In the title dimeric complex, [Cu
2(Ac)
4(3-PyOH)
2] or [Cu
2(C
2H
3O
2)
4(C
5H
5NO)
2] (Ac
− is acetate and PyOH is hydroxypyridine), each Cu
II atom exists in a square pyramidal coordination environment, defined by four different acetate O atoms and one 3-hydroxypyridine N atom. Two Cu
II atoms are bridged by four acetate groups, and the center of the dimer corresponds to a crystallographic center of symmetry, the Cu
Cu separation being 2.6598 (8) Å. These dimeric units are linked
via O—H
O hydrogen bonds into a two-dimensional layer supramolecular network.
Supporting information
CCDC reference: 252762
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.043
- wR factor = 0.095
- Data-to-parameter ratio = 17.1
checkCIF/PLATON results
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Data collection: RAPID-AUTO (Rigaku Corporation, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC & Rigaku Corporation, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: SHELXL97.
Tetrakis(µ-acetato-
κ2O:
O')bis[(3-hydroxypyridine-
κN)copper]
top
Crystal data top
[Cu2(C2H3O2)4(C5H5NO)2] | F(000) = 1128 |
Mr = 553.48 | Dx = 1.638 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 15896 reflections |
a = 13.248 (3) Å | θ = 3.0–27.4° |
b = 8.5327 (17) Å | µ = 1.95 mm−1 |
c = 19.858 (4) Å | T = 293 K |
V = 2244.8 (8) Å3 | Prism, green |
Z = 4 | 0.38 × 0.25 × 0.17 mm |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 2566 independent reflections |
Radiation source: fine-focus sealed tube | 1880 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.068 |
Detector resolution: 10 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω scan | h = −17→17 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −10→11 |
Tmin = 0.514, Tmax = 0.718 | l = −25→25 |
19830 measured reflections | |
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.095 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0484P)2 + 0.9981P] where P = (Fo2 + 2Fc2)/3 |
2566 reflections | (Δ/σ)max = 0.001 |
150 parameters | Δρmax = 0.45 e Å−3 |
1 restraint | Δρmin = −0.27 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cu1 | 0.46588 (3) | 0.57742 (4) | 0.553482 (17) | 0.02836 (13) | |
O1 | 0.43930 (17) | 0.3640 (2) | 0.59143 (11) | 0.0364 (5) | |
O2 | 0.50073 (19) | 0.2382 (3) | 0.50239 (13) | 0.0438 (6) | |
O3 | 0.60826 (17) | 0.5622 (3) | 0.58185 (12) | 0.0441 (5) | |
O4 | 0.66597 (16) | 0.4371 (3) | 0.49159 (11) | 0.0443 (6) | |
O5 | 0.17909 (18) | 0.8760 (4) | 0.70393 (12) | 0.0550 (7) | |
H10 | 0.150 (3) | 0.868 (5) | 0.6661 (12) | 0.082* | |
N1 | 0.41258 (18) | 0.7045 (3) | 0.64076 (12) | 0.0304 (5) | |
C1 | 0.4401 (3) | 0.0869 (4) | 0.5930 (2) | 0.0516 (10) | |
H1A | 0.3693 | 0.0645 | 0.5895 | 0.077* | |
H1B | 0.4589 | 0.0923 | 0.6396 | 0.077* | |
H1C | 0.4779 | 0.0053 | 0.5712 | 0.077* | |
C2 | 0.4621 (2) | 0.2404 (4) | 0.55967 (17) | 0.0340 (7) | |
C3 | 0.7839 (3) | 0.5146 (5) | 0.5741 (2) | 0.0577 (10) | |
H3A | 0.7828 | 0.5575 | 0.6188 | 0.087* | |
H3B | 0.8233 | 0.5810 | 0.5453 | 0.087* | |
H3C | 0.8131 | 0.4117 | 0.5752 | 0.087* | |
C4 | 0.6773 (2) | 0.5045 (4) | 0.54738 (17) | 0.0356 (7) | |
C5 | 0.3159 (2) | 0.7524 (3) | 0.64454 (15) | 0.0331 (7) | |
H5 | 0.2737 | 0.7332 | 0.6080 | 0.040* | |
C6 | 0.2763 (2) | 0.8284 (4) | 0.69975 (16) | 0.0364 (7) | |
C7 | 0.3393 (3) | 0.8580 (5) | 0.75372 (18) | 0.0534 (9) | |
H7 | 0.3154 | 0.9089 | 0.7919 | 0.064* | |
C8 | 0.4382 (3) | 0.8103 (5) | 0.74950 (19) | 0.0581 (11) | |
H8 | 0.4822 | 0.8295 | 0.7850 | 0.070* | |
C9 | 0.4720 (3) | 0.7347 (4) | 0.69304 (18) | 0.0436 (8) | |
H9 | 0.5392 | 0.7032 | 0.6912 | 0.052* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.02673 (19) | 0.02873 (19) | 0.02960 (19) | −0.00019 (16) | 0.00466 (15) | −0.00100 (16) |
O1 | 0.0437 (13) | 0.0298 (10) | 0.0356 (12) | −0.0036 (10) | 0.0095 (10) | 0.0019 (10) |
O2 | 0.0596 (14) | 0.0297 (11) | 0.0421 (13) | −0.0017 (11) | 0.0193 (11) | 0.0013 (10) |
O3 | 0.0289 (11) | 0.0579 (15) | 0.0455 (12) | −0.0027 (11) | −0.0001 (11) | −0.0075 (12) |
O4 | 0.0315 (12) | 0.0571 (14) | 0.0444 (13) | 0.0076 (11) | −0.0020 (10) | −0.0074 (12) |
O5 | 0.0375 (14) | 0.0841 (19) | 0.0433 (14) | 0.0201 (13) | −0.0006 (11) | −0.0128 (14) |
N1 | 0.0275 (13) | 0.0324 (13) | 0.0314 (13) | −0.0004 (10) | 0.0017 (11) | 0.0009 (11) |
C1 | 0.065 (2) | 0.0292 (17) | 0.060 (2) | −0.0001 (17) | 0.0207 (19) | 0.0096 (17) |
C2 | 0.0320 (15) | 0.0295 (15) | 0.0406 (18) | −0.0017 (13) | 0.0019 (14) | 0.0027 (14) |
C3 | 0.0276 (18) | 0.088 (3) | 0.058 (2) | −0.0026 (19) | −0.0021 (16) | 0.001 (2) |
C4 | 0.0277 (15) | 0.0382 (16) | 0.0410 (17) | −0.0040 (14) | 0.0005 (14) | 0.0034 (15) |
C5 | 0.0304 (16) | 0.0387 (16) | 0.0302 (15) | −0.0043 (13) | −0.0013 (13) | −0.0009 (13) |
C6 | 0.0331 (17) | 0.0420 (18) | 0.0340 (15) | 0.0043 (15) | 0.0028 (13) | −0.0014 (15) |
C7 | 0.050 (2) | 0.077 (2) | 0.0336 (17) | 0.011 (2) | −0.0015 (16) | −0.0175 (19) |
C8 | 0.047 (2) | 0.086 (3) | 0.041 (2) | 0.012 (2) | −0.0147 (17) | −0.018 (2) |
C9 | 0.0317 (16) | 0.055 (2) | 0.0439 (19) | 0.0088 (16) | −0.0025 (16) | −0.0034 (17) |
Geometric parameters (Å, º) top
Cu1—Cu1i | 2.6598 (8) | C1—H1A | 0.9600 |
Cu1—O4i | 1.967 (2) | C1—H1B | 0.9600 |
Cu1—O3 | 1.973 (2) | C1—H1C | 0.9600 |
Cu1—O2i | 1.976 (2) | C3—C4 | 1.511 (5) |
Cu1—O1 | 2.002 (2) | C3—H3A | 0.9600 |
Cu1—N1 | 2.163 (2) | C3—H3B | 0.9600 |
N1—C9 | 1.328 (4) | C3—H3C | 0.9600 |
N1—C5 | 1.346 (4) | C5—C6 | 1.378 (4) |
O1—C2 | 1.265 (4) | C5—H5 | 0.9300 |
O2—C2 | 1.247 (4) | C6—C7 | 1.381 (5) |
O3—C4 | 1.244 (4) | C7—C8 | 1.374 (5) |
O4—C4 | 1.257 (4) | C7—H7 | 0.9300 |
O5—C6 | 1.353 (4) | C8—C9 | 1.369 (5) |
O5—H10 | 0.85 (3) | C8—H8 | 0.9300 |
C1—C2 | 1.496 (4) | C9—H9 | 0.9300 |
| | | |
O4i—Cu1—O3 | 167.17 (9) | H1B—C1—H1C | 109.5 |
O4i—Cu1—O2i | 89.62 (11) | O2—C2—O1 | 124.4 (3) |
O3—Cu1—O2i | 89.92 (11) | O2—C2—C1 | 118.0 (3) |
O4i—Cu1—O1 | 87.58 (10) | O1—C2—C1 | 117.5 (3) |
O3—Cu1—O1 | 90.05 (9) | C4—C3—H3A | 109.5 |
O2i—Cu1—O1 | 167.23 (9) | C4—C3—H3B | 109.5 |
O4i—Cu1—N1 | 96.10 (9) | H3A—C3—H3B | 109.5 |
O3—Cu1—N1 | 96.68 (9) | C4—C3—H3C | 109.5 |
O2i—Cu1—N1 | 97.12 (9) | H3A—C3—H3C | 109.5 |
O1—Cu1—N1 | 95.56 (9) | H3B—C3—H3C | 109.5 |
O4i—Cu1—Cu1i | 84.67 (7) | O3—C4—O4 | 125.3 (3) |
O3—Cu1—Cu1i | 82.56 (7) | O3—C4—C3 | 118.1 (3) |
O2i—Cu1—Cu1i | 82.59 (7) | O4—C4—C3 | 116.6 (3) |
O1—Cu1—Cu1i | 84.75 (6) | N1—C5—C6 | 123.3 (3) |
N1—Cu1—Cu1i | 179.18 (7) | N1—C5—H5 | 118.3 |
C2—O1—Cu1 | 121.9 (2) | C6—C5—H5 | 118.3 |
C2—O2—Cu1i | 126.3 (2) | O5—C6—C5 | 123.5 (3) |
C4—O3—Cu1 | 124.9 (2) | O5—C6—C7 | 118.2 (3) |
C4—O4—Cu1i | 122.4 (2) | C5—C6—C7 | 118.3 (3) |
C6—O5—H10 | 111 (3) | C8—C7—C6 | 118.3 (3) |
C9—N1—C5 | 117.5 (3) | C8—C7—H7 | 120.9 |
C9—N1—Cu1 | 122.0 (2) | C6—C7—H7 | 120.9 |
C5—N1—Cu1 | 120.49 (19) | C9—C8—C7 | 120.1 (3) |
C2—C1—H1A | 109.5 | C9—C8—H8 | 119.9 |
C2—C1—H1B | 109.5 | C7—C8—H8 | 119.9 |
H1A—C1—H1B | 109.5 | N1—C9—C8 | 122.5 (3) |
C2—C1—H1C | 109.5 | N1—C9—H9 | 118.7 |
H1A—C1—H1C | 109.5 | C8—C9—H9 | 118.7 |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H10···O1ii | 0.85 (3) | 1.90 (3) | 2.732 (3) | 168 (5) |
Symmetry code: (ii) −x+1/2, y+1/2, z. |