)
O10.2971 (4)0.0550 (2)1.0367 (3)0.0380 (9)
O20.4074 (4)0.0459 (2)0.8445 (3)0.0385 (9)
O30.4449 (4)0.2153 (2)0.9920 (3)0.0503 (10)
O40.6056 (4)0.1167 (2)1.0270 (3)0.0443 (9)
C10.0013 (6)0.1209 (3)1.0048 (4)0.0361 (12)
H10.10180.12920.99960.043*
C20.0553 (5)0.0690 (3)1.0896 (4)0.0344 (12)
C30.2005 (5)0.0375 (3)1.0997 (4)0.0335 (12)
C40.2332 (6)0.0153 (3)1.1855 (4)0.0437 (14)
H40.32510.03901.19410.052*
C50.1352 (7)0.0326 (4)1.2558 (5)0.0558 (17)
H50.16240.06661.31200.067*
C60.0052 (6)0.0005 (4)1.2456 (5)0.0510 (15)
H60.07120.01171.29480.061*
C70.0418 (6)0.0467 (3)1.1633 (5)0.0436 (14)
H70.13700.06591.15400.052*
C80.0207 (6)0.2057 (4)0.8581 (5)0.0532 (16)
H8A0.12250.20250.87190.064*
H8B0.01240.18330.78860.064*
C90.0236 (7)0.2922 (4)0.8572 (6)0.0601 (17)
H9A0.04210.31970.80520.072*
H9B0.00890.31490.92550.072*
C100.1773 (7)0.3101 (4)0.8340 (5)0.0554 (17)
H10A0.18710.36760.82840.066*
H10B0.24220.29300.89430.066*
C110.2288 (7)0.2741 (3)0.7394 (5)0.0562 (16)
H11A0.31140.30460.71920.067*
H11B0.15170.27760.68220.067*
C120.2887 (6)0.1493 (4)0.6710 (5)0.0458 (14)
H120.26900.17660.60770.055*
C130.3332 (6)0.0666 (4)0.6625 (4)0.0404 (13)
C140.3888 (5)0.0185 (3)0.7481 (4)0.0348 (12)
C150.4265 (6)0.0602 (3)0.7244 (4)0.0459 (14)
H150.46600.09290.77890.055*
C160.4079 (8)0.0906 (4)0.6265 (5)0.0638 (18)
H160.43470.14320.61480.077*
C170.3504 (9)0.0452 (5)0.5439 (5)0.081 (2)
H170.33570.06690.47650.097*
C180.3148 (8)0.0319 (4)0.5614 (5)0.068 (2)
H180.27700.06290.50470.082*
C190.5638 (6)0.1876 (3)1.0345 (4)0.0436 (14)
C200.6621 (7)0.2446 (4)1.0989 (5)0.069 (2)
H20A0.71940.21561.15310.104*
H20B0.60390.28391.13060.104*
H20C0.72580.27071.05400.104*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0472 (5)0.0356 (5)0.0515 (5)0.0088 (3)0.0018 (3)0.0046 (3)
Co20.0407 (6)0.0336 (6)0.0507 (7)0.0081 (5)0.0025 (5)0.0028 (5)
N10.037 (3)0.026 (2)0.060 (3)0.006 (2)0.009 (2)0.000 (2)
N20.050 (3)0.033 (3)0.050 (3)0.007 (2)0.005 (2)0.017 (2)
O10.032 (2)0.035 (2)0.048 (2)0.0109 (16)0.0062 (16)0.0106 (16)
O20.042 (2)0.033 (2)0.039 (2)0.0135 (16)0.0043 (15)0.0024 (16)
O30.042 (2)0.037 (2)0.069 (3)0.0049 (18)0.0142 (19)0.0033 (19)
O40.039 (2)0.032 (2)0.060 (2)0.0034 (17)0.0017 (17)0.0039 (17)
C10.030 (3)0.026 (3)0.051 (3)0.002 (2)0.001 (2)0.007 (2)
C20.031 (3)0.029 (3)0.043 (3)0.006 (2)0.000 (2)0.013 (2)
C30.033 (3)0.023 (3)0.043 (3)0.002 (2)0.003 (2)0.007 (2)
C40.034 (3)0.041 (3)0.053 (4)0.005 (3)0.007 (3)0.004 (3)
C50.062 (4)0.050 (4)0.053 (4)0.022 (3)0.011 (3)0.014 (3)
C60.042 (3)0.058 (4)0.055 (4)0.016 (3)0.016 (3)0.005 (3)
C70.034 (3)0.039 (3)0.058 (4)0.003 (2)0.001 (3)0.013 (3)
C80.043 (3)0.047 (4)0.067 (4)0.009 (3)0.010 (3)0.017 (3)
C90.059 (4)0.037 (4)0.081 (5)0.012 (3)0.008 (3)0.013 (3)
C100.070 (5)0.024 (3)0.068 (4)0.010 (3)0.013 (3)0.005 (3)
C110.073 (4)0.032 (3)0.063 (4)0.011 (3)0.002 (3)0.019 (3)
C120.052 (4)0.043 (4)0.041 (3)0.002 (3)0.002 (3)0.017 (3)
C130.041 (3)0.048 (4)0.033 (3)0.002 (3)0.006 (2)0.002 (2)
C140.024 (3)0.035 (3)0.044 (3)0.000 (2)0.001 (2)0.003 (2)
C150.053 (4)0.036 (3)0.046 (3)0.008 (3)0.005 (3)0.001 (3)
C160.085 (5)0.049 (4)0.055 (4)0.010 (4)0.007 (3)0.014 (3)
C170.118 (6)0.074 (6)0.047 (4)0.012 (5)0.006 (4)0.022 (4)
C180.095 (5)0.064 (5)0.044 (4)0.014 (4)0.005 (3)0.002 (3)
C190.041 (3)0.037 (4)0.052 (3)0.006 (3)0.002 (3)0.001 (3)
C200.072 (5)0.039 (4)0.090 (5)0.002 (3)0.028 (4)0.003 (3)
Geometric parameters (Å, º) top
Co1—O32.088 (4)C6—H60.9300
Co1—O22.090 (4)C7—H70.9300
Co1—O12.104 (4)C8—C91.503 (9)
Co1—N12.167 (5)C8—H8A0.9700
Co1—N22.184 (5)C8—H8B0.9700
Co2—O12.170 (4)C9—C101.500 (9)
Co2—O1i2.170 (4)C9—H9A0.9700
Co2—O42.193 (4)C9—H9B0.9700
Co2—O4i2.193 (4)C10—C111.464 (9)
Co2—O22.218 (4)C10—H10A0.9700
Co2—O2i2.218 (4)C10—H10B0.9700
N1—C11.264 (7)C11—H11A0.9700
N1—C81.474 (7)C11—H11B0.9700
N2—C121.262 (7)C12—C131.449 (8)
N2—C111.487 (7)C12—H120.9300
O1—C31.284 (6)C13—C181.408 (8)
O2—C141.307 (6)C13—C141.412 (7)
O3—C191.262 (6)C14—C151.402 (8)
O4—C191.253 (7)C15—C161.342 (8)
C1—C21.444 (7)C15—H150.9300
C1—H10.9300C16—C171.363 (9)
C2—C71.404 (7)C16—H160.9300
C2—C31.430 (7)C17—C181.354 (10)
C3—C41.415 (7)C17—H170.9300
C4—C51.359 (8)C18—H180.9300
C4—H40.9300C19—C201.503 (8)
C5—C61.392 (9)C20—H20A0.9600
C5—H50.9300C20—H20B0.9600
C6—C71.331 (8)C20—H20C0.9600
O3—Co1—O2108.87 (16)C6—C7—C2123.7 (5)
O3—Co1—O194.64 (16)C6—C7—H7118.2
O2—Co1—O181.51 (15)C2—C7—H7118.2
O3—Co1—N1116.64 (17)N1—C8—C9114.3 (5)
O2—Co1—N1133.56 (16)N1—C8—H8A108.7
O1—Co1—N186.05 (15)C9—C8—H8A108.7
O3—Co1—N2101.88 (18)N1—C8—H8B108.7
O2—Co1—N284.91 (17)C9—C8—H8B108.7
O1—Co1—N2161.32 (17)H8A—C8—H8B107.6
N1—Co1—N294.17 (17)C10—C9—C8117.0 (5)
O1—Co2—O1i180.0C10—C9—H9A108.0
O1—Co2—O488.04 (15)C8—C9—H9A108.0
O1i—Co2—O491.96 (15)C10—C9—H9B108.0
O1—Co2—O4i91.96 (15)C8—C9—H9B108.0
O1i—Co2—O4i88.04 (15)H9A—C9—H9B107.3
O4—Co2—O4i180.0C11—C10—C9117.5 (6)
O1—Co2—O277.22 (13)C11—C10—H10A107.9
O1i—Co2—O2102.78 (13)C9—C10—H10A107.9
O4—Co2—O287.67 (14)C11—C10—H10B107.9
O4i—Co2—O292.33 (14)C9—C10—H10B107.9
O1—Co2—O2i102.78 (13)H10A—C10—H10B107.2
O1i—Co2—O2i77.22 (13)C10—C11—N2113.6 (5)
O4—Co2—O2i92.33 (14)C10—C11—H11A108.9
O4i—Co2—O2i87.67 (14)N2—C11—H11A108.9
O2—Co2—O2i180.0C10—C11—H11B108.9
C1—N1—C8117.2 (5)N2—C11—H11B108.9
C1—N1—Co1125.1 (4)H11A—C11—H11B107.7
C8—N1—Co1117.0 (4)N2—C12—C13128.3 (5)
C12—N2—C11117.0 (5)N2—C12—H12115.9
C12—N2—Co1123.8 (4)C13—C12—H12115.9
C11—N2—Co1119.1 (4)C18—C13—C14118.3 (5)
C3—O1—Co1131.3 (3)C18—C13—C12116.9 (5)
C3—O1—Co2134.1 (3)C14—C13—C12124.8 (5)
Co1—O1—Co293.94 (14)O2—C14—C15121.2 (5)
C14—O2—Co1128.3 (3)O2—C14—C13122.1 (5)
C14—O2—Co2136.3 (3)C15—C14—C13116.7 (5)
Co1—O2—Co292.96 (15)C16—C15—C14122.9 (5)
C19—O3—Co1119.4 (4)C16—C15—H15118.6
C19—O4—Co2136.0 (3)C14—C15—H15118.6
N1—C1—C2129.0 (5)C15—C16—C17120.8 (6)
N1—C1—H1115.5C15—C16—H16119.6
C2—C1—H1115.5C17—C16—H16119.6
C7—C2—C3119.2 (5)C18—C17—C16119.1 (6)
C7—C2—C1116.9 (5)C18—C17—H17120.5
C3—C2—C1123.9 (5)C16—C17—H17120.5
O1—C3—C4121.0 (5)C17—C18—C13122.2 (6)
O1—C3—C2123.6 (5)C17—C18—H18118.9
C4—C3—C2115.4 (5)C13—C18—H18118.9
C5—C4—C3122.3 (5)O4—C19—O3125.0 (5)
C5—C4—H4118.9O4—C19—C20117.9 (5)
C3—C4—H4118.9O3—C19—C20117.0 (5)
C4—C5—C6121.5 (6)C19—C20—H20A109.5
C4—C5—H5119.2C19—C20—H20B109.5
C6—C5—H5119.2H20A—C20—H20B109.5
C7—C6—C5117.8 (5)C19—C20—H20C109.5
C7—C6—H6121.1H20A—C20—H20C109.5
C5—C6—H6121.1H20B—C20—H20C109.5
Symmetry code: (i) x+1, y, z+2.
 

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