Buy article online - an online subscription or single-article purchase is required to access this article.
In the title compound {systematic name: bis[2-(acetyloxy)benzoato-κ2O,O′]diaquacadmium(II)}, [Cd(C9H7O4)2(H2O)2], the CdII ion is located on a twofold rotation axis and is coordinated by two water molecules and two aspirinate ligands. The complex is almost isostructural with the corresponding zinc(II) complex. However, for the title compound, the aspirinate should be considered as an asymmetric chelating ligand, with Cd—O(carboxylate) bond lengths of 2.2777 (12) and 2.4121 (12) Å.
Supporting information
CCDC reference: 255422
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.002 Å
- R factor = 0.020
- wR factor = 0.055
- Data-to-parameter ratio = 20.7
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd1 - O1 .. 9.65 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd1 - O5 .. 5.14 su
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXTL-Plus (Sheldrick, 1998); program(s) used to refine structure: SHELXTL-Plus; molecular graphics: SHELXTL-Plus; software used to prepare material for publication: SHELXTL-Plus.
bis[2-(acetyloxy)benzoato-
κ2O,
O']diaquacadmium(II)
top
Crystal data top
[Cd(C9H7O4)2(H2O)2] | F(000) = 1016 |
Mr = 506.72 | Dx = 1.702 Mg m−3 |
Monoclinic, C2/c | Melting point: 563 K |
Hall symbol: -C 2yc | Mo Kα radiation, λ = 0.71073 Å |
a = 26.006 (3) Å | Cell parameters from 56 reflections |
b = 7.3714 (6) Å | θ = 4.5–13.1° |
c = 10.7541 (12) Å | µ = 1.16 mm−1 |
β = 106.416 (8)° | T = 293 K |
V = 1977.6 (3) Å3 | Irregular fragment, colorless |
Z = 4 | 0.6 × 0.4 × 0.2 mm |
Data collection top
Bruker P4 diffractometer | 2763 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube, FN4 | Rint = 0.017 |
Graphite monochromator | θmax = 30.0°, θmin = 2.9° |
2θ/ω scans | h = −36→16 |
Absorption correction: ψ scan (XSCANS; Siemens, 1996) | k = −10→10 |
Tmin = 0.607, Tmax = 0.794 | l = −14→15 |
6264 measured reflections | 3 standard reflections every 97 reflections |
2881 independent reflections | intensity decay: 1% |
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)] = 0.020 | Hydrogen site location: See text |
wR(F2) = 0.055 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | w = 1/[σ2(Fo2) + (0.0309P)2 + 0.8564P] where P = (Fo2 + 2Fc2)/3 |
2881 reflections | (Δ/σ)max = 0.007 |
139 parameters | Δρmax = 0.33 e Å−3 |
0 restraints | Δρmin = −0.58 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 | |
Cd1 | 0.5000 | −0.074578 (18) | 0.2500 | 0.02949 (5) | |
C1 | 0.63734 (5) | 0.19532 (18) | 0.21768 (12) | 0.0283 (2) | |
C2 | 0.67368 (5) | 0.27559 (19) | 0.32526 (13) | 0.0309 (2) | |
C3 | 0.72066 (6) | 0.3548 (2) | 0.31520 (17) | 0.0410 (3) | |
H3A | 0.7444 | 0.4073 | 0.3876 | 0.049* | |
C4 | 0.73212 (7) | 0.3556 (3) | 0.1969 (2) | 0.0463 (4) | |
H4A | 0.7636 | 0.4088 | 0.1898 | 0.056* | |
C5 | 0.69676 (7) | 0.2774 (2) | 0.08938 (17) | 0.0421 (3) | |
H5A | 0.7045 | 0.2780 | 0.0101 | 0.050* | |
C6 | 0.64966 (6) | 0.1980 (2) | 0.09956 (14) | 0.0347 (3) | |
H6A | 0.6261 | 0.1460 | 0.0268 | 0.042* | |
C7 | 0.58667 (6) | 0.10556 (18) | 0.22581 (13) | 0.0287 (2) | |
C8 | 0.62199 (6) | 0.3597 (2) | 0.46456 (14) | 0.0355 (3) | |
C9 | 0.61539 (9) | 0.3239 (3) | 0.59550 (17) | 0.0488 (4) | |
H9A | 0.5946 | 0.4195 | 0.6182 | 0.073* | |
H9B | 0.6500 | 0.3189 | 0.6580 | 0.073* | |
H9C | 0.5973 | 0.2102 | 0.5947 | 0.073* | |
O1 | 0.58593 (5) | 0.02581 (19) | 0.32859 (11) | 0.0428 (3) | |
O2 | 0.54629 (5) | 0.10624 (18) | 0.12861 (11) | 0.0408 (2) | |
O3 | 0.66565 (4) | 0.27252 (16) | 0.44811 (10) | 0.0366 (2) | |
O4 | 0.59350 (6) | 0.45246 (19) | 0.38121 (14) | 0.0499 (3) | |
O5 | 0.48522 (5) | −0.29485 (16) | 0.09816 (11) | 0.0375 (2) | |
H51 | 0.4754 (13) | −0.245 (5) | 0.028 (3) | 0.080* | |
H52 | 0.4625 (14) | −0.374 (5) | 0.107 (3) | 0.080* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.02387 (7) | 0.03119 (8) | 0.03300 (8) | 0.000 | 0.00739 (5) | 0.000 |
C1 | 0.0256 (5) | 0.0273 (5) | 0.0319 (6) | 0.0006 (5) | 0.0079 (5) | 0.0002 (4) |
C2 | 0.0264 (6) | 0.0303 (6) | 0.0344 (6) | 0.0015 (5) | 0.0059 (5) | −0.0007 (5) |
C3 | 0.0268 (6) | 0.0399 (7) | 0.0521 (8) | −0.0040 (6) | 0.0043 (6) | −0.0022 (7) |
C4 | 0.0296 (7) | 0.0467 (9) | 0.0666 (11) | −0.0044 (7) | 0.0201 (7) | 0.0033 (8) |
C5 | 0.0371 (7) | 0.0471 (8) | 0.0488 (8) | 0.0034 (7) | 0.0231 (6) | 0.0035 (7) |
C6 | 0.0329 (7) | 0.0374 (7) | 0.0355 (6) | 0.0002 (6) | 0.0123 (5) | −0.0018 (5) |
C7 | 0.0285 (6) | 0.0280 (5) | 0.0301 (6) | −0.0022 (5) | 0.0091 (5) | −0.0021 (4) |
C8 | 0.0366 (7) | 0.0335 (6) | 0.0358 (6) | −0.0035 (6) | 0.0095 (5) | −0.0060 (5) |
C9 | 0.0563 (10) | 0.0510 (9) | 0.0436 (8) | −0.0100 (8) | 0.0215 (8) | −0.0026 (7) |
O1 | 0.0371 (6) | 0.0527 (6) | 0.0350 (5) | −0.0130 (5) | 0.0043 (4) | 0.0115 (5) |
O2 | 0.0319 (5) | 0.0549 (6) | 0.0320 (5) | −0.0119 (5) | 0.0029 (4) | 0.0052 (5) |
O3 | 0.0328 (5) | 0.0428 (5) | 0.0308 (4) | 0.0009 (4) | 0.0032 (4) | −0.0017 (4) |
O4 | 0.0549 (8) | 0.0507 (7) | 0.0451 (6) | 0.0192 (6) | 0.0155 (6) | 0.0018 (5) |
O5 | 0.0403 (6) | 0.0377 (5) | 0.0334 (5) | −0.0052 (5) | 0.0087 (4) | −0.0012 (4) |
Geometric parameters (Å, º) top
Cd1—O5 | 2.2574 (11) | C4—H4A | 0.9300 |
Cd1—O5i | 2.2574 (11) | C5—C6 | 1.390 (2) |
Cd1—O1 | 2.2777 (12) | C5—H5A | 0.9300 |
Cd1—O1i | 2.2777 (12) | C6—H6A | 0.9300 |
Cd1—O2 | 2.4121 (12) | C7—O2 | 1.2549 (18) |
Cd1—O2i | 2.4121 (12) | C7—O1 | 1.2569 (18) |
C1—C6 | 1.3952 (19) | C8—O4 | 1.202 (2) |
C1—C2 | 1.4013 (18) | C8—O3 | 1.3590 (19) |
C1—C7 | 1.4990 (19) | C8—C9 | 1.489 (2) |
C2—C3 | 1.386 (2) | C9—H9A | 0.9600 |
C2—O3 | 1.3948 (17) | C9—H9B | 0.9600 |
C3—C4 | 1.387 (3) | C9—H9C | 0.9600 |
C3—H3A | 0.9300 | O5—H51 | 0.81 (3) |
C4—C5 | 1.383 (3) | O5—H52 | 0.86 (4) |
| | | |
O5—Cd1—O5i | 88.01 (6) | C4—C5—C6 | 120.16 (15) |
O5—Cd1—O1 | 116.79 (5) | C4—C5—H5A | 119.9 |
O5i—Cd1—O1 | 90.96 (4) | C6—C5—H5A | 119.9 |
O5—Cd1—O1i | 90.96 (4) | C5—C6—C1 | 120.81 (14) |
O5i—Cd1—O1i | 116.79 (5) | C5—C6—H6A | 119.6 |
O1—Cd1—O1i | 142.08 (7) | C1—C6—H6A | 119.6 |
O5—Cd1—O2 | 90.86 (4) | O2—C7—O1 | 121.14 (14) |
O5i—Cd1—O2 | 141.26 (4) | O2—C7—C1 | 119.48 (13) |
O1—Cd1—O2 | 55.52 (4) | O1—C7—C1 | 119.34 (13) |
O1i—Cd1—O2 | 101.95 (5) | O2—C7—Cd1 | 63.64 (8) |
O5—Cd1—O2i | 141.26 (4) | O1—C7—Cd1 | 57.51 (8) |
O5i—Cd1—O2i | 90.86 (4) | C1—C7—Cd1 | 175.95 (10) |
O1—Cd1—O2i | 101.95 (5) | O4—C8—O3 | 122.24 (15) |
O1i—Cd1—O2i | 55.52 (4) | O4—C8—C9 | 126.47 (17) |
O2—Cd1—O2i | 112.91 (7) | O3—C8—C9 | 111.29 (14) |
C6—C1—C2 | 118.08 (13) | C8—C9—H9A | 109.5 |
C6—C1—C7 | 119.42 (12) | C8—C9—H9B | 109.5 |
C2—C1—C7 | 122.49 (12) | H9A—C9—H9B | 109.5 |
C3—C2—O3 | 116.87 (13) | C8—C9—H9C | 109.5 |
C3—C2—C1 | 121.15 (14) | H9A—C9—H9C | 109.5 |
O3—C2—C1 | 121.91 (12) | H9B—C9—H9C | 109.5 |
C2—C3—C4 | 119.76 (15) | C7—O1—Cd1 | 94.75 (9) |
C2—C3—H3A | 120.1 | C7—O2—Cd1 | 88.58 (9) |
C4—C3—H3A | 120.1 | C8—O3—C2 | 118.03 (11) |
C5—C4—C3 | 120.03 (15) | Cd1—O5—H51 | 107 (2) |
C5—C4—H4A | 120.0 | Cd1—O5—H52 | 113 (2) |
C3—C4—H4A | 120.0 | H51—O5—H52 | 111 (3) |
| | | |
C6—C1—C2—C3 | −0.3 (2) | O2—Cd1—C7—O1 | 179.40 (16) |
C7—C1—C2—C3 | 178.87 (14) | O2i—Cd1—C7—O1 | 77.68 (11) |
C6—C1—C2—O3 | −177.32 (13) | C7i—Cd1—C7—O1 | 106.03 (10) |
C7—C1—C2—O3 | 1.8 (2) | O2—C7—O1—Cd1 | 0.63 (16) |
O3—C2—C3—C4 | 177.36 (15) | C1—C7—O1—Cd1 | −177.03 (11) |
C1—C2—C3—C4 | 0.2 (2) | O5—Cd1—O1—C7 | 70.61 (11) |
C2—C3—C4—C5 | −0.1 (3) | O5i—Cd1—O1—C7 | 158.86 (10) |
C3—C4—C5—C6 | 0.1 (3) | O1i—Cd1—O1—C7 | −62.12 (9) |
C4—C5—C6—C1 | −0.2 (3) | O2—Cd1—O1—C7 | −0.34 (9) |
C2—C1—C6—C5 | 0.3 (2) | O2i—Cd1—O1—C7 | −110.06 (10) |
C7—C1—C6—C5 | −178.91 (14) | C7i—Cd1—O1—C7 | −92.01 (12) |
C6—C1—C7—O2 | −31.5 (2) | O1—C7—O2—Cd1 | −0.59 (15) |
C2—C1—C7—O2 | 149.39 (14) | C1—C7—O2—Cd1 | 177.07 (11) |
C6—C1—C7—O1 | 146.23 (15) | O5—Cd1—O2—C7 | −122.11 (9) |
C2—C1—C7—O1 | −32.9 (2) | O5i—Cd1—O2—C7 | −34.22 (13) |
O5—Cd1—C7—O2 | 61.32 (10) | O1—Cd1—O2—C7 | 0.34 (9) |
O5i—Cd1—C7—O2 | 156.81 (9) | O1i—Cd1—O2—C7 | 146.73 (9) |
O1—Cd1—C7—O2 | −179.40 (16) | O2i—Cd1—O2—C7 | 89.33 (9) |
O1i—Cd1—C7—O2 | −40.55 (11) | C7i—Cd1—O2—C7 | 119.04 (10) |
O2i—Cd1—C7—O2 | −101.71 (11) | O4—C8—O3—C2 | −7.3 (2) |
C7i—Cd1—C7—O2 | −73.37 (9) | C9—C8—O3—C2 | 172.71 (13) |
O5—Cd1—C7—O1 | −119.28 (10) | C3—C2—O3—C8 | 119.35 (15) |
O5i—Cd1—C7—O1 | −23.79 (11) | C1—C2—O3—C8 | −63.48 (18) |
O1i—Cd1—C7—O1 | 138.85 (10) | | |
Symmetry code: (i) −x+1, y, −z+1/2. |
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.