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The crystal structure of the title compound, [Cd2(C3H2O4)2(H2O)4]n, was previously reported by Chung, Hong, Do & Moon [J. Chem. Soc. Chem. Commun. (1995), pp. 2333–2335; J. Chem. Soc. Dalton Trans. (1996), pp. 3363–3369]. We present here a new monoclinic polymorph which has a polymeric structure in which one Cd atom lies on an inversion centre and the other on a crystallographic twofold rotation axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680601155X/sj2033sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680601155X/sj2033Isup2.hkl
Contains datablock I

CCDC reference: 608492

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.030
  • wR factor = 0.086
  • Data-to-parameter ratio = 12.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.21 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cd1 PLAT480_ALERT_4_C Long H...A H-Bond Reported H5B .. O6 .. 2.69 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H6A .. O3 .. 2.70 Ang. PLAT731_ALERT_1_C Bond Calc 0.83(6), Rep 0.83(2) ...... 3.00 su-Rat O5 -H5B 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.836(19) ...... 2.11 su-Rat O5 -H5A 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.842(19) ...... 2.11 su-Rat O6 -H6B 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.83(5), Rep 0.830(19) ...... 2.63 su-Rat O6 -H6A 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.83(6), Rep 0.83(2) ...... 3.00 su-Rat O5 -H5B 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.83(6), Rep 0.83(2) ...... 3.00 su-Rat O5 -H5B 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.836(19) ...... 2.11 su-Rat O5 -H5A 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.842(19) ...... 2.11 su-Rat O6 -H6B 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.83(5), Rep 0.830(19) ...... 2.63 su-Rat O6 -H6A 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.83(5), Rep 0.830(19) ...... 2.63 su-Rat O6 -H6A 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 2.02(5), Rep 2.02(2) ...... 2.50 su-Rat H5B -O2 1.555 4.645
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 19 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 15 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.

poly[tetraaquadi-µ3-malonatodicadmium(II)] top
Crystal data top
[Cd2(C3H2O4)2(H2O)4]F(000) = 960
Mr = 250.48Dx = 2.626 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3478 reflections
a = 14.680 (3) Åθ = 2.8–28.2°
b = 7.2790 (15) ŵ = 3.42 mm1
c = 13.198 (3) ÅT = 293 K
β = 116.02 (3)°Needle, colorless
V = 1267.3 (4) Å30.56 × 0.43 × 0.20 mm
Z = 8
Data collection top
Bruker CCD area detector
diffractometer
1377 independent reflections
Radiation source: fine-focus sealed tube1353 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
φ and ω scansθmax = 27.0°, θmin = 3.1°
Absorption correction: multi-scan
SADABS, (Bruker 2000)
h = 1816
Tmin = 0.185, Tmax = 0.505k = 96
3478 measured reflectionsl = 1516
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)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.086H atoms treated by a mixture of independent and constrained refinement
S = 1.24 w = 1/[σ2(Fo2) + (0.054P)2 + 1.7017P]
where P = (Fo2 + 2Fc2)/3
1377 reflections(Δ/σ)max = 0.002
109 parametersΔρmax = 0.75 e Å3
6 restraintsΔρmin = 2.57 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
Cd10.75000.75000.50000.02193 (15)
Cd20.50000.36953 (4)0.25000.02134 (15)
O30.6689 (2)0.5972 (3)0.3393 (2)0.0276 (5)
O40.55013 (19)0.6012 (3)0.1654 (2)0.0307 (5)
O10.6891 (2)1.0084 (3)0.3904 (2)0.0342 (6)
O20.6022 (2)1.1477 (3)0.2265 (2)0.0287 (6)
C10.6511 (2)1.0137 (4)0.2842 (3)0.0203 (6)
C20.6668 (3)0.8512 (4)0.2204 (3)0.0231 (6)
H2A0.63330.87680.14020.028*
H2B0.73870.83730.24200.028*
O50.8949 (2)0.7616 (6)0.4770 (3)0.0550 (11)
C30.6259 (2)0.6726 (4)0.2433 (3)0.0189 (6)
O60.4070 (2)0.2895 (4)0.0569 (2)0.0308 (6)
H5B0.906 (5)0.726 (10)0.424 (4)0.09 (2)*
H5A0.949 (3)0.801 (8)0.528 (3)0.056 (16)*
H6B0.364 (3)0.205 (5)0.047 (4)0.047 (14)*
H6A0.369 (4)0.374 (5)0.020 (5)0.056 (19)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0221 (2)0.0245 (2)0.0166 (2)0.00195 (11)0.00603 (15)0.00434 (11)
Cd20.0288 (2)0.0169 (2)0.0207 (2)0.0000.01308 (16)0.000
O30.0334 (13)0.0215 (11)0.0229 (12)0.0016 (10)0.0077 (10)0.0034 (9)
O40.0296 (12)0.0292 (12)0.0243 (12)0.0089 (10)0.0036 (10)0.0009 (9)
O10.0552 (17)0.0231 (12)0.0204 (12)0.0106 (11)0.0128 (12)0.0027 (9)
O20.0385 (14)0.0241 (12)0.0258 (12)0.0127 (10)0.0161 (11)0.0072 (9)
C10.0222 (14)0.0175 (14)0.0216 (15)0.0001 (11)0.0099 (12)0.0026 (11)
C20.0314 (16)0.0186 (14)0.0245 (16)0.0013 (12)0.0172 (14)0.0002 (11)
O50.0232 (14)0.115 (3)0.0305 (17)0.0164 (16)0.0147 (13)0.0240 (17)
C30.0207 (14)0.0160 (13)0.0210 (15)0.0017 (11)0.0101 (12)0.0005 (12)
O60.0382 (14)0.0272 (13)0.0254 (13)0.0009 (12)0.0125 (11)0.0003 (11)
Geometric parameters (Å, º) top
Cd1—O3i2.222 (3)O4—C31.249 (4)
Cd1—O32.222 (3)O1—C11.261 (4)
Cd1—O52.278 (3)O2—C11.252 (4)
Cd1—O5i2.278 (3)O2—Cd2v2.316 (2)
Cd1—O1i2.301 (2)C1—C21.528 (4)
Cd1—O12.301 (2)C2—C31.517 (4)
Cd2—O4ii2.314 (3)C2—H2A0.9700
Cd2—O42.314 (3)C2—H2B0.9700
Cd2—O2iii2.316 (2)O5—H5B0.83 (2)
Cd2—O2iv2.316 (2)O5—H5A0.836 (19)
Cd2—O6ii2.376 (3)O6—H6B0.842 (19)
Cd2—O62.376 (3)O6—H6A0.830 (19)
O3—C31.267 (4)
O3i—Cd1—O3180.000 (1)O4—Cd2—O679.40 (9)
O3i—Cd1—O588.17 (11)O2iii—Cd2—O682.61 (10)
O3—Cd1—O591.83 (11)O2iv—Cd2—O677.69 (10)
O3i—Cd1—O5i91.83 (11)O6ii—Cd2—O6151.61 (14)
O3—Cd1—O5i88.17 (11)C3—O3—Cd1124.2 (2)
O5—Cd1—O5i180.00 (2)C3—O4—Cd2105.2 (2)
O3i—Cd1—O1i84.94 (10)C1—O1—Cd1125.7 (2)
O3—Cd1—O1i95.06 (10)C1—O2—Cd2v133.9 (2)
O5—Cd1—O1i89.20 (13)O2—C1—O1123.8 (3)
O5i—Cd1—O1i90.80 (13)O2—C1—C2116.9 (3)
O3i—Cd1—O195.06 (10)O1—C1—C2119.3 (3)
O3—Cd1—O184.94 (10)C3—C2—C1112.7 (3)
O5—Cd1—O190.80 (13)C3—C2—H2A109.1
O5i—Cd1—O189.20 (13)C1—C2—H2A109.1
O1i—Cd1—O1180.00 (13)C3—C2—H2B109.1
O4ii—Cd2—O486.41 (14)C1—C2—H2B109.1
O4ii—Cd2—O2iii94.68 (10)H2A—C2—H2B107.8
O4—Cd2—O2iii159.19 (9)Cd1—O5—H5B130 (4)
O4ii—Cd2—O2iv159.19 (9)Cd1—O5—H5A121 (4)
O4—Cd2—O2iv94.68 (10)H5B—O5—H5A109 (5)
O2iii—Cd2—O2iv91.60 (14)O4—C3—O3121.1 (3)
O4ii—Cd2—O6ii79.40 (9)O4—C3—C2118.7 (3)
O4—Cd2—O6ii122.78 (9)O3—C3—C2120.2 (3)
O2iii—Cd2—O6ii77.69 (10)Cd2—O6—H6B113 (4)
O2iv—Cd2—O6ii82.61 (10)Cd2—O6—H6A112 (4)
O4ii—Cd2—O6122.78 (9)H6B—O6—H6A101 (4)
Symmetry codes: (i) x+3/2, y+3/2, z+1; (ii) x+1, y, z+1/2; (iii) x+1, y1, z+1/2; (iv) x, y1, z; (v) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5B···O2vi0.83 (2)2.02 (2)2.829 (4)167 (6)
O5—H5B···O6vii0.83 (2)2.69 (6)3.138 (4)116 (5)
O5—H5A···O4viii0.84 (2)1.91 (2)2.720 (4)164 (5)
O6—H6B···O1iii0.84 (2)1.98 (3)2.742 (4)150 (5)
O6—H6A···O3ii0.83 (2)2.70 (6)3.077 (4)109 (5)
O6—H6A···O1ix0.83 (2)2.58 (3)3.325 (4)150 (5)
Symmetry codes: (ii) x+1, y, z+1/2; (iii) x+1, y1, z+1/2; (vi) x+3/2, y1/2, z+1/2; (vii) x+3/2, y+1/2, z+1/2; (viii) x+1/2, y+3/2, z+1/2; (ix) x1/2, y+3/2, z1/2.
 

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