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The title linear trinuclear complex, di-μ-acetato-1:2κ
2O,O′;2:3κ
2O,O′-bis{2,2′-[1,4-butanediylbis(nitrilomethylidyne)]diphenolato}-1:2κ
6O,
N,N,O′:
O,O′;2,3κ
6O,O′:
O,
N,N,
O′-tricobalt(II), [Co
3(C
18H
18N
2O
2)
2(C
2H
3O
2)
2], was prepared by the reaction of the tetradentate Schiff base ligand bis(salicylidene)-1,4-diaminobutane and Co(CH
3COO)
2·2H
2O in a methanol solution. The central Co
II 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 Co
II 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 Co
II ions are mutually
trans. The closest Co
Co separation is 3.125 (4) Å.
Supporting information
CCDC reference: 227248
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (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
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-1:2
κ2O:
O';2:3
κ2O:
O'-bis{2,2'-[1,4- butanediylbis(nitrilomethylidyne)]diphenolato}-
1:2
κ6O,
N,
N,
O':
O,
O';2,3
κ6O,
O':
O,
N,
N,
O'-tricobalt(II)
top
Crystal data top
[Co3(C18H18N2O2)2(C2H3O2)2] | F(000) = 910 |
Mr = 883.57 | Dx = 1.506 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2101 reflections |
a = 9.193 (9) Å | θ = 2.5–22.7° |
b = 16.726 (17) Å | µ = 1.32 mm−1 |
c = 12.729 (13) Å | T = 298 K |
β = 95.314 (18)° | Block, red |
V = 1949 (3) Å3 | 0.38 × 0.32 × 0.22 mm |
Z = 2 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 3360 independent reflections |
Radiation source: fine-focus sealed tube | 1992 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.137 |
ω scans | θmax = 25.0°, θmin = 2.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→10 |
Tmin = 0.621, Tmax = 0.745 | k = −19→17 |
9778 measured reflections | l = −15→14 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.070 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.171 | H-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 parameters | Δρmax = 1.04 e Å−3 |
0 restraints | Δρmin = −0.69 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Co1 | 0.29424 (8) | 0.13802 (5) | 0.91226 (6) | 0.0451 (3) | |
Co2 | 0.5000 | 0.0000 | 1.0000 | 0.0421 (3) | |
N1 | 0.0665 (5) | 0.1565 (3) | 0.9367 (4) | 0.0417 (11) | |
N2 | 0.2732 (5) | 0.1890 (3) | 0.7536 (4) | 0.0446 (11) | |
O1 | 0.2971 (4) | 0.0550 (2) | 1.0367 (3) | 0.0380 (9) | |
O2 | 0.4074 (4) | 0.0459 (2) | 0.8445 (3) | 0.0385 (9) | |
O3 | 0.4449 (4) | 0.2153 (2) | 0.9920 (3) | 0.0503 (10) | |
O4 | 0.6056 (4) | 0.1167 (2) | 1.0270 (3) | 0.0443 (9) | |
C1 | −0.0013 (6) | 0.1209 (3) | 1.0048 (4) | 0.0361 (12) | |
H1 | −0.1018 | 0.1292 | 0.9996 | 0.043* | |
C2 | 0.0553 (5) | 0.0690 (3) | 1.0896 (4) | 0.0344 (12) | |
C3 | 0.2005 (5) | 0.0375 (3) | 1.0997 (4) | 0.0335 (12) | |
C4 | 0.2332 (6) | −0.0153 (3) | 1.1855 (4) | 0.0437 (14) | |
H4 | 0.3251 | −0.0390 | 1.1941 | 0.052* | |
C5 | 0.1352 (7) | −0.0326 (4) | 1.2558 (5) | 0.0558 (17) | |
H5 | 0.1624 | −0.0666 | 1.3120 | 0.067* | |
C6 | −0.0052 (6) | −0.0005 (4) | 1.2456 (5) | 0.0510 (15) | |
H6 | −0.0712 | −0.0117 | 1.2948 | 0.061* | |
C7 | −0.0418 (6) | 0.0467 (3) | 1.1633 (5) | 0.0436 (14) | |
H7 | −0.1370 | 0.0659 | 1.1540 | 0.052* | |
C8 | −0.0207 (6) | 0.2057 (4) | 0.8581 (5) | 0.0532 (16) | |
H8A | −0.1225 | 0.2025 | 0.8719 | 0.064* | |
H8B | −0.0124 | 0.1833 | 0.7886 | 0.064* | |
C9 | 0.0236 (7) | 0.2922 (4) | 0.8572 (6) | 0.0601 (17) | |
H9A | −0.0421 | 0.3197 | 0.8052 | 0.072* | |
H9B | 0.0089 | 0.3149 | 0.9255 | 0.072* | |
C10 | 0.1773 (7) | 0.3101 (4) | 0.8340 (5) | 0.0554 (17) | |
H10A | 0.1871 | 0.3676 | 0.8284 | 0.066* | |
H10B | 0.2422 | 0.2930 | 0.8943 | 0.066* | |
C11 | 0.2288 (7) | 0.2741 (3) | 0.7394 (5) | 0.0562 (16) | |
H11A | 0.3114 | 0.3046 | 0.7192 | 0.067* | |
H11B | 0.1517 | 0.2776 | 0.6822 | 0.067* | |
C12 | 0.2887 (6) | 0.1493 (4) | 0.6710 (5) | 0.0458 (14) | |
H12 | 0.2690 | 0.1766 | 0.6077 | 0.055* | |
C13 | 0.3332 (6) | 0.0666 (4) | 0.6625 (4) | 0.0404 (13) | |
C14 | 0.3888 (5) | 0.0185 (3) | 0.7481 (4) | 0.0348 (12) | |
C15 | 0.4265 (6) | −0.0602 (3) | 0.7244 (4) | 0.0459 (14) | |
H15 | 0.4660 | −0.0929 | 0.7789 | 0.055* | |
C16 | 0.4079 (8) | −0.0906 (4) | 0.6265 (5) | 0.0638 (18) | |
H16 | 0.4347 | −0.1432 | 0.6148 | 0.077* | |
C17 | 0.3504 (9) | −0.0452 (5) | 0.5439 (5) | 0.081 (2) | |
H17 | 0.3357 | −0.0669 | 0.4765 | 0.097* | |
C18 | 0.3148 (8) | 0.0319 (4) | 0.5614 (5) | 0.068 (2) | |
H18 | 0.2770 | 0.0629 | 0.5047 | 0.082* | |
C19 | 0.5638 (6) | 0.1876 (3) | 1.0345 (4) | 0.0436 (14) | |
C20 | 0.6621 (7) | 0.2446 (4) | 1.0989 (5) | 0.069 (2) | |
H20A | 0.7194 | 0.2156 | 1.1531 | 0.104* | |
H20B | 0.6039 | 0.2839 | 1.1306 | 0.104* | |
H20C | 0.7258 | 0.2707 | 1.0540 | 0.104* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0472 (5) | 0.0356 (5) | 0.0515 (5) | 0.0088 (3) | −0.0018 (3) | 0.0046 (3) |
Co2 | 0.0407 (6) | 0.0336 (6) | 0.0507 (7) | 0.0081 (5) | −0.0025 (5) | 0.0028 (5) |
N1 | 0.037 (3) | 0.026 (2) | 0.060 (3) | 0.006 (2) | −0.009 (2) | 0.000 (2) |
N2 | 0.050 (3) | 0.033 (3) | 0.050 (3) | 0.007 (2) | −0.005 (2) | 0.017 (2) |
O1 | 0.032 (2) | 0.035 (2) | 0.048 (2) | 0.0109 (16) | 0.0062 (16) | 0.0106 (16) |
O2 | 0.042 (2) | 0.033 (2) | 0.039 (2) | 0.0135 (16) | −0.0043 (15) | 0.0024 (16) |
O3 | 0.042 (2) | 0.037 (2) | 0.069 (3) | 0.0049 (18) | −0.0142 (19) | 0.0033 (19) |
O4 | 0.039 (2) | 0.032 (2) | 0.060 (2) | 0.0034 (17) | −0.0017 (17) | −0.0039 (17) |
C1 | 0.030 (3) | 0.026 (3) | 0.051 (3) | 0.002 (2) | −0.001 (2) | −0.007 (2) |
C2 | 0.031 (3) | 0.029 (3) | 0.043 (3) | −0.006 (2) | 0.000 (2) | −0.013 (2) |
C3 | 0.033 (3) | 0.023 (3) | 0.043 (3) | −0.002 (2) | −0.003 (2) | −0.007 (2) |
C4 | 0.034 (3) | 0.041 (3) | 0.053 (4) | −0.005 (3) | −0.007 (3) | 0.004 (3) |
C5 | 0.062 (4) | 0.050 (4) | 0.053 (4) | −0.022 (3) | −0.011 (3) | 0.014 (3) |
C6 | 0.042 (3) | 0.058 (4) | 0.055 (4) | −0.016 (3) | 0.016 (3) | −0.005 (3) |
C7 | 0.034 (3) | 0.039 (3) | 0.058 (4) | −0.003 (2) | 0.001 (3) | −0.013 (3) |
C8 | 0.043 (3) | 0.047 (4) | 0.067 (4) | 0.009 (3) | −0.010 (3) | 0.017 (3) |
C9 | 0.059 (4) | 0.037 (4) | 0.081 (5) | 0.012 (3) | −0.008 (3) | 0.013 (3) |
C10 | 0.070 (5) | 0.024 (3) | 0.068 (4) | 0.010 (3) | −0.013 (3) | 0.005 (3) |
C11 | 0.073 (4) | 0.032 (3) | 0.063 (4) | 0.011 (3) | 0.002 (3) | 0.019 (3) |
C12 | 0.052 (4) | 0.043 (4) | 0.041 (3) | 0.002 (3) | −0.002 (3) | 0.017 (3) |
C13 | 0.041 (3) | 0.048 (4) | 0.033 (3) | 0.002 (3) | 0.006 (2) | 0.002 (2) |
C14 | 0.024 (3) | 0.035 (3) | 0.044 (3) | 0.000 (2) | −0.001 (2) | −0.003 (2) |
C15 | 0.053 (4) | 0.036 (3) | 0.046 (3) | 0.008 (3) | −0.005 (3) | 0.001 (3) |
C16 | 0.085 (5) | 0.049 (4) | 0.055 (4) | 0.010 (4) | −0.007 (3) | −0.014 (3) |
C17 | 0.118 (6) | 0.074 (6) | 0.047 (4) | 0.012 (5) | −0.006 (4) | −0.022 (4) |
C18 | 0.095 (5) | 0.064 (5) | 0.044 (4) | 0.014 (4) | −0.005 (3) | 0.002 (3) |
C19 | 0.041 (3) | 0.037 (4) | 0.052 (3) | −0.006 (3) | −0.002 (3) | −0.001 (3) |
C20 | 0.072 (5) | 0.039 (4) | 0.090 (5) | −0.002 (3) | −0.028 (4) | −0.003 (3) |
Geometric parameters (Å, º) top
Co1—O3 | 2.088 (4) | C6—H6 | 0.9300 |
Co1—O2 | 2.090 (4) | C7—H7 | 0.9300 |
Co1—O1 | 2.104 (4) | C8—C9 | 1.503 (9) |
Co1—N1 | 2.167 (5) | C8—H8A | 0.9700 |
Co1—N2 | 2.184 (5) | C8—H8B | 0.9700 |
Co2—O1 | 2.170 (4) | C9—C10 | 1.500 (9) |
Co2—O1i | 2.170 (4) | C9—H9A | 0.9700 |
Co2—O4 | 2.193 (4) | C9—H9B | 0.9700 |
Co2—O4i | 2.193 (4) | C10—C11 | 1.464 (9) |
Co2—O2 | 2.218 (4) | C10—H10A | 0.9700 |
Co2—O2i | 2.218 (4) | C10—H10B | 0.9700 |
N1—C1 | 1.264 (7) | C11—H11A | 0.9700 |
N1—C8 | 1.474 (7) | C11—H11B | 0.9700 |
N2—C12 | 1.262 (7) | C12—C13 | 1.449 (8) |
N2—C11 | 1.487 (7) | C12—H12 | 0.9300 |
O1—C3 | 1.284 (6) | C13—C18 | 1.408 (8) |
O2—C14 | 1.307 (6) | C13—C14 | 1.412 (7) |
O3—C19 | 1.262 (6) | C14—C15 | 1.402 (8) |
O4—C19 | 1.253 (7) | C15—C16 | 1.342 (8) |
C1—C2 | 1.444 (7) | C15—H15 | 0.9300 |
C1—H1 | 0.9300 | C16—C17 | 1.363 (9) |
C2—C7 | 1.404 (7) | C16—H16 | 0.9300 |
C2—C3 | 1.430 (7) | C17—C18 | 1.354 (10) |
C3—C4 | 1.415 (7) | C17—H17 | 0.9300 |
C4—C5 | 1.359 (8) | C18—H18 | 0.9300 |
C4—H4 | 0.9300 | C19—C20 | 1.503 (8) |
C5—C6 | 1.392 (9) | C20—H20A | 0.9600 |
C5—H5 | 0.9300 | C20—H20B | 0.9600 |
C6—C7 | 1.331 (8) | C20—H20C | 0.9600 |
| | | |
O3—Co1—O2 | 108.87 (16) | C6—C7—C2 | 123.7 (5) |
O3—Co1—O1 | 94.64 (16) | C6—C7—H7 | 118.2 |
O2—Co1—O1 | 81.51 (15) | C2—C7—H7 | 118.2 |
O3—Co1—N1 | 116.64 (17) | N1—C8—C9 | 114.3 (5) |
O2—Co1—N1 | 133.56 (16) | N1—C8—H8A | 108.7 |
O1—Co1—N1 | 86.05 (15) | C9—C8—H8A | 108.7 |
O3—Co1—N2 | 101.88 (18) | N1—C8—H8B | 108.7 |
O2—Co1—N2 | 84.91 (17) | C9—C8—H8B | 108.7 |
O1—Co1—N2 | 161.32 (17) | H8A—C8—H8B | 107.6 |
N1—Co1—N2 | 94.17 (17) | C10—C9—C8 | 117.0 (5) |
O1—Co2—O1i | 180.0 | C10—C9—H9A | 108.0 |
O1—Co2—O4 | 88.04 (15) | C8—C9—H9A | 108.0 |
O1i—Co2—O4 | 91.96 (15) | C10—C9—H9B | 108.0 |
O1—Co2—O4i | 91.96 (15) | C8—C9—H9B | 108.0 |
O1i—Co2—O4i | 88.04 (15) | H9A—C9—H9B | 107.3 |
O4—Co2—O4i | 180.0 | C11—C10—C9 | 117.5 (6) |
O1—Co2—O2 | 77.22 (13) | C11—C10—H10A | 107.9 |
O1i—Co2—O2 | 102.78 (13) | C9—C10—H10A | 107.9 |
O4—Co2—O2 | 87.67 (14) | C11—C10—H10B | 107.9 |
O4i—Co2—O2 | 92.33 (14) | C9—C10—H10B | 107.9 |
O1—Co2—O2i | 102.78 (13) | H10A—C10—H10B | 107.2 |
O1i—Co2—O2i | 77.22 (13) | C10—C11—N2 | 113.6 (5) |
O4—Co2—O2i | 92.33 (14) | C10—C11—H11A | 108.9 |
O4i—Co2—O2i | 87.67 (14) | N2—C11—H11A | 108.9 |
O2—Co2—O2i | 180.0 | C10—C11—H11B | 108.9 |
C1—N1—C8 | 117.2 (5) | N2—C11—H11B | 108.9 |
C1—N1—Co1 | 125.1 (4) | H11A—C11—H11B | 107.7 |
C8—N1—Co1 | 117.0 (4) | N2—C12—C13 | 128.3 (5) |
C12—N2—C11 | 117.0 (5) | N2—C12—H12 | 115.9 |
C12—N2—Co1 | 123.8 (4) | C13—C12—H12 | 115.9 |
C11—N2—Co1 | 119.1 (4) | C18—C13—C14 | 118.3 (5) |
C3—O1—Co1 | 131.3 (3) | C18—C13—C12 | 116.9 (5) |
C3—O1—Co2 | 134.1 (3) | C14—C13—C12 | 124.8 (5) |
Co1—O1—Co2 | 93.94 (14) | O2—C14—C15 | 121.2 (5) |
C14—O2—Co1 | 128.3 (3) | O2—C14—C13 | 122.1 (5) |
C14—O2—Co2 | 136.3 (3) | C15—C14—C13 | 116.7 (5) |
Co1—O2—Co2 | 92.96 (15) | C16—C15—C14 | 122.9 (5) |
C19—O3—Co1 | 119.4 (4) | C16—C15—H15 | 118.6 |
C19—O4—Co2 | 136.0 (3) | C14—C15—H15 | 118.6 |
N1—C1—C2 | 129.0 (5) | C15—C16—C17 | 120.8 (6) |
N1—C1—H1 | 115.5 | C15—C16—H16 | 119.6 |
C2—C1—H1 | 115.5 | C17—C16—H16 | 119.6 |
C7—C2—C3 | 119.2 (5) | C18—C17—C16 | 119.1 (6) |
C7—C2—C1 | 116.9 (5) | C18—C17—H17 | 120.5 |
C3—C2—C1 | 123.9 (5) | C16—C17—H17 | 120.5 |
O1—C3—C4 | 121.0 (5) | C17—C18—C13 | 122.2 (6) |
O1—C3—C2 | 123.6 (5) | C17—C18—H18 | 118.9 |
C4—C3—C2 | 115.4 (5) | C13—C18—H18 | 118.9 |
C5—C4—C3 | 122.3 (5) | O4—C19—O3 | 125.0 (5) |
C5—C4—H4 | 118.9 | O4—C19—C20 | 117.9 (5) |
C3—C4—H4 | 118.9 | O3—C19—C20 | 117.0 (5) |
C4—C5—C6 | 121.5 (6) | C19—C20—H20A | 109.5 |
C4—C5—H5 | 119.2 | C19—C20—H20B | 109.5 |
C6—C5—H5 | 119.2 | H20A—C20—H20B | 109.5 |
C7—C6—C5 | 117.8 (5) | C19—C20—H20C | 109.5 |
C7—C6—H6 | 121.1 | H20A—C20—H20C | 109.5 |
C5—C6—H6 | 121.1 | H20B—C20—H20C | 109.5 |
Symmetry code: (i) −x+1, −y, −z+2. |
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