The title compound, {[Cd3(C9H3O6)2(H2O)2]·2H2O}n, consists of a three-dimensional channel-like network. The asymmetric unit contains two crystallographically independent CdII ions, one of which shows a distorted trigonal prismatic coordination provided by six O atoms from one bidentate and three monodentate carboxylate groups, and one water molecule. The second independent CdII ion, which lies on an inversion centre, displays a distorted octahedral coordination environment provided by six O atoms from four monodentate carboxylate groups and two water molecules.
Supporting information
CCDC reference: 262276
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.013 Å
- R factor = 0.048
- wR factor = 0.116
- Data-to-parameter ratio = 10.5
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D H7C .. H8A .. 2.03 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H8A .. H8A .. 1.45 Ang.
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13
PLAT417_ALERT_2_C Short Inter D-H..H-D H7C .. H8B .. 2.10 Ang.
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.18 Ratio
0 ALERT level A = In general: serious problem
2 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
3 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
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens, 1994); data reduction: XPREP (Siemens, 1994); program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
Poly[[diaqua(µ
6-1,3,5-benzenetricarboxylato)tricadmium(II)] dihydrate]
top
Crystal data top
[Cd3(C9H3O6)2(H2O)2]·2H2O | Z = 1 |
Mr = 823.50 | F(000) = 394 |
Triclinic, P1 | Dx = 2.554 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.5573 (10) Å | Cell parameters from 1498 reflections |
b = 9.5294 (14) Å | θ = 2.3–25.0° |
c = 9.8799 (15) Å | µ = 3.04 mm−1 |
α = 62.979 (2)° | T = 273 K |
β = 79.162 (2)° | Plate, colorless |
γ = 78.385 (1)° | 0.22 × 0.14 × 0.06 mm |
V = 535.40 (14) Å3 | |
Data collection top
Bruker SMART CCD diffractometer | 1898 independent reflections |
Radiation source: fine-focus sealed tube | 1510 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
ω scans | θmax = 25.0°, θmin = 2.3° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −5→7 |
Tmin = 0.616, Tmax = 0.830 | k = −8→11 |
2767 measured reflections | l = −11→11 |
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)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.116 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.09 | w = 1/[σ2(Fo2) + (0.04P)2 + 7.0083P] where P = (Fo2 + 2Fc2)/3 |
1898 reflections | (Δ/σ)max < 0.001 |
181 parameters | Δρmax = 0.82 e Å−3 |
5 restraints | Δρmin = −0.85 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 | 0.19917 (11) | 0.43515 (7) | −0.64066 (7) | 0.0215 (2) | |
Cd2 | 0.5000 | −0.5000 | 0.0000 | 0.0248 (3) | |
C1 | 0.1570 (15) | 0.2545 (11) | 0.2086 (11) | 0.025 (2) | |
C2 | 0.2109 (14) | 0.3121 (10) | −0.3230 (10) | 0.0190 (19) | |
C3 | 0.2942 (14) | −0.2303 (10) | 0.1094 (10) | 0.0184 (18) | |
C4 | 0.1790 (14) | 0.1768 (10) | 0.1029 (10) | 0.0198 (19) | |
C5 | 0.1752 (14) | 0.2733 (10) | −0.0533 (10) | 0.0201 (19) | |
H5A | 0.1468 | 0.3831 | −0.0891 | 0.024* | |
C6 | 0.2134 (13) | 0.2064 (10) | −0.1547 (9) | 0.0160 (18) | |
C7 | 0.2603 (14) | 0.0420 (10) | −0.1008 (10) | 0.0204 (19) | |
H7A | 0.2959 | −0.0033 | −0.1693 | 0.024* | |
C8 | 0.2539 (13) | −0.0540 (10) | 0.0553 (10) | 0.0182 (18) | |
C9 | 0.2143 (14) | 0.0135 (10) | 0.1577 (10) | 0.0195 (19) | |
H9A | 0.2116 | −0.0508 | 0.2622 | 0.023* | |
O1 | 0.2588 (12) | 0.2476 (8) | −0.4128 (7) | 0.0352 (17) | |
O2 | 0.1538 (10) | 0.4607 (7) | −0.3686 (7) | 0.0257 (15) | |
O3 | 0.1035 (13) | 0.1865 (8) | 0.3471 (7) | 0.0390 (18) | |
O4 | 0.1999 (10) | 0.3983 (7) | 0.1475 (7) | 0.0265 (15) | |
O5 | 0.3524 (11) | −0.2796 (7) | 0.0084 (7) | 0.0279 (15) | |
O6 | 0.2672 (11) | −0.3164 (7) | 0.2505 (7) | 0.0261 (15) | |
O7 | 0.4146 (11) | −0.3899 (8) | −0.2659 (8) | 0.0309 (16) | |
H7B | 0.354 (16) | −0.431 (12) | −0.313 (12) | 0.037* | |
H7C | 0.423 (17) | −0.283 (6) | −0.329 (10) | 0.037* | |
O8 | 0.3110 (19) | −0.0801 (12) | −0.3989 (11) | 0.068 (3) | |
H8A | 0.416 (15) | −0.049 (19) | −0.474 (12) | 0.082* | |
H8B | 0.207 (14) | −0.085 (18) | −0.443 (14) | 0.082* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.0324 (4) | 0.0156 (3) | 0.0139 (3) | −0.0017 (3) | −0.0008 (3) | −0.0053 (3) |
Cd2 | 0.0344 (6) | 0.0158 (5) | 0.0212 (5) | −0.0023 (4) | 0.0062 (4) | −0.0092 (4) |
C1 | 0.023 (5) | 0.026 (5) | 0.025 (5) | 0.006 (4) | −0.007 (4) | −0.013 (4) |
C2 | 0.023 (5) | 0.016 (4) | 0.012 (4) | −0.002 (4) | −0.003 (3) | 0.000 (4) |
C3 | 0.021 (5) | 0.014 (4) | 0.017 (5) | −0.004 (3) | −0.002 (4) | −0.003 (4) |
C4 | 0.022 (5) | 0.020 (4) | 0.020 (5) | −0.005 (4) | 0.001 (4) | −0.011 (4) |
C5 | 0.026 (5) | 0.013 (4) | 0.016 (4) | −0.001 (4) | −0.005 (4) | −0.001 (4) |
C6 | 0.020 (5) | 0.015 (4) | 0.011 (4) | −0.005 (3) | −0.003 (3) | −0.002 (3) |
C7 | 0.019 (5) | 0.022 (5) | 0.025 (5) | −0.004 (4) | 0.001 (4) | −0.015 (4) |
C8 | 0.016 (5) | 0.019 (4) | 0.022 (5) | 0.000 (3) | −0.004 (4) | −0.011 (4) |
C9 | 0.021 (5) | 0.020 (4) | 0.009 (4) | −0.001 (4) | 0.000 (3) | −0.001 (3) |
O1 | 0.060 (5) | 0.024 (4) | 0.017 (4) | 0.001 (3) | −0.004 (3) | −0.008 (3) |
O2 | 0.032 (4) | 0.020 (3) | 0.019 (3) | 0.000 (3) | −0.003 (3) | −0.005 (3) |
O3 | 0.068 (5) | 0.034 (4) | 0.015 (4) | −0.013 (4) | 0.002 (3) | −0.010 (3) |
O4 | 0.035 (4) | 0.018 (3) | 0.029 (4) | −0.004 (3) | 0.002 (3) | −0.015 (3) |
O5 | 0.040 (4) | 0.017 (3) | 0.027 (4) | 0.001 (3) | 0.000 (3) | −0.013 (3) |
O6 | 0.038 (4) | 0.016 (3) | 0.027 (4) | −0.002 (3) | −0.004 (3) | −0.012 (3) |
O7 | 0.038 (4) | 0.019 (3) | 0.032 (4) | 0.002 (3) | −0.008 (3) | −0.008 (3) |
O8 | 0.085 (8) | 0.053 (6) | 0.061 (7) | 0.008 (6) | −0.029 (6) | −0.019 (5) |
Geometric parameters (Å, º) top
Cd1—O1 | 2.193 (7) | C3—C8 | 1.495 (12) |
Cd1—O6i | 2.212 (6) | C4—C9 | 1.380 (12) |
Cd1—O4ii | 2.273 (6) | C4—C5 | 1.394 (12) |
Cd1—O2iii | 2.330 (7) | C5—C6 | 1.376 (12) |
Cd1—O7iv | 2.548 (7) | C5—H5A | 0.9300 |
Cd1—O3ii | 2.629 (7) | C6—C7 | 1.393 (12) |
Cd2—O5v | 2.159 (6) | C7—C8 | 1.388 (13) |
Cd2—O5 | 2.159 (6) | C7—H7A | 0.9300 |
Cd2—O4vi | 2.311 (7) | C8—C9 | 1.389 (12) |
Cd2—O4vii | 2.311 (7) | C9—H9A | 0.9300 |
Cd2—O7 | 2.475 (7) | O2—Cd1iii | 2.330 (7) |
Cd2—O7v | 2.475 (7) | O3—Cd1viii | 2.629 (7) |
C1—O3 | 1.233 (11) | O4—Cd1viii | 2.273 (6) |
C1—O4 | 1.289 (11) | O4—Cd2ix | 2.311 (7) |
C1—C4 | 1.504 (12) | O6—Cd1x | 2.212 (6) |
C2—O1 | 1.255 (11) | O7—Cd1iv | 2.548 (7) |
C2—O2 | 1.272 (10) | O7—H7B | 0.91 (11) |
C2—C6 | 1.504 (11) | O7—H7C | 0.93 (5) |
C3—O6 | 1.255 (10) | O8—H8A | 0.90 (11) |
C3—O5 | 1.255 (11) | O8—H8B | 0.89 (5) |
| | | |
O1—Cd1—O6i | 128.9 (3) | O6—C3—O5 | 125.4 (8) |
O1—Cd1—O4ii | 125.9 (2) | O6—C3—C8 | 118.0 (8) |
O6i—Cd1—O4ii | 99.9 (2) | O5—C3—C8 | 116.6 (8) |
O1—Cd1—O2iii | 108.2 (3) | C9—C4—C5 | 120.4 (8) |
O6i—Cd1—O2iii | 86.7 (2) | C9—C4—C1 | 120.9 (8) |
O4ii—Cd1—O2iii | 94.7 (2) | C5—C4—C1 | 118.6 (8) |
O1—Cd1—O7iv | 89.5 (3) | C6—C5—C4 | 120.2 (8) |
O6i—Cd1—O7iv | 80.8 (2) | C6—C5—H5A | 119.9 |
O4ii—Cd1—O7iv | 75.2 (2) | C4—C5—H5A | 119.9 |
O2iii—Cd1—O7iv | 162.3 (2) | C5—C6—C7 | 119.6 (8) |
O1—Cd1—O3ii | 78.4 (2) | C5—C6—C2 | 119.6 (7) |
O6i—Cd1—O3ii | 151.9 (2) | C7—C6—C2 | 120.8 (8) |
O4ii—Cd1—O3ii | 52.4 (2) | C8—C7—C6 | 119.9 (8) |
O2iii—Cd1—O3ii | 90.4 (2) | C8—C7—H7A | 120.0 |
O7iv—Cd1—O3ii | 94.6 (2) | C6—C7—H7A | 120.0 |
O5v—Cd2—O5 | 180.0 (4) | C7—C8—C9 | 120.2 (8) |
O5v—Cd2—O4vi | 85.4 (2) | C7—C8—C3 | 118.5 (8) |
O5—Cd2—O4vi | 94.6 (2) | C9—C8—C3 | 121.3 (8) |
O5v—Cd2—O4vii | 94.6 (2) | C4—C9—C8 | 119.4 (8) |
O5—Cd2—O4vii | 85.4 (2) | C4—C9—H9A | 120.3 |
O4vi—Cd2—O4vii | 180.0 (3) | C8—C9—H9A | 120.3 |
O5v—Cd2—O7 | 91.0 (2) | C2—O1—Cd1 | 106.4 (5) |
O5—Cd2—O7 | 89.0 (2) | C2—O2—Cd1iii | 121.3 (6) |
O4vi—Cd2—O7 | 76.0 (2) | C1—O3—Cd1viii | 85.6 (6) |
O4vii—Cd2—O7 | 104.0 (2) | C1—O4—Cd1viii | 100.9 (5) |
O5v—Cd2—O7v | 89.0 (2) | C1—O4—Cd2ix | 129.3 (6) |
O5—Cd2—O7v | 91.0 (2) | Cd1viii—O4—Cd2ix | 102.3 (3) |
O4vi—Cd2—O7v | 104.0 (2) | C3—O5—Cd2 | 136.6 (6) |
O4vii—Cd2—O7v | 76.0 (2) | C3—O6—Cd1x | 125.9 (5) |
O7—Cd2—O7v | 180.0 (3) | Cd2—O7—Cd1iv | 90.5 (2) |
O3—C1—O4 | 120.4 (8) | Cd2—O7—H7B | 131 (7) |
O3—C1—C4 | 123.1 (9) | Cd1iv—O7—H7B | 102 (7) |
O4—C1—C4 | 116.5 (8) | Cd2—O7—H7C | 118 (7) |
O1—C2—O2 | 122.6 (8) | Cd1iv—O7—H7C | 86 (7) |
O1—C2—C6 | 117.8 (7) | H7B—O7—H7C | 110 (10) |
O2—C2—C6 | 119.5 (8) | H8A—O8—H8B | 105 (7) |
| | | |
O3—C1—C4—C9 | −23.5 (14) | O6i—Cd1—O1—C2 | 41.5 (8) |
O4—C1—C4—C9 | 155.7 (9) | O4ii—Cd1—O1—C2 | −169.4 (6) |
O3—C1—C4—C5 | 160.2 (9) | O2iii—Cd1—O1—C2 | −59.3 (7) |
O4—C1—C4—C5 | −20.7 (12) | O7iv—Cd1—O1—C2 | 119.3 (6) |
C9—C4—C5—C6 | −2.1 (14) | O3ii—Cd1—O1—C2 | −145.9 (7) |
C1—C4—C5—C6 | 174.3 (8) | O1—C2—O2—Cd1iii | 97.7 (10) |
C4—C5—C6—C7 | −1.4 (13) | C6—C2—O2—Cd1iii | −79.6 (9) |
C4—C5—C6—C2 | −179.4 (8) | O4—C1—O3—Cd1viii | −7.7 (9) |
O1—C2—C6—C5 | 175.8 (9) | C4—C1—O3—Cd1viii | 171.4 (8) |
O2—C2—C6—C5 | −6.8 (13) | O3—C1—O4—Cd1viii | 9.0 (10) |
O1—C2—C6—C7 | −2.2 (13) | C4—C1—O4—Cd1viii | −170.1 (6) |
O2—C2—C6—C7 | 175.3 (8) | O3—C1—O4—Cd2ix | 124.9 (8) |
C5—C6—C7—C8 | 4.5 (13) | C4—C1—O4—Cd2ix | −54.2 (11) |
C2—C6—C7—C8 | −177.5 (8) | O6—C3—O5—Cd2 | −17.2 (15) |
C6—C7—C8—C9 | −4.2 (13) | C8—C3—O5—Cd2 | 163.0 (6) |
C6—C7—C8—C3 | 176.9 (8) | O4vi—Cd2—O5—C3 | −115.8 (9) |
O6—C3—C8—C7 | −172.9 (8) | O4vii—Cd2—O5—C3 | 64.2 (9) |
O5—C3—C8—C7 | 7.0 (13) | O7—Cd2—O5—C3 | 168.3 (9) |
O6—C3—C8—C9 | 8.2 (13) | O7v—Cd2—O5—C3 | −11.7 (9) |
O5—C3—C8—C9 | −171.9 (8) | O5—C3—O6—Cd1x | −23.8 (13) |
C5—C4—C9—C8 | 2.4 (13) | C8—C3—O6—Cd1x | 156.0 (6) |
C1—C4—C9—C8 | −173.9 (8) | O5v—Cd2—O7—Cd1iv | −57.3 (2) |
C7—C8—C9—C4 | 0.7 (13) | O5—Cd2—O7—Cd1iv | 122.7 (2) |
C3—C8—C9—C4 | 179.6 (8) | O4vi—Cd2—O7—Cd1iv | 27.6 (2) |
O2—C2—O1—Cd1 | −4.2 (11) | O4vii—Cd2—O7—Cd1iv | −152.4 (2) |
C6—C2—O1—Cd1 | 173.2 (6) | | |
Symmetry codes: (i) x, y+1, z−1; (ii) x, y, z−1; (iii) −x, −y+1, −z−1; (iv) −x+1, −y, −z−1; (v) −x+1, −y−1, −z; (vi) −x+1, −y, −z; (vii) x, y−1, z; (viii) x, y, z+1; (ix) x, y+1, z; (x) x, y−1, z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7C···O8 | 0.93 (5) | 1.77 (7) | 2.628 (12) | 151 (10) |