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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804024717/bt6519sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804024717/bt6519Isup2.hkl
Contains datablock I

CCDC reference: 255422

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.020
  • wR factor = 0.055
  • Data-to-parameter ratio = 20.7

checkCIF/PLATON results

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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

Computing details top

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 = 506.72Dx = 1.702 Mg m3
Monoclinic, C2/cMelting point: 563 K
Hall symbol: -C 2ycMo Kα radiation, λ = 0.71073 Å
a = 26.006 (3) ÅCell parameters from 56 reflections
b = 7.3714 (6) Åθ = 4.5–13.1°
c = 10.7541 (12) ŵ = 1.16 mm1
β = 106.416 (8)°T = 293 K
V = 1977.6 (3) Å3Irregular fragment, colorless
Z = 40.6 × 0.4 × 0.2 mm
Data collection top
Bruker P4
diffractometer
2763 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube, FN4Rint = 0.017
Graphite monochromatorθmax = 30.0°, θmin = 2.9°
2θ/ω scansh = 3616
Absorption correction: ψ scan
(XSCANS; Siemens, 1996)
k = 1010
Tmin = 0.607, Tmax = 0.794l = 1415
6264 measured reflections3 standard reflections every 97 reflections
2881 independent reflections intensity decay: 1%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.020Hydrogen site location: See text
wR(F2) = 0.055H 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 parametersΔρmax = 0.33 e Å3
0 restraintsΔρmin = 0.58 e Å3
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
xyzUiso*/Ueq
Cd10.50000.074578 (18)0.25000.02949 (5)
C10.63734 (5)0.19532 (18)0.21768 (12)0.0283 (2)
C20.67368 (5)0.27559 (19)0.32526 (13)0.0309 (2)
C30.72066 (6)0.3548 (2)0.31520 (17)0.0410 (3)
H3A0.74440.40730.38760.049*
C40.73212 (7)0.3556 (3)0.1969 (2)0.0463 (4)
H4A0.76360.40880.18980.056*
C50.69676 (7)0.2774 (2)0.08938 (17)0.0421 (3)
H5A0.70450.27800.01010.050*
C60.64966 (6)0.1980 (2)0.09956 (14)0.0347 (3)
H6A0.62610.14600.02680.042*
C70.58667 (6)0.10556 (18)0.22581 (13)0.0287 (2)
C80.62199 (6)0.3597 (2)0.46456 (14)0.0355 (3)
C90.61539 (9)0.3239 (3)0.59550 (17)0.0488 (4)
H9A0.59460.41950.61820.073*
H9B0.65000.31890.65800.073*
H9C0.59730.21020.59470.073*
O10.58593 (5)0.02581 (19)0.32859 (11)0.0428 (3)
O20.54629 (5)0.10624 (18)0.12861 (11)0.0408 (2)
O30.66565 (4)0.27252 (16)0.44811 (10)0.0366 (2)
O40.59350 (6)0.45246 (19)0.38121 (14)0.0499 (3)
O50.48522 (5)0.29485 (16)0.09816 (11)0.0375 (2)
H510.4754 (13)0.245 (5)0.028 (3)0.080*
H520.4625 (14)0.374 (5)0.107 (3)0.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.02387 (7)0.03119 (8)0.03300 (8)0.0000.00739 (5)0.000
C10.0256 (5)0.0273 (5)0.0319 (6)0.0006 (5)0.0079 (5)0.0002 (4)
C20.0264 (6)0.0303 (6)0.0344 (6)0.0015 (5)0.0059 (5)0.0007 (5)
C30.0268 (6)0.0399 (7)0.0521 (8)0.0040 (6)0.0043 (6)0.0022 (7)
C40.0296 (7)0.0467 (9)0.0666 (11)0.0044 (7)0.0201 (7)0.0033 (8)
C50.0371 (7)0.0471 (8)0.0488 (8)0.0034 (7)0.0231 (6)0.0035 (7)
C60.0329 (7)0.0374 (7)0.0355 (6)0.0002 (6)0.0123 (5)0.0018 (5)
C70.0285 (6)0.0280 (5)0.0301 (6)0.0022 (5)0.0091 (5)0.0021 (4)
C80.0366 (7)0.0335 (6)0.0358 (6)0.0035 (6)0.0095 (5)0.0060 (5)
C90.0563 (10)0.0510 (9)0.0436 (8)0.0100 (8)0.0215 (8)0.0026 (7)
O10.0371 (6)0.0527 (6)0.0350 (5)0.0130 (5)0.0043 (4)0.0115 (5)
O20.0319 (5)0.0549 (6)0.0320 (5)0.0119 (5)0.0029 (4)0.0052 (5)
O30.0328 (5)0.0428 (5)0.0308 (4)0.0009 (4)0.0032 (4)0.0017 (4)
O40.0549 (8)0.0507 (7)0.0451 (6)0.0192 (6)0.0155 (6)0.0018 (5)
O50.0403 (6)0.0377 (5)0.0334 (5)0.0052 (5)0.0087 (4)0.0012 (4)
Geometric parameters (Å, º) top
Cd1—O52.2574 (11)C4—H4A0.9300
Cd1—O5i2.2574 (11)C5—C61.390 (2)
Cd1—O12.2777 (12)C5—H5A0.9300
Cd1—O1i2.2777 (12)C6—H6A0.9300
Cd1—O22.4121 (12)C7—O21.2549 (18)
Cd1—O2i2.4121 (12)C7—O11.2569 (18)
C1—C61.3952 (19)C8—O41.202 (2)
C1—C21.4013 (18)C8—O31.3590 (19)
C1—C71.4990 (19)C8—C91.489 (2)
C2—C31.386 (2)C9—H9A0.9600
C2—O31.3948 (17)C9—H9B0.9600
C3—C41.387 (3)C9—H9C0.9600
C3—H3A0.9300O5—H510.81 (3)
C4—C51.383 (3)O5—H520.86 (4)
O5—Cd1—O5i88.01 (6)C4—C5—C6120.16 (15)
O5—Cd1—O1116.79 (5)C4—C5—H5A119.9
O5i—Cd1—O190.96 (4)C6—C5—H5A119.9
O5—Cd1—O1i90.96 (4)C5—C6—C1120.81 (14)
O5i—Cd1—O1i116.79 (5)C5—C6—H6A119.6
O1—Cd1—O1i142.08 (7)C1—C6—H6A119.6
O5—Cd1—O290.86 (4)O2—C7—O1121.14 (14)
O5i—Cd1—O2141.26 (4)O2—C7—C1119.48 (13)
O1—Cd1—O255.52 (4)O1—C7—C1119.34 (13)
O1i—Cd1—O2101.95 (5)O2—C7—Cd163.64 (8)
O5—Cd1—O2i141.26 (4)O1—C7—Cd157.51 (8)
O5i—Cd1—O2i90.86 (4)C1—C7—Cd1175.95 (10)
O1—Cd1—O2i101.95 (5)O4—C8—O3122.24 (15)
O1i—Cd1—O2i55.52 (4)O4—C8—C9126.47 (17)
O2—Cd1—O2i112.91 (7)O3—C8—C9111.29 (14)
C6—C1—C2118.08 (13)C8—C9—H9A109.5
C6—C1—C7119.42 (12)C8—C9—H9B109.5
C2—C1—C7122.49 (12)H9A—C9—H9B109.5
C3—C2—O3116.87 (13)C8—C9—H9C109.5
C3—C2—C1121.15 (14)H9A—C9—H9C109.5
O3—C2—C1121.91 (12)H9B—C9—H9C109.5
C2—C3—C4119.76 (15)C7—O1—Cd194.75 (9)
C2—C3—H3A120.1C7—O2—Cd188.58 (9)
C4—C3—H3A120.1C8—O3—C2118.03 (11)
C5—C4—C3120.03 (15)Cd1—O5—H51107 (2)
C5—C4—H4A120.0Cd1—O5—H52113 (2)
C3—C4—H4A120.0H51—O5—H52111 (3)
C6—C1—C2—C30.3 (2)O2—Cd1—C7—O1179.40 (16)
C7—C1—C2—C3178.87 (14)O2i—Cd1—C7—O177.68 (11)
C6—C1—C2—O3177.32 (13)C7i—Cd1—C7—O1106.03 (10)
C7—C1—C2—O31.8 (2)O2—C7—O1—Cd10.63 (16)
O3—C2—C3—C4177.36 (15)C1—C7—O1—Cd1177.03 (11)
C1—C2—C3—C40.2 (2)O5—Cd1—O1—C770.61 (11)
C2—C3—C4—C50.1 (3)O5i—Cd1—O1—C7158.86 (10)
C3—C4—C5—C60.1 (3)O1i—Cd1—O1—C762.12 (9)
C4—C5—C6—C10.2 (3)O2—Cd1—O1—C70.34 (9)
C2—C1—C6—C50.3 (2)O2i—Cd1—O1—C7110.06 (10)
C7—C1—C6—C5178.91 (14)C7i—Cd1—O1—C792.01 (12)
C6—C1—C7—O231.5 (2)O1—C7—O2—Cd10.59 (15)
C2—C1—C7—O2149.39 (14)C1—C7—O2—Cd1177.07 (11)
C6—C1—C7—O1146.23 (15)O5—Cd1—O2—C7122.11 (9)
C2—C1—C7—O132.9 (2)O5i—Cd1—O2—C734.22 (13)
O5—Cd1—C7—O261.32 (10)O1—Cd1—O2—C70.34 (9)
O5i—Cd1—C7—O2156.81 (9)O1i—Cd1—O2—C7146.73 (9)
O1—Cd1—C7—O2179.40 (16)O2i—Cd1—O2—C789.33 (9)
O1i—Cd1—C7—O240.55 (11)C7i—Cd1—O2—C7119.04 (10)
O2i—Cd1—C7—O2101.71 (11)O4—C8—O3—C27.3 (2)
C7i—Cd1—C7—O273.37 (9)C9—C8—O3—C2172.71 (13)
O5—Cd1—C7—O1119.28 (10)C3—C2—O3—C8119.35 (15)
O5i—Cd1—C7—O123.79 (11)C1—C2—O3—C863.48 (18)
O1i—Cd1—C7—O1138.85 (10)
Symmetry code: (i) x+1, y, z+1/2.
 

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