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The crystal structure of the title compound, [Pd(C
5H
7O
2)
2], has been redetermined at 100 K using modern equipment, resulting in improved precision compared to the previous study [Knyazeva
et al. (1970).
Zh. Strukt. Khim. 11, 938-939]. The new measurements reveal that the plane of the 2,4-pentanedionate ligand is tilted by 3.4 (1)° with respect to the PdO
4 unit (Pd site symmetry =
). Possible reasons for this bending are examined in terms of previously undiscussed intermolecular interactions.
Supporting information
CCDC reference: 289749
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.002 Å
- R factor = 0.024
- wR factor = 0.068
- Data-to-parameter ratio = 22.0
checkCIF/PLATON results
No syntax errors found
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
Tmin and Tmax reported: 0.453 0.650
Tmin and Tmax expected: 0.368 0.650
RR = 1.230
Please check that your absorption correction is appropriate.
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.23
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
2 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
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2002); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; 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.
bis(2,4-pentanedionato)palladium(II)
top
Crystal data top
[Pd(C5H7O2)2] | F(000) = 304 |
Mr = 304.61 | Dx = 1.891 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 4907 reflections |
a = 9.9119 (10) Å | θ = 3.0–30.2° |
b = 5.2232 (5) Å | µ = 1.73 mm−1 |
c = 10.3877 (10) Å | T = 100 K |
β = 95.807 (2)° | Block, orange |
V = 535.03 (9) Å3 | 0.60 × 0.55 × 0.25 mm |
Z = 2 | |
Data collection top
Bruker SMART APEX CCD diffractometer | 1581 independent reflections |
Radiation source: fine-focus sealed tube | 1457 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
ω scans | θmax = 30.2°, θmin = 3.9° |
Absorption correction: multi-scan (SADABS in SAINT-Plus; Bruker, 2003) | h = −14→13 |
Tmin = 0.453, Tmax = 0.65 | k = −7→7 |
5832 measured reflections | l = −14→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)] = 0.024 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.068 | H-atom parameters constrained |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0402P)2 + 0.24P] where P = (Fo2 + 2Fc2)/3 |
1581 reflections | (Δ/σ)max < 0.001 |
72 parameters | Δρmax = 1.23 e Å−3 |
0 restraints | Δρmin = −1.73 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 | |
Pd1 | 0.0000 | 0.0000 | 0.0000 | 0.01332 (8) | |
O2 | 0.16908 (10) | 0.2016 (2) | −0.00239 (10) | 0.0177 (2) | |
O1 | −0.06801 (10) | 0.1940 (2) | 0.14436 (10) | 0.0179 (2) | |
C2 | −0.00692 (14) | 0.3901 (3) | 0.19495 (13) | 0.0165 (3) | |
C4 | 0.19486 (14) | 0.3966 (3) | 0.06983 (13) | 0.0165 (3) | |
C3 | 0.1164 (2) | 0.4891 (2) | 0.1640 (2) | 0.0169 (4) | |
H3 | 0.1505 | 0.6343 | 0.2119 | 0.020* | |
C1 | −0.0787 (2) | 0.5240 (3) | 0.2962 (2) | 0.0206 (4) | |
H1A | −0.1572 | 0.4220 | 0.3156 | 0.031* | |
H1B | −0.1094 | 0.6927 | 0.2641 | 0.031* | |
H1C | −0.0165 | 0.5445 | 0.3750 | 0.031* | |
C5 | 0.3224 (2) | 0.5367 (4) | 0.0475 (2) | 0.0203 (3) | |
H5A | 0.3867 | 0.5266 | 0.1255 | 0.030* | |
H5B | 0.3012 | 0.7165 | 0.0276 | 0.030* | |
H5C | 0.3629 | 0.4584 | −0.0253 | 0.030* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pd1 | 0.01223 (11) | 0.01361 (12) | 0.01494 (12) | −0.00067 (4) | 0.00536 (7) | −0.00084 (4) |
O2 | 0.0159 (4) | 0.0172 (5) | 0.0210 (5) | −0.0024 (4) | 0.0066 (4) | −0.0020 (4) |
O1 | 0.0173 (4) | 0.0181 (5) | 0.0195 (5) | −0.0013 (4) | 0.0078 (4) | −0.0029 (4) |
C2 | 0.0175 (6) | 0.0171 (6) | 0.0153 (6) | 0.0019 (5) | 0.0033 (5) | 0.0013 (5) |
C4 | 0.0145 (6) | 0.0176 (7) | 0.0176 (6) | −0.0004 (5) | 0.0024 (4) | 0.0022 (5) |
C3 | 0.0173 (9) | 0.0166 (9) | 0.0172 (9) | −0.0014 (4) | 0.0030 (7) | −0.0016 (4) |
C1 | 0.0212 (9) | 0.0233 (8) | 0.0186 (8) | 0.0004 (5) | 0.0092 (7) | −0.0038 (5) |
C5 | 0.0135 (7) | 0.0236 (7) | 0.0247 (8) | −0.0046 (6) | 0.0057 (6) | −0.0015 (7) |
Geometric parameters (Å, º) top
Pd1—O2 | 1.9815 (10) | C4—C5 | 1.499 (2) |
Pd1—O2i | 1.9816 (10) | C3—H3 | 0.9500 |
Pd1—O1 | 1.9837 (10) | C1—H1A | 0.9800 |
Pd1—O1i | 1.9837 (10) | C1—H1B | 0.9800 |
O2—C4 | 1.2755 (18) | C1—H1C | 0.9800 |
O1—C2 | 1.2757 (18) | C5—H5A | 0.9800 |
C2—C3 | 1.394 (3) | C5—H5B | 0.9800 |
C2—C1 | 1.501 (2) | C5—H5C | 0.9800 |
C4—C3 | 1.396 (3) | | |
| | | |
O2—Pd1—O2i | 180.0 | C2—C3—H3 | 116.7 |
O2—Pd1—O1 | 95.19 (4) | C4—C3—H3 | 116.7 |
O2i—Pd1—O1 | 84.81 (4) | C2—C1—H1A | 109.5 |
O2—Pd1—O1i | 84.81 (4) | C2—C1—H1B | 109.5 |
O2i—Pd1—O1i | 95.19 (4) | H1A—C1—H1B | 109.5 |
O1—Pd1—O1i | 180.0 | C2—C1—H1C | 109.5 |
C4—O2—Pd1 | 122.44 (9) | H1A—C1—H1C | 109.5 |
C2—O1—Pd1 | 122.56 (9) | H1B—C1—H1C | 109.5 |
O1—C2—C3 | 126.41 (14) | C4—C5—H5A | 109.5 |
O1—C2—C1 | 115.06 (13) | C4—C5—H5B | 109.5 |
C3—C2—C1 | 118.53 (15) | H5A—C5—H5B | 109.5 |
O2—C4—C3 | 126.58 (14) | C4—C5—H5C | 109.5 |
O2—C4—C5 | 114.87 (13) | H5A—C5—H5C | 109.5 |
C3—C4—C5 | 118.55 (15) | H5B—C5—H5C | 109.5 |
C2—C3—C4 | 126.62 (15) | | |
Symmetry code: (i) −x, −y, −z. |
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