Buy article online - an online subscription or single-article purchase is required to access this article.
In the title compound, [Cu2(C7H8O3)2(C5H5N)2], each centrosymmetric molecule contains two square-pyramidally coordinated Cu atoms connected to two O atoms from each of the two diacetylacetonate anions. The Cu atoms and the two diacetylacetonate anions are approximately coplanar, and the pyramidal coordination of Cu is completed by pyridine ligands, which coordinate to the two metals on opposite sides of this plane.
Supporting information
CCDC reference: 272010
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C)= 0.002 Å
- R factor = 0.031
- wR factor = 0.080
- Data-to-parameter ratio = 33.4
checkCIF/PLATON results
No syntax errors found
No errors found in this datablock
Data collection: APEXII (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXL97; software used to prepare material for publication: enCIFer (Allen et al., 2004) and WinGX (Farrugia, 1999).
Crystal data top
[Cu2(C7H8O3)2(C5H5N)2] | Z = 1 |
Mr = 565.55 | F(000) = 290 |
Triclinic, P1 | Dx = 1.584 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.4152 (3) Å | Cell parameters from 4210 reflections |
b = 8.7177 (3) Å | θ = 2.6–31.2° |
c = 9.3451 (3) Å | µ = 1.84 mm−1 |
α = 67.769 (2)° | T = 100 K |
β = 87.591 (2)° | Block, light-green |
γ = 69.878 (2)° | 0.10 × 0.08 × 0.05 mm |
V = 592.80 (4) Å3 | |
Data collection top
Bruker SMART APEXII CCD-based diffractometer | 4448 independent reflections |
Radiation source: fine-focus sealed tube, Siemens K FFMO 2K 90 | 3703 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
Detector resolution: 83.33 pixels mm-1 | θmax = 33.1°, θmin = 2.6° |
φ–scans and ω–scans | h = −12→12 |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996). | k = −13→13 |
Tmin = 0.776, Tmax = 0.91 | l = −14→12 |
11199 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)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.080 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0425P)2 + 0.063P] where P = (Fo2 + 2Fc2)/3 |
5141 reflections | (Δ/σ)max = 0.001 |
154 parameters | Δρmax = 0.51 e Å−3 |
0 restraints | Δρmin = −0.50 e Å−3 |
Special details top
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 | |
Cu1 | 0.40605 (2) | 0.64492 (2) | 0.345428 (19) | 0.01356 (5) | |
O1 | 0.24431 (13) | 0.87642 (13) | 0.30392 (13) | 0.0185 (2) | |
O2 | 0.53855 (12) | 0.39395 (13) | 0.43877 (12) | 0.01546 (18) | |
O3 | 0.32206 (13) | 0.62841 (14) | 0.16715 (12) | 0.01750 (19) | |
C1 | 0.1049 (2) | 1.1476 (2) | 0.3296 (2) | 0.0260 (3) | |
H11 | 0.1221 | 1.2130 | 0.2225 | 0.039* | |
H12 | 0.1151 | 1.2096 | 0.3951 | 0.039* | |
H13 | −0.0087 | 1.1398 | 0.3320 | 0.039* | |
C2 | 0.23741 (17) | 0.96355 (18) | 0.38992 (18) | 0.0181 (3) | |
C3 | 0.33629 (18) | 0.90483 (19) | 0.52899 (18) | 0.0195 (3) | |
H3 | 0.3280 | 0.9905 | 0.5711 | 0.023* | |
C4 | 0.55238 (17) | 0.26991 (19) | 0.38676 (17) | 0.0156 (2) | |
C5 | 0.45804 (18) | 0.3141 (2) | 0.24661 (18) | 0.0189 (3) | |
H5 | 0.4687 | 0.2196 | 0.2153 | 0.023* | |
C6 | 0.35099 (17) | 0.4821 (2) | 0.14963 (17) | 0.0173 (3) | |
C7 | 0.2546 (2) | 0.5020 (2) | 0.00769 (18) | 0.0235 (3) | |
H7A | 0.1322 | 0.5447 | 0.0170 | 0.035* | |
H7B | 0.2881 | 0.3869 | −0.0014 | 0.035* | |
H7C | 0.2808 | 0.5872 | −0.0850 | 0.035* | |
N1 | 0.63583 (14) | 0.72275 (16) | 0.27105 (14) | 0.0153 (2) | |
C1A | 0.79548 (18) | 0.6078 (2) | 0.32087 (17) | 0.0194 (3) | |
H1A | 0.8122 | 0.4892 | 0.3888 | 0.023* | |
C1B | 0.93675 (18) | 0.6547 (2) | 0.27746 (18) | 0.0222 (3) | |
H1B | 1.0480 | 0.5702 | 0.3162 | 0.027* | |
C1C | 0.91357 (19) | 0.8269 (2) | 0.17654 (19) | 0.0221 (3) | |
H1C | 1.0086 | 0.8621 | 0.1443 | 0.027* | |
C1D | 0.74917 (19) | 0.9469 (2) | 0.12360 (18) | 0.0199 (3) | |
H1D | 0.7288 | 1.0656 | 0.0540 | 0.024* | |
C1E | 0.61539 (17) | 0.88847 (19) | 0.17522 (16) | 0.0164 (2) | |
H1E | 0.5027 | 0.9711 | 0.1404 | 0.020* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.01303 (8) | 0.01207 (8) | 0.01341 (8) | −0.00308 (6) | −0.00069 (5) | −0.00368 (6) |
O1 | 0.0156 (4) | 0.0154 (5) | 0.0212 (5) | −0.0026 (4) | −0.0012 (4) | −0.0059 (4) |
O2 | 0.0180 (5) | 0.0119 (4) | 0.0151 (5) | −0.0037 (4) | −0.0006 (3) | −0.0049 (4) |
O3 | 0.0174 (5) | 0.0180 (5) | 0.0157 (5) | −0.0055 (4) | −0.0009 (4) | −0.0054 (4) |
C1 | 0.0219 (7) | 0.0165 (7) | 0.0331 (9) | 0.0000 (6) | −0.0028 (6) | −0.0080 (6) |
C2 | 0.0136 (6) | 0.0141 (6) | 0.0243 (7) | −0.0040 (5) | 0.0031 (5) | −0.0059 (5) |
C3 | 0.0196 (6) | 0.0150 (6) | 0.0247 (7) | −0.0041 (5) | 0.0012 (5) | −0.0102 (5) |
C4 | 0.0133 (6) | 0.0169 (6) | 0.0183 (6) | −0.0059 (5) | 0.0040 (5) | −0.0082 (5) |
C5 | 0.0197 (6) | 0.0186 (6) | 0.0211 (7) | −0.0057 (5) | 0.0015 (5) | −0.0115 (6) |
C6 | 0.0136 (6) | 0.0246 (7) | 0.0162 (6) | −0.0079 (5) | 0.0032 (5) | −0.0096 (5) |
C7 | 0.0236 (7) | 0.0292 (8) | 0.0190 (7) | −0.0091 (6) | −0.0010 (5) | −0.0108 (6) |
N1 | 0.0142 (5) | 0.0155 (5) | 0.0154 (5) | −0.0045 (4) | 0.0014 (4) | −0.0060 (4) |
C1A | 0.0157 (6) | 0.0174 (6) | 0.0195 (7) | −0.0038 (5) | 0.0003 (5) | −0.0030 (5) |
C1B | 0.0132 (6) | 0.0253 (7) | 0.0220 (7) | −0.0047 (5) | 0.0001 (5) | −0.0047 (6) |
C1C | 0.0181 (6) | 0.0277 (7) | 0.0222 (7) | −0.0122 (6) | 0.0040 (5) | −0.0081 (6) |
C1D | 0.0200 (6) | 0.0189 (6) | 0.0199 (7) | −0.0088 (5) | 0.0031 (5) | −0.0051 (5) |
C1E | 0.0150 (6) | 0.0168 (6) | 0.0162 (6) | −0.0043 (5) | 0.0010 (5) | −0.0060 (5) |
Geometric parameters (Å, º) top
Cu1—O1 | 1.9074 (10) | C5—H5 | 0.9500 |
Cu1—O3 | 1.9095 (10) | C6—C7 | 1.506 (2) |
Cu1—O2 | 1.9365 (10) | C7—H7A | 0.9800 |
Cu1—O2i | 1.9628 (10) | C7—H7B | 0.9800 |
Cu1—N1 | 2.2617 (12) | C7—H7C | 0.9800 |
O1—C2 | 1.2860 (18) | N1—C1E | 1.3348 (18) |
O2—C4 | 1.3136 (16) | N1—C1A | 1.3413 (18) |
O3—C6 | 1.2864 (18) | C1A—C1B | 1.383 (2) |
C1—C2 | 1.508 (2) | C1A—H1A | 0.9500 |
C1—H11 | 0.9800 | C1B—C1C | 1.387 (2) |
C1—H12 | 0.9800 | C1B—H1B | 0.9500 |
C1—H13 | 0.9800 | C1C—C1D | 1.387 (2) |
C2—C3 | 1.392 (2) | C1C—H1C | 0.9500 |
C3—C4i | 1.411 (2) | C1D—C1E | 1.386 (2) |
C3—H3 | 0.9500 | C1D—H1D | 0.9500 |
C4—C5 | 1.410 (2) | C1E—H1E | 0.9500 |
C5—C6 | 1.390 (2) | | |
| | | |
O1—Cu1—O3 | 93.93 (4) | O2—C4—C3i | 119.29 (13) |
O1—Cu1—O2 | 164.19 (5) | C5—C4—C3i | 121.18 (13) |
O3—Cu1—O2 | 93.44 (4) | C6—C5—C4 | 126.61 (13) |
O1—Cu1—O2i | 92.32 (4) | C6—C5—H5 | 116.7 |
O3—Cu1—O2i | 162.28 (4) | C4—C5—H5 | 116.7 |
O2—Cu1—O2i | 76.77 (5) | O3—C6—C5 | 127.03 (13) |
O1—Cu1—N1 | 97.86 (4) | O3—C6—C7 | 114.08 (13) |
O3—Cu1—N1 | 104.37 (4) | C5—C6—C7 | 118.89 (13) |
O2—Cu1—N1 | 93.83 (4) | C6—C7—H7A | 109.5 |
O2i—Cu1—N1 | 91.16 (4) | C6—C7—H7B | 109.5 |
O1—Cu1—Cu1i | 129.46 (3) | H7A—C7—H7B | 109.5 |
O3—Cu1—Cu1i | 130.52 (3) | C6—C7—H7C | 109.5 |
O2—Cu1—Cu1i | 38.69 (3) | H7A—C7—H7C | 109.5 |
O2i—Cu1—Cu1i | 38.08 (3) | H7B—C7—H7C | 109.5 |
N1—Cu1—Cu1i | 93.17 (3) | C1E—N1—C1A | 117.57 (12) |
C2—O1—Cu1 | 123.71 (9) | C1E—N1—Cu1 | 120.09 (9) |
C4—O2—Cu1 | 128.87 (9) | C1A—N1—Cu1 | 122.34 (10) |
C4—O2—Cu1i | 125.82 (9) | N1—C1A—C1B | 122.76 (14) |
Cu1—O2—Cu1i | 103.23 (5) | N1—C1A—H1A | 118.6 |
C6—O3—Cu1 | 124.27 (9) | C1B—C1A—H1A | 118.6 |
C2—C1—H11 | 109.5 | C1A—C1B—C1C | 119.02 (13) |
C2—C1—H12 | 109.5 | C1A—C1B—H1B | 120.5 |
H11—C1—H12 | 109.5 | C1C—C1B—H1B | 120.5 |
C2—C1—H13 | 109.5 | C1D—C1C—C1B | 118.79 (14) |
H11—C1—H13 | 109.5 | C1D—C1C—H1C | 120.6 |
H12—C1—H13 | 109.5 | C1B—C1C—H1C | 120.6 |
O1—C2—C3 | 127.01 (13) | C1C—C1D—C1E | 118.09 (14) |
O1—C2—C1 | 114.26 (13) | C1C—C1D—H1D | 121.0 |
C3—C2—C1 | 118.72 (13) | C1E—C1D—H1D | 121.0 |
C2—C3—C4i | 126.15 (13) | N1—C1E—C1D | 123.75 (13) |
C2—C3—H3 | 116.9 | N1—C1E—H1E | 118.1 |
C4i—C3—H3 | 116.9 | C1D—C1E—H1E | 118.1 |
O2—C4—C5 | 119.52 (12) | | |
| | | |
O3—Cu1—O1—C2 | −179.85 (11) | Cu1i—O2—C4—C3i | −22.29 (18) |
O2—Cu1—O1—C2 | 62.5 (2) | O2—C4—C5—C6 | 2.2 (2) |
O2i—Cu1—O1—C2 | 16.74 (12) | C3i—C4—C5—C6 | −176.71 (15) |
N1—Cu1—O1—C2 | −74.74 (12) | Cu1—O3—C6—C5 | −6.2 (2) |
Cu1i—Cu1—O1—C2 | 25.97 (13) | Cu1—O3—C6—C7 | 173.38 (10) |
O1—Cu1—O2—C4 | 116.72 (17) | C4—C5—C6—O3 | 2.2 (3) |
O3—Cu1—O2—C4 | −0.96 (12) | C4—C5—C6—C7 | −177.35 (14) |
O2i—Cu1—O2—C4 | 164.08 (14) | O1—Cu1—N1—C1E | −21.24 (11) |
N1—Cu1—O2—C4 | −105.63 (11) | O3—Cu1—N1—C1E | 74.89 (11) |
Cu1i—Cu1—O2—C4 | 164.08 (14) | O2—Cu1—N1—C1E | 169.44 (10) |
O1—Cu1—O2—Cu1i | −47.37 (17) | O2i—Cu1—N1—C1E | −113.74 (11) |
O3—Cu1—O2—Cu1i | −165.05 (5) | Cu1i—Cu1—N1—C1E | −151.80 (10) |
O2i—Cu1—O2—Cu1i | 0.0 | O1—Cu1—N1—C1A | 158.22 (11) |
N1—Cu1—O2—Cu1i | 90.29 (5) | O3—Cu1—N1—C1A | −105.65 (11) |
O1—Cu1—O3—C6 | −161.12 (11) | O2—Cu1—N1—C1A | −11.10 (12) |
O2—Cu1—O3—C6 | 4.88 (11) | O2i—Cu1—N1—C1A | 65.71 (11) |
O2i—Cu1—O3—C6 | −50.73 (19) | Cu1i—Cu1—N1—C1A | 27.66 (11) |
N1—Cu1—O3—C6 | 99.72 (11) | C1E—N1—C1A—C1B | 0.2 (2) |
Cu1i—Cu1—O3—C6 | −7.37 (13) | Cu1—N1—C1A—C1B | −179.24 (12) |
Cu1—O1—C2—C3 | −3.7 (2) | N1—C1A—C1B—C1C | −0.9 (2) |
Cu1—O1—C2—C1 | 176.99 (10) | C1A—C1B—C1C—C1D | 0.6 (2) |
O1—C2—C3—C4i | −9.1 (3) | C1B—C1C—C1D—C1E | 0.4 (2) |
C1—C2—C3—C4i | 170.21 (15) | C1A—N1—C1E—C1D | 0.8 (2) |
Cu1—O2—C4—C5 | −2.03 (19) | Cu1—N1—C1E—C1D | −179.75 (11) |
Cu1i—O2—C4—C5 | 158.75 (10) | C1C—C1D—C1E—N1 | −1.1 (2) |
Cu1—O2—C4—C3i | 176.93 (10) | | |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.