The title compound, [Cd(C
4H
3O
4)
2(H
2O)
4], crystallizes in the centrosymmetric space group
P with the Cd atom occupying an inversion centre and the monodentate hydrogen maleate anions arranged in a
trans configuration. A network of intra- and intermolecular O—H
O bonds helps to stabilize the crystal packing.
Supporting information
CCDC reference: 270330
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.019
- wR factor = 0.049
- Data-to-parameter ratio = 11.4
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT052_ALERT_1_A (Proper) Absorption Correction Method Missing .. ?
PLAT057_ALERT_3_A Correction for Absorption Required RT(exp) ... 1.58
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98
PLAT354_ALERT_3_C Short O-H Bond (0.82A) O5 - H2O5 ... 0.70 Ang.
PLAT354_ALERT_3_C Short O-H Bond (0.82A) O6 - H2O6 ... 0.68 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
2 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 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
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
4 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: XSCANS (Bruker, 1996); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXTL (Bruker, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Tetraaquabis(hydrogen maleato)cadmium(II)
top
Crystal data top
[Cd(C4H3O4)2(H2O)4] | Z = 1 |
Mr = 414.59 | F(000) = 206 |
Triclinic, P1 | Dx = 2.029 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 5.4094 (5) Å | Cell parameters from 36 reflections |
b = 7.4222 (8) Å | θ = 2.3–10.3° |
c = 9.4238 (14) Å | µ = 1.67 mm−1 |
α = 110.151 (8)° | T = 293 K |
β = 105.133 (11)° | Plate, colourless |
γ = 92.302 (7)° | 0.40 × 0.30 × 0.08 mm |
V = 339.33 (8) Å3 | |
Data collection top
Bruker P4 diffractometer | 1292 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.021 |
Graphite monochromator | θmax = 26.0°, θmin = 2.4° |
ω scans | h = −6→1 |
Absorption correction: ψ scan (XSCANS; Bruker, 1996) | k = −8→8 |
Tmin = 0.593, Tmax = 0.877 | l = −11→11 |
1723 measured reflections | 3 standard reflections every 97 reflections |
1296 independent reflections | intensity decay: none |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.019 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.049 | w = 1/[σ2(Fo2) + (0.0361P)2 + 0.0305P] where P = (Fo2 + 2Fc2)/3 |
S = 1.11 | (Δ/σ)max < 0.001 |
1296 reflections | Δρmax = 0.53 e Å−3 |
114 parameters | Δρmin = −0.45 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.231 (9) |
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 | |
C1 | 0.1709 (4) | 0.4065 (3) | 0.7280 (2) | 0.0309 (4) | |
C2 | −0.0798 (4) | 0.2801 (3) | 0.6300 (2) | 0.0321 (4) | |
H2A | −0.1918 | 0.2658 | 0.6866 | 0.039* | |
C3 | −0.1696 (4) | 0.1841 (3) | 0.4741 (2) | 0.0320 (4) | |
H3A | −0.3366 | 0.1176 | 0.4387 | 0.038* | |
C4 | −0.0435 (4) | 0.1670 (3) | 0.3479 (2) | 0.0270 (4) | |
O1 | 0.2145 (4) | 0.4723 (3) | 0.87204 (18) | 0.0471 (4) | |
O2 | 0.3333 (3) | 0.4478 (3) | 0.66121 (19) | 0.0465 (4) | |
H2B | 0.2826 | 0.3843 | 0.5660 | 0.070* | |
O3 | 0.1781 (3) | 0.2581 (3) | 0.38002 (18) | 0.0439 (4) | |
O4 | −0.1673 (3) | 0.0566 (2) | 0.21069 (17) | 0.0349 (3) | |
O5 | −0.2544 (4) | −0.2843 (3) | −0.0842 (2) | 0.0439 (4) | |
H1O5 | −0.243 (7) | −0.355 (6) | −0.029 (5) | 0.068 (11)* | |
H2O5 | −0.337 (8) | −0.335 (6) | −0.161 (5) | 0.068 (12)* | |
O6 | 0.3291 (3) | −0.1460 (3) | 0.1053 (2) | 0.0328 (3) | |
H1O6 | 0.324 (7) | −0.248 (6) | 0.036 (4) | 0.050 (9)* | |
H2O6 | 0.450 (7) | −0.095 (5) | 0.132 (4) | 0.043 (9)* | |
Cd1 | 0.0000 | 0.0000 | 0.0000 | 0.02941 (14) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0376 (11) | 0.0280 (9) | 0.0241 (9) | 0.0015 (8) | 0.0055 (8) | 0.0088 (7) |
C2 | 0.0313 (11) | 0.0378 (11) | 0.0287 (10) | 0.0010 (9) | 0.0143 (8) | 0.0103 (8) |
C3 | 0.0229 (9) | 0.0398 (11) | 0.0297 (10) | −0.0034 (8) | 0.0099 (8) | 0.0075 (8) |
C4 | 0.0243 (9) | 0.0317 (10) | 0.0241 (9) | 0.0026 (7) | 0.0081 (7) | 0.0087 (7) |
O1 | 0.0672 (12) | 0.0427 (9) | 0.0223 (7) | −0.0098 (8) | 0.0062 (7) | 0.0078 (6) |
O2 | 0.0358 (9) | 0.0621 (11) | 0.0261 (7) | −0.0184 (8) | 0.0038 (6) | 0.0042 (7) |
O3 | 0.0328 (8) | 0.0631 (11) | 0.0274 (7) | −0.0125 (7) | 0.0119 (6) | 0.0064 (7) |
O4 | 0.0311 (8) | 0.0439 (8) | 0.0233 (7) | −0.0025 (6) | 0.0087 (6) | 0.0048 (6) |
O5 | 0.0469 (10) | 0.0449 (9) | 0.0304 (8) | −0.0176 (8) | −0.0002 (7) | 0.0135 (7) |
O6 | 0.0265 (8) | 0.0364 (9) | 0.0327 (8) | 0.0024 (7) | 0.0087 (6) | 0.0095 (7) |
Cd1 | 0.02378 (16) | 0.03528 (17) | 0.03277 (17) | 0.00054 (8) | 0.01124 (9) | 0.01510 (10) |
Geometric parameters (Å, º) top
Cd1—O4 | 2.3090 (15) | C4—O4 | 1.251 (2) |
Cd1—O5 | 2.2405 (17) | C4—O3 | 1.261 (3) |
Cd1—O6 | 2.3027 (16) | O2—H2B | 0.8200 |
C1—O1 | 1.226 (3) | O5—H1O5 | 0.86 (5) |
C1—O2 | 1.289 (3) | O5—H2O5 | 0.71 (4) |
C1—C2 | 1.490 (3) | O6—H1O6 | 0.80 (4) |
C2—C3 | 1.335 (3) | O6—H2O6 | 0.68 (3) |
C2—H2A | 0.9300 | Cd1—O5i | 2.2405 (17) |
C3—C4 | 1.490 (3) | Cd1—O6i | 2.3027 (16) |
C3—H3A | 0.9300 | Cd1—O4i | 2.3090 (15) |
| | | |
O1—C1—O2 | 121.6 (2) | Cd1—O6—H2O6 | 116 (3) |
O1—C1—C2 | 118.2 (2) | H1O6—O6—H2O6 | 110 (4) |
O2—C1—C2 | 120.19 (18) | O5i—Cd1—O5 | 180.0 |
C3—C2—C1 | 130.4 (2) | O5i—Cd1—O6i | 86.76 (7) |
C3—C2—H2A | 114.8 | O5—Cd1—O6i | 93.24 (7) |
C1—C2—H2A | 114.8 | O5i—Cd1—O6 | 93.24 (7) |
C2—C3—C4 | 130.02 (19) | O5—Cd1—O6 | 86.76 (7) |
C2—C3—H3A | 115.0 | O6i—Cd1—O6 | 180.0 |
C4—C3—H3A | 115.0 | O5i—Cd1—O4i | 80.95 (6) |
O4—C4—O3 | 122.42 (19) | O5—Cd1—O4i | 99.05 (6) |
O4—C4—C3 | 116.59 (18) | O6i—Cd1—O4i | 92.75 (6) |
O3—C4—C3 | 120.98 (18) | O6—Cd1—O4i | 87.25 (6) |
C1—O2—H2B | 109.5 | O5i—Cd1—O4 | 99.05 (6) |
C4—O4—Cd1 | 122.10 (13) | O5—Cd1—O4 | 80.95 (6) |
Cd1—O5—H1O5 | 122 (3) | O6i—Cd1—O4 | 87.25 (6) |
Cd1—O5—H2O5 | 126 (4) | O6—Cd1—O4 | 92.75 (6) |
H1O5—O5—H2O5 | 110 (4) | O4i—Cd1—O4 | 180.0 |
Cd1—O6—H1O6 | 106 (2) | | |
Symmetry code: (i) −x, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H1O5···O1ii | 0.86 (5) | 1.93 (5) | 2.777 (3) | 170 (4) |
O5—H2O5···O2iii | 0.71 (4) | 2.22 (4) | 2.872 (2) | 154 (5) |
O6—H1O6···O1iv | 0.80 (4) | 2.06 (4) | 2.846 (3) | 164 (3) |
O6—H2O6···O4v | 0.68 (3) | 2.13 (4) | 2.811 (2) | 178 (4) |
O2—H2B···O3 | 0.82 | 1.61 | 2.425 (2) | 179 |
Symmetry codes: (ii) −x, −y, −z+1; (iii) x−1, y−1, z−1; (iv) x, y−1, z−1; (v) x+1, y, z. |