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
CCDC reference: 608492
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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-µ
3-malonatodicadmium(II)]
top
Crystal data top
[Cd2(C3H2O4)2(H2O)4] | F(000) = 960 |
Mr = 250.48 | Dx = 2.626 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 3478 reflections |
a = 14.680 (3) Å | θ = 2.8–28.2° |
b = 7.2790 (15) Å | µ = 3.42 mm−1 |
c = 13.198 (3) Å | T = 293 K |
β = 116.02 (3)° | Needle, colorless |
V = 1267.3 (4) Å3 | 0.56 × 0.43 × 0.20 mm |
Z = 8 | |
Data collection top
Bruker CCD area detector diffractometer | 1377 independent reflections |
Radiation source: fine-focus sealed tube | 1353 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
φ and ω scans | θmax = 27.0°, θmin = 3.1° |
Absorption correction: multi-scan SADABS, (Bruker 2000) | h = −18→16 |
Tmin = 0.185, Tmax = 0.505 | k = −9→6 |
3478 measured reflections | l = −15→16 |
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)] = 0.030 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.086 | H 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 parameters | Δρmax = 0.75 e Å−3 |
6 restraints | Δρmin = −2.57 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 | 0.7500 | 0.7500 | 0.5000 | 0.02193 (15) | |
Cd2 | 0.5000 | 0.36953 (4) | 0.2500 | 0.02134 (15) | |
O3 | 0.6689 (2) | 0.5972 (3) | 0.3393 (2) | 0.0276 (5) | |
O4 | 0.55013 (19) | 0.6012 (3) | 0.1654 (2) | 0.0307 (5) | |
O1 | 0.6891 (2) | 1.0084 (3) | 0.3904 (2) | 0.0342 (6) | |
O2 | 0.6022 (2) | 1.1477 (3) | 0.2265 (2) | 0.0287 (6) | |
C1 | 0.6511 (2) | 1.0137 (4) | 0.2842 (3) | 0.0203 (6) | |
C2 | 0.6668 (3) | 0.8512 (4) | 0.2204 (3) | 0.0231 (6) | |
H2A | 0.6333 | 0.8768 | 0.1402 | 0.028* | |
H2B | 0.7387 | 0.8373 | 0.2420 | 0.028* | |
O5 | 0.8949 (2) | 0.7616 (6) | 0.4770 (3) | 0.0550 (11) | |
C3 | 0.6259 (2) | 0.6726 (4) | 0.2433 (3) | 0.0189 (6) | |
O6 | 0.4070 (2) | 0.2895 (4) | 0.0569 (2) | 0.0308 (6) | |
H5B | 0.906 (5) | 0.726 (10) | 0.424 (4) | 0.09 (2)* | |
H5A | 0.949 (3) | 0.801 (8) | 0.528 (3) | 0.056 (16)* | |
H6B | 0.364 (3) | 0.205 (5) | 0.047 (4) | 0.047 (14)* | |
H6A | 0.369 (4) | 0.374 (5) | 0.020 (5) | 0.056 (19)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.0221 (2) | 0.0245 (2) | 0.0166 (2) | 0.00195 (11) | 0.00603 (15) | 0.00434 (11) |
Cd2 | 0.0288 (2) | 0.0169 (2) | 0.0207 (2) | 0.000 | 0.01308 (16) | 0.000 |
O3 | 0.0334 (13) | 0.0215 (11) | 0.0229 (12) | −0.0016 (10) | 0.0077 (10) | 0.0034 (9) |
O4 | 0.0296 (12) | 0.0292 (12) | 0.0243 (12) | −0.0089 (10) | 0.0036 (10) | 0.0009 (9) |
O1 | 0.0552 (17) | 0.0231 (12) | 0.0204 (12) | 0.0106 (11) | 0.0128 (12) | 0.0027 (9) |
O2 | 0.0385 (14) | 0.0241 (12) | 0.0258 (12) | 0.0127 (10) | 0.0161 (11) | 0.0072 (9) |
C1 | 0.0222 (14) | 0.0175 (14) | 0.0216 (15) | 0.0001 (11) | 0.0099 (12) | 0.0026 (11) |
C2 | 0.0314 (16) | 0.0186 (14) | 0.0245 (16) | −0.0013 (12) | 0.0172 (14) | −0.0002 (11) |
O5 | 0.0232 (14) | 0.115 (3) | 0.0305 (17) | −0.0164 (16) | 0.0147 (13) | −0.0240 (17) |
C3 | 0.0207 (14) | 0.0160 (13) | 0.0210 (15) | 0.0017 (11) | 0.0101 (12) | 0.0005 (12) |
O6 | 0.0382 (14) | 0.0272 (13) | 0.0254 (13) | −0.0009 (12) | 0.0125 (11) | 0.0003 (11) |
Geometric parameters (Å, º) top
Cd1—O3i | 2.222 (3) | O4—C3 | 1.249 (4) |
Cd1—O3 | 2.222 (3) | O1—C1 | 1.261 (4) |
Cd1—O5 | 2.278 (3) | O2—C1 | 1.252 (4) |
Cd1—O5i | 2.278 (3) | O2—Cd2v | 2.316 (2) |
Cd1—O1i | 2.301 (2) | C1—C2 | 1.528 (4) |
Cd1—O1 | 2.301 (2) | C2—C3 | 1.517 (4) |
Cd2—O4ii | 2.314 (3) | C2—H2A | 0.9700 |
Cd2—O4 | 2.314 (3) | C2—H2B | 0.9700 |
Cd2—O2iii | 2.316 (2) | O5—H5B | 0.83 (2) |
Cd2—O2iv | 2.316 (2) | O5—H5A | 0.836 (19) |
Cd2—O6ii | 2.376 (3) | O6—H6B | 0.842 (19) |
Cd2—O6 | 2.376 (3) | O6—H6A | 0.830 (19) |
O3—C3 | 1.267 (4) | | |
| | | |
O3i—Cd1—O3 | 180.000 (1) | O4—Cd2—O6 | 79.40 (9) |
O3i—Cd1—O5 | 88.17 (11) | O2iii—Cd2—O6 | 82.61 (10) |
O3—Cd1—O5 | 91.83 (11) | O2iv—Cd2—O6 | 77.69 (10) |
O3i—Cd1—O5i | 91.83 (11) | O6ii—Cd2—O6 | 151.61 (14) |
O3—Cd1—O5i | 88.17 (11) | C3—O3—Cd1 | 124.2 (2) |
O5—Cd1—O5i | 180.00 (2) | C3—O4—Cd2 | 105.2 (2) |
O3i—Cd1—O1i | 84.94 (10) | C1—O1—Cd1 | 125.7 (2) |
O3—Cd1—O1i | 95.06 (10) | C1—O2—Cd2v | 133.9 (2) |
O5—Cd1—O1i | 89.20 (13) | O2—C1—O1 | 123.8 (3) |
O5i—Cd1—O1i | 90.80 (13) | O2—C1—C2 | 116.9 (3) |
O3i—Cd1—O1 | 95.06 (10) | O1—C1—C2 | 119.3 (3) |
O3—Cd1—O1 | 84.94 (10) | C3—C2—C1 | 112.7 (3) |
O5—Cd1—O1 | 90.80 (13) | C3—C2—H2A | 109.1 |
O5i—Cd1—O1 | 89.20 (13) | C1—C2—H2A | 109.1 |
O1i—Cd1—O1 | 180.00 (13) | C3—C2—H2B | 109.1 |
O4ii—Cd2—O4 | 86.41 (14) | C1—C2—H2B | 109.1 |
O4ii—Cd2—O2iii | 94.68 (10) | H2A—C2—H2B | 107.8 |
O4—Cd2—O2iii | 159.19 (9) | Cd1—O5—H5B | 130 (4) |
O4ii—Cd2—O2iv | 159.19 (9) | Cd1—O5—H5A | 121 (4) |
O4—Cd2—O2iv | 94.68 (10) | H5B—O5—H5A | 109 (5) |
O2iii—Cd2—O2iv | 91.60 (14) | O4—C3—O3 | 121.1 (3) |
O4ii—Cd2—O6ii | 79.40 (9) | O4—C3—C2 | 118.7 (3) |
O4—Cd2—O6ii | 122.78 (9) | O3—C3—C2 | 120.2 (3) |
O2iii—Cd2—O6ii | 77.69 (10) | Cd2—O6—H6B | 113 (4) |
O2iv—Cd2—O6ii | 82.61 (10) | Cd2—O6—H6A | 112 (4) |
O4ii—Cd2—O6 | 122.78 (9) | H6B—O6—H6A | 101 (4) |
Symmetry codes: (i) −x+3/2, −y+3/2, −z+1; (ii) −x+1, y, −z+1/2; (iii) −x+1, y−1, −z+1/2; (iv) x, y−1, z; (v) x, y+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5B···O2vi | 0.83 (2) | 2.02 (2) | 2.829 (4) | 167 (6) |
O5—H5B···O6vii | 0.83 (2) | 2.69 (6) | 3.138 (4) | 116 (5) |
O5—H5A···O4viii | 0.84 (2) | 1.91 (2) | 2.720 (4) | 164 (5) |
O6—H6B···O1iii | 0.84 (2) | 1.98 (3) | 2.742 (4) | 150 (5) |
O6—H6A···O3ii | 0.83 (2) | 2.70 (6) | 3.077 (4) | 109 (5) |
O6—H6A···O1ix | 0.83 (2) | 2.58 (3) | 3.325 (4) | 150 (5) |
Symmetry codes: (ii) −x+1, y, −z+1/2; (iii) −x+1, y−1, −z+1/2; (vi) −x+3/2, y−1/2, −z+1/2; (vii) −x+3/2, y+1/2, −z+1/2; (viii) x+1/2, −y+3/2, z+1/2; (ix) x−1/2, −y+3/2, z−1/2. |