metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 68| Part 6| June 2012| Pages m801-m802

Poly[[tetra­aqua­bis­­(μ3-5-carboxybenzene-1,2,4-tri­carboxyl­ato)tricadmium] tetra­hydrate]

aPharmacy College, Henan University of Traditional Chinese Medicine, Zhengzhou 450008, People's Republic of China
*Correspondence e-mail: 13623712409@139.com

(Received 14 May 2012; accepted 18 May 2012; online 26 May 2012)

There are three independent CdII ions in the title complex, {[Cd3(C10H3O8)2(H2O)4]·4H2O}n, one of which is coordinated by four O atoms from three 5-carboxybenzene-1,2,4-tri­carboxyl­ate ligands and by two water mol­ecules in a distorted octa­hedral geometry. The second CdII ion is coordinated by five O atoms from four 5-carboxybenzene-1,2,4-tri­carboxyl­ate ligands and by one water mol­ecule also in a distorted octa­hedral geometry while the third CdII ion is coordinated by five O atoms from three 5-carboxybenzene-1,2,4-tri­carboxyl­ate ligands and by one water mol­ecule in a highly distorted octa­hedral geometry. The 5-carboxybenzene-1,2,4-tri­carboxyl­ate ligands bridge the CdII ions, resulting in the formation of a three-dimensional structure. Intra- and inter­molecular O—H⋯O hydrogen bonds are present throughout the three-dimensional structure.

Related literature

For background information on CdII complexes constructed from benzene-1,2,4,5-tetra­carb­oxy­lic acid ligand see: Lin et al. (2008[Lin, J.-D., Cheng, J.-W. & Du, S.-W. (2008). Cryst. Growth Des. 8, 3345-3353.]); Prajapati et al. (2009[Prajapati, R., Mishra, L., Kimura, K. & Raghavaiah, P. (2009). Polyhedron, 28, 600-608.]); Wang et al. (2012[Wang, X., Liu, Y., Xu, C., Guo, Q., Hou, H. & Fan, Y. (2012). Cryst. Growth Des. 12, 2435-2444.]).

[Scheme 1]

Experimental

Crystal data
  • [Cd3(C10H3O8)2(H2O)4]·4H2O

  • Mr = 983.58

  • Triclinic, [P \overline 1]

  • a = 8.3244 (17) Å

  • b = 12.992 (3) Å

  • c = 13.540 (3) Å

  • α = 85.79 (3)°

  • β = 84.67 (3)°

  • γ = 87.17 (3)°

  • V = 1452.6 (5) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 2.28 mm−1

  • T = 293 K

  • 0.20 × 0.17 × 0.16 mm

Data collection
  • Rigaku Saturn diffractometer

  • Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2004[Rigaku/MSC (2004). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA.]) Tmin = 0.658, Tmax = 0.712

  • 18101 measured reflections

  • 6873 independent reflections

  • 6308 reflections with I > 2σ(I)

  • Rint = 0.022

Refinement
  • R[F2 > 2σ(F2)] = 0.029

  • wR(F2) = 0.068

  • S = 1.05

  • 6873 reflections

  • 424 parameters

  • H-atom parameters constrained

  • Δρmax = 0.64 e Å−3

  • Δρmin = −0.84 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O11—H11⋯O22 0.82 2.16 2.895 (4) 149
O17—H17C⋯O8 0.84 2.32 3.158 (4) 179
O18—H18B⋯O3 0.85 2.50 3.292 (4) 156
O2—H2⋯O10i 0.82 2.53 3.237 (3) 145
O18—H18A⋯O10ii 0.85 2.19 3.031 (4) 168
O24—H24B⋯O15iii 0.85 2.09 2.841 (4) 147
O19—H19A⋯O23iv 0.85 1.92 2.720 (4) 157
O17—H17B⋯O23v 0.85 2.29 3.073 (5) 155
O19—H19B⋯O6vi 0.85 1.85 2.698 (3) 173
O20—H20B⋯O6vi 0.85 2.18 2.996 (4) 160
O20—H20C⋯O13vii 0.85 2.23 3.047 (4) 161
O22—H22A⋯O2vii 0.85 2.05 2.807 (4) 147
O23—H23B⋯O7vii 0.85 2.09 2.894 (4) 158
O24—H24A⋯O4viii 0.85 1.94 2.783 (4) 173
O21—H21A⋯O9ix 0.85 1.91 2.748 (4) 168
O21—H21B⋯O12x 0.85 1.94 2.765 (4) 163
O22—H22B⋯O21xi 0.85 1.99 2.825 (4) 166
O23—H23A⋯O2xii 0.85 2.20 2.944 (4) 147
Symmetry codes: (i) -x, -y, -z; (ii) -x+1, -y, -z; (iii) -x+1, -y+1, -z; (iv) x, y+1, z-1; (v) -x+1, -y, -z+1; (vi) x+1, y+1, z-1; (vii) x+1, y, z; (viii) x+1, y+1, z; (ix) -x, -y+1, -z+1; (x) x, y, z+1; (xi) -x+1, -y+1, -z+1; (xii) -x, -y, -z+1.

Data collection: CrystalClear (Rigaku/MSC, 2004[Rigaku/MSC (2004). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA.]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information


Comment top

A large number of CdII complexes constructed from benzene-1,2,4,5-tetracarboxylic acid have been extensively studied because of the diversity coordination modes and sensitivity to pH values of the carboxylate groups. Some of the final products exhibit useful functional properties (Lin et al., 2008; Prajapati et al., 2009; Wang et al., 2012). In order to further explore such compounds with new structures, we selected benzene-1,2,4,5-tetracarboxylic acid as ligand to self-assembly with Cd(NO3)2 and obtained the title complex, {[Cd3(C10H3O8)2(H2O)4] (H2O)4}n, the crystal structure of which is reported herein. As shown in Fig. 1, there are three crystallographically independent cadmium ions (Cd1, Cd2 and Cd3), two crystallographically independent 5-carboxybenzene-1,2,4-tricarboxylate ligands, four crystallographically independent coordination water molecules and four crystallographically independent solvent water molecules in the asymmetric unit. Atom Cd1 displays a distorted octahedral geometry defined by atoms O1, O9, O10 from two 5-carboxybenzene-1,2,4-tricarboxylate groups and O18 from water molecule in equatorial positions and by atoms O1A, O17 from one 5-carboxybenzene-1,2,4-tricarboxylate group and one water molecule in axial positions (symmetry codes A to F are given in the figure caption). Atom Cd2 is coordinated by six oxygen atoms from four 5-carboxybenzene-1,2,4-tricarboxylate groups (O5B, O7C, O13, O15D, O16D) and one water molecule (O19) leading to a distorted octahedral geometry. Atom Cd3 is coordinated by five O atoms (O3E, O4E, O11F, O12F, O14) from three 5-carboxybenzene-1,2,4-tricarboxylate groups and by one O atom (O20) from water molecule in a seriously distorted octahedral geometry. As depicted in Fig. 2, Cd1, Cd2 and Cd3 ions are bridged by 5-carboxybenzene-1,2,4-tricarboxylate ligands forming the three-dimensional structure in which the carboxylate groups of the 5-carboxybenzene-1,2,4-tricarboxylate ligands coordinate to CdII ions in monodentate mode, or in chelating mode or in bridging mode. In addition, intramolecular O—H···O hydrogen bonds between the coordinated water molecules and carboxylate groups stabilize the molecular conformation. In the crystal, O—H···O hydrogen bonds (see Table 1 for full listing) form a three-dimensional network throughout the polymer structure (Fig. 2).

Related literature top

For background information on CdII complexes constructed from benzene-1,2,4,5-tetracarboxylic acid ligand see: Lin et al. (2008); Prajapati et al. (2009); Wang et al. (2012).

Experimental top

A mixture of Cd(NO3)2 (0.05 mmol), benzene-1,2,4,5-tetracarboxylic acid (0.05 mmol),water (4 ml) and methanol(4 ml) was placed in a 25 ml Teflon-lined stainless steel vessel and heated at 293K for 72 h, then cooled to room temperature. Colourless crystals were obtained from the filtrate and dried in air.

Refinement top

H atoms bound to C atoms were positioned geometrically and refined as riding atoms, with C-H = 0.93 Å. H atoms bound to O atoms were found from difference maps and included with O—H = 0.82—0.85Å All H atoms were refined with Uiso(H) = 1.2 Ueq(C,O).

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2004); cell refinement: CrystalClear (Rigaku/MSC, 2004); data reduction: CrystalClear (Rigaku/MSC, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. View of the title complex showing labeling and 30% probability displacement ellipsolids. [Symmetry code A: -x, -y, -z, B: x, y + 1, z - 1; C: -x, -y + 1, -z; D: -x + 1, -y + 1, -z - 1; E: -x + 1, -y, -z; F: -x + 1, -y + 1, -z.].
[Figure 2] Fig. 2. Packing plot of the title complex with hydrogen bonds indicated by dashed lines.
Poly[[tetraaquabis(µ3-5-carboxybenzene-1,2,4-tricarboxylato)tricadmium] tetrahydrate] top
Crystal data top
[Cd3(C10H3O8)2(H2O)4]·4H2OZ = 2
Mr = 983.58F(000) = 956
Triclinic, P1Dx = 2.249 Mg m3
a = 8.3244 (17) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.992 (3) ÅCell parameters from 4891 reflections
c = 13.540 (3) Åθ = 1.6–27.9°
α = 85.79 (3)°µ = 2.28 mm1
β = 84.67 (3)°T = 293 K
γ = 87.17 (3)°Prism, colourless
V = 1452.6 (5) Å30.20 × 0.17 × 0.16 mm
Data collection top
Rigaku Saturn
diffractometer
6873 independent reflections
Radiation source: fine-focus sealed tube6308 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.022
Detector resolution: 28.5714 pixels mm-1θmax = 27.9°, θmin = 1.5°
ω scansh = 1010
Absorption correction: multi-scan
(CrystalClear; Rigaku/MSC, 2004)
k = 1716
Tmin = 0.658, Tmax = 0.712l = 1717
18101 measured reflections
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)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.068H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.031P)2 + 2.6215P]
where P = (Fo2 + 2Fc2)/3
6873 reflections(Δ/σ)max = 0.002
424 parametersΔρmax = 0.64 e Å3
0 restraintsΔρmin = 0.84 e Å3
Crystal data top
[Cd3(C10H3O8)2(H2O)4]·4H2Oγ = 87.17 (3)°
Mr = 983.58V = 1452.6 (5) Å3
Triclinic, P1Z = 2
a = 8.3244 (17) ÅMo Kα radiation
b = 12.992 (3) ŵ = 2.28 mm1
c = 13.540 (3) ÅT = 293 K
α = 85.79 (3)°0.20 × 0.17 × 0.16 mm
β = 84.67 (3)°
Data collection top
Rigaku Saturn
diffractometer
6873 independent reflections
Absorption correction: multi-scan
(CrystalClear; Rigaku/MSC, 2004)
6308 reflections with I > 2σ(I)
Tmin = 0.658, Tmax = 0.712Rint = 0.022
18101 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0290 restraints
wR(F2) = 0.068H-atom parameters constrained
S = 1.05Δρmax = 0.64 e Å3
6873 reflectionsΔρmin = 0.84 e Å3
424 parameters
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
Cd10.16008 (3)0.030815 (17)0.077320 (17)0.02133 (6)
Cd20.38339 (3)0.741101 (16)0.452927 (15)0.01619 (6)
Cd30.82987 (3)0.508576 (17)0.221027 (15)0.01826 (6)
O10.1133 (3)0.01484 (17)0.09031 (15)0.0218 (5)
O20.3553 (3)0.00697 (18)0.17445 (17)0.0253 (5)
H20.39530.03810.14650.030*
O30.1589 (3)0.33132 (18)0.21984 (18)0.0309 (6)
O40.0193 (3)0.40654 (16)0.34811 (17)0.0257 (5)
O50.1396 (3)0.30563 (17)0.50753 (18)0.0240 (5)
O60.1027 (3)0.2697 (2)0.58004 (18)0.0371 (6)
O70.2938 (3)0.08991 (18)0.46215 (17)0.0303 (6)
O80.2171 (3)0.14979 (17)0.30916 (17)0.0256 (5)
O90.1276 (3)0.19607 (18)0.00883 (17)0.0239 (5)
O100.3778 (3)0.13809 (17)0.00776 (17)0.0239 (5)
O110.2987 (3)0.35204 (18)0.10793 (16)0.0259 (5)
H110.39020.32560.10100.031*
O120.2293 (4)0.50979 (18)0.05480 (17)0.0332 (6)
O130.3761 (3)0.59828 (17)0.33999 (16)0.0216 (5)
O140.6352 (3)0.56376 (16)0.31637 (16)0.0196 (4)
O150.5157 (3)0.39054 (17)0.43313 (15)0.0219 (5)
O160.5220 (4)0.22733 (19)0.37873 (19)0.0388 (7)
O170.1438 (4)0.1222 (3)0.2170 (2)0.0504 (8)
H17B0.18580.08890.26500.060*
H17C0.04720.12940.24120.060*
O180.3002 (4)0.1137 (3)0.1143 (3)0.0722 (12)
H18A0.39660.11630.08730.087*
H18B0.28590.16680.15420.087*
O190.5894 (3)0.79789 (18)0.37472 (19)0.0298 (5)
H19A0.57940.86340.37730.036*
H19B0.68890.78050.38570.036*
O201.0312 (3)0.6158 (2)0.2434 (2)0.0431 (7)
H20B1.00470.66080.28840.052*
H20C1.12370.59550.26850.052*
O210.1511 (4)0.6937 (2)0.9506 (2)0.0476 (8)
H21A0.06100.71990.97370.057*
H21B0.16060.64180.99200.057*
O220.5749 (4)0.2208 (2)0.1579 (2)0.0488 (8)
H22A0.56930.15810.14500.059*
H22B0.66640.23810.13010.059*
O230.6103 (4)0.0002 (2)0.6595 (2)0.0484 (8)
H23A0.52770.02230.69480.058*
H23B0.62880.04150.60840.058*
O240.7826 (3)0.5204 (2)0.4913 (2)0.0378 (6)
H24A0.85070.54740.44760.045*
H24B0.69300.52250.46560.045*
C10.2069 (4)0.0074 (2)0.1688 (2)0.0171 (6)
C20.0634 (4)0.3266 (2)0.2965 (2)0.0179 (6)
C30.0021 (4)0.2601 (2)0.5089 (2)0.0176 (6)
C40.2286 (4)0.0777 (2)0.3753 (2)0.0186 (6)
C50.1338 (3)0.0616 (2)0.2577 (2)0.0152 (5)
C60.0544 (3)0.1566 (2)0.2429 (2)0.0163 (6)
H6A0.03200.17700.17840.020*
C70.0074 (3)0.2223 (2)0.3227 (2)0.0153 (5)
C80.0389 (3)0.1918 (2)0.4193 (2)0.0150 (5)
C90.1116 (4)0.0943 (2)0.4335 (2)0.0171 (6)
H9A0.12930.07270.49770.021*
C100.1586 (3)0.0284 (2)0.3547 (2)0.0162 (6)
C110.2780 (4)0.2045 (2)0.0247 (2)0.0174 (6)
C120.2843 (4)0.4197 (2)0.0387 (2)0.0179 (6)
C130.4879 (3)0.5440 (2)0.3039 (2)0.0142 (5)
C140.4981 (4)0.3204 (2)0.3644 (2)0.0184 (6)
C150.3382 (3)0.2933 (2)0.0935 (2)0.0154 (5)
C160.3343 (4)0.3948 (2)0.0658 (2)0.0168 (6)
C170.3824 (4)0.4731 (2)0.1368 (2)0.0179 (6)
H17A0.37790.54090.11860.021*
C180.4369 (3)0.4528 (2)0.2338 (2)0.0144 (5)
C190.4427 (3)0.3504 (2)0.2610 (2)0.0155 (5)
C200.3926 (4)0.2723 (2)0.1903 (2)0.0164 (6)
H20A0.39560.20450.20850.020*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.02465 (12)0.01847 (12)0.02003 (11)0.00301 (9)0.00097 (9)0.00440 (8)
Cd20.02026 (11)0.01366 (11)0.01385 (10)0.00249 (8)0.00120 (8)0.00115 (8)
Cd30.02283 (11)0.01690 (11)0.01451 (10)0.00382 (8)0.00031 (8)0.00328 (8)
O10.0248 (11)0.0261 (12)0.0142 (10)0.0037 (9)0.0006 (9)0.0023 (9)
O20.0191 (11)0.0274 (12)0.0292 (12)0.0018 (9)0.0038 (9)0.0004 (10)
O30.0424 (14)0.0185 (12)0.0276 (12)0.0088 (10)0.0142 (11)0.0024 (10)
O40.0343 (13)0.0126 (10)0.0281 (12)0.0004 (9)0.0075 (10)0.0012 (9)
O50.0196 (11)0.0203 (11)0.0327 (12)0.0063 (9)0.0082 (9)0.0023 (9)
O60.0302 (13)0.0521 (17)0.0235 (12)0.0133 (12)0.0058 (10)0.0142 (12)
O70.0465 (15)0.0221 (12)0.0201 (11)0.0132 (11)0.0041 (10)0.0052 (9)
O80.0343 (13)0.0148 (11)0.0267 (12)0.0031 (9)0.0031 (10)0.0025 (9)
O90.0209 (11)0.0248 (12)0.0245 (11)0.0038 (9)0.0012 (9)0.0055 (9)
O100.0254 (11)0.0192 (11)0.0248 (12)0.0027 (9)0.0030 (9)0.0058 (9)
O110.0337 (13)0.0269 (12)0.0150 (10)0.0087 (10)0.0025 (9)0.0009 (9)
O120.0628 (18)0.0184 (12)0.0154 (11)0.0084 (11)0.0076 (11)0.0019 (9)
O130.0201 (11)0.0199 (11)0.0227 (11)0.0018 (8)0.0002 (9)0.0082 (9)
O140.0181 (10)0.0206 (11)0.0192 (10)0.0029 (8)0.0002 (8)0.0031 (8)
O150.0264 (11)0.0247 (12)0.0125 (10)0.0026 (9)0.0036 (8)0.0025 (8)
O160.0687 (19)0.0186 (12)0.0254 (13)0.0009 (12)0.0180 (12)0.0073 (10)
O170.0495 (18)0.062 (2)0.0403 (17)0.0057 (15)0.0029 (14)0.0101 (15)
O180.048 (2)0.059 (2)0.097 (3)0.0194 (17)0.0208 (19)0.030 (2)
O190.0222 (12)0.0239 (12)0.0442 (15)0.0033 (9)0.0041 (10)0.0090 (11)
O200.0369 (15)0.0461 (17)0.0446 (17)0.0025 (13)0.0032 (13)0.0001 (13)
O210.0448 (17)0.0389 (16)0.0519 (18)0.0145 (13)0.0113 (14)0.0152 (14)
O220.0494 (18)0.0419 (17)0.0553 (19)0.0009 (14)0.0129 (15)0.0043 (14)
O230.0538 (19)0.0310 (15)0.060 (2)0.0038 (13)0.0118 (15)0.0063 (14)
O240.0309 (14)0.0459 (16)0.0350 (14)0.0020 (12)0.0001 (11)0.0040 (12)
C10.0244 (15)0.0106 (13)0.0165 (14)0.0007 (11)0.0017 (11)0.0018 (10)
C20.0191 (14)0.0169 (14)0.0177 (14)0.0021 (11)0.0016 (11)0.0033 (11)
C30.0202 (14)0.0159 (14)0.0169 (14)0.0022 (11)0.0049 (11)0.0014 (11)
C40.0190 (14)0.0136 (14)0.0235 (15)0.0044 (11)0.0052 (12)0.0035 (11)
C50.0163 (13)0.0129 (13)0.0158 (13)0.0006 (10)0.0001 (10)0.0001 (10)
C60.0178 (13)0.0163 (14)0.0138 (13)0.0027 (11)0.0019 (11)0.0005 (11)
C70.0177 (13)0.0124 (13)0.0155 (13)0.0017 (10)0.0004 (11)0.0017 (10)
C80.0169 (13)0.0129 (13)0.0148 (13)0.0016 (10)0.0012 (10)0.0005 (10)
C90.0211 (14)0.0165 (14)0.0135 (13)0.0032 (11)0.0002 (11)0.0039 (11)
C100.0184 (14)0.0154 (14)0.0145 (13)0.0030 (11)0.0008 (11)0.0036 (11)
C110.0253 (15)0.0163 (14)0.0105 (12)0.0035 (11)0.0019 (11)0.0020 (11)
C120.0232 (15)0.0181 (14)0.0120 (13)0.0014 (11)0.0019 (11)0.0021 (11)
C130.0221 (14)0.0111 (13)0.0085 (12)0.0014 (10)0.0012 (10)0.0000 (10)
C140.0176 (14)0.0203 (15)0.0165 (14)0.0012 (11)0.0018 (11)0.0020 (11)
C150.0165 (13)0.0136 (13)0.0152 (13)0.0001 (10)0.0001 (11)0.0020 (10)
C160.0216 (14)0.0160 (14)0.0118 (13)0.0021 (11)0.0019 (11)0.0008 (11)
C170.0255 (15)0.0124 (13)0.0151 (13)0.0010 (11)0.0017 (11)0.0022 (11)
C180.0151 (13)0.0138 (13)0.0134 (13)0.0005 (10)0.0016 (10)0.0028 (10)
C190.0186 (14)0.0158 (14)0.0114 (12)0.0019 (11)0.0014 (10)0.0003 (10)
C200.0227 (14)0.0096 (13)0.0164 (13)0.0014 (11)0.0003 (11)0.0025 (10)
Geometric parameters (Å, º) top
Cd1—O182.212 (3)O15—Cd2iv2.453 (2)
Cd1—O12.285 (2)O16—C141.243 (4)
Cd1—O172.296 (3)O16—Cd2iv2.355 (3)
Cd1—O92.382 (2)O17—H17B0.8473
Cd1—O102.419 (2)O17—H17C0.8429
Cd1—O1i2.457 (2)O18—H18A0.8500
Cd1—C112.733 (3)O18—H18B0.8500
Cd2—O5ii2.268 (2)O19—H19A0.8500
Cd2—O192.277 (2)O19—H19B0.8500
Cd2—O7iii2.282 (2)O20—H20B0.8500
Cd2—O132.316 (2)O20—H20C0.8500
Cd2—O16iv2.355 (3)O21—H21A0.8500
Cd2—O15iv2.453 (2)O21—H21B0.8500
Cd2—C14iv2.737 (3)O22—H22A0.8500
Cd3—O202.217 (3)O22—H22B0.8500
Cd3—O142.224 (2)O23—H23A0.8500
Cd3—O12v2.256 (2)O23—H23B0.8499
Cd3—O3vi2.299 (2)O24—H24A0.8500
Cd3—O4vi2.462 (2)O24—H24B0.8500
Cd3—O11v2.585 (2)C1—C51.511 (4)
Cd3—C2vi2.721 (3)C2—C71.504 (4)
O1—C11.282 (4)C2—Cd3vi2.721 (3)
O1—Cd1i2.457 (2)C3—C81.505 (4)
O2—C11.237 (4)C4—C101.505 (4)
O2—H20.8199C5—C61.391 (4)
O3—C21.251 (4)C5—C101.406 (4)
O3—Cd3vi2.299 (2)C6—C71.400 (4)
O4—C21.259 (4)C6—H6A0.9300
O4—Cd3vi2.462 (2)C7—C81.391 (4)
O5—C31.262 (4)C8—C91.395 (4)
O5—Cd2vii2.268 (2)C9—C101.390 (4)
O6—C31.242 (4)C9—H9A0.9300
O7—C41.266 (4)C11—C151.505 (4)
O7—Cd2iii2.282 (2)C12—C161.492 (4)
O8—C41.248 (4)C13—C181.515 (4)
O9—C111.260 (4)C14—C191.505 (4)
O10—C111.252 (4)C14—Cd2iv2.737 (3)
O11—C121.247 (4)C15—C201.389 (4)
O11—Cd3v2.585 (2)C15—C161.394 (4)
O11—H110.8193C16—C171.394 (4)
O12—C121.262 (4)C17—C181.389 (4)
O12—Cd3v2.256 (2)C17—H17A0.9300
O13—C131.254 (4)C18—C191.404 (4)
O14—C131.258 (4)C19—C201.394 (4)
O15—C141.258 (4)C20—H20A0.9300
O18—Cd1—O1114.51 (11)H17B—O17—H17C100.8
O18—Cd1—O17105.77 (15)Cd1—O18—H18A114.7
O1—Cd1—O1791.67 (10)Cd1—O18—H18B135.9
O18—Cd1—O9152.67 (11)H18A—O18—H18B109.1
O1—Cd1—O989.85 (8)Cd2—O19—H19A107.1
O17—Cd1—O984.60 (10)Cd2—O19—H19B126.1
O18—Cd1—O1099.67 (11)H19A—O19—H19B108.6
O1—Cd1—O10144.38 (8)Cd3—O20—H20B105.3
O17—Cd1—O1088.28 (10)Cd3—O20—H20C120.5
O9—Cd1—O1054.67 (8)H20B—O20—H20C100.4
O18—Cd1—O1i94.72 (13)H21A—O21—H21B100.1
O1—Cd1—O1i77.86 (9)H22A—O22—H22B104.0
O17—Cd1—O1i159.43 (10)H23A—O23—H23B109.7
O9—Cd1—O1i77.79 (8)H24A—O24—H24B106.7
O10—Cd1—O1i90.13 (8)O2—C1—O1123.9 (3)
O18—Cd1—C11126.25 (11)O2—C1—C5117.6 (3)
O1—Cd1—C11117.16 (9)O1—C1—C5118.3 (3)
O17—Cd1—C1186.72 (10)O3—C2—O4121.8 (3)
O9—Cd1—C1127.42 (8)O3—C2—C7118.2 (3)
O10—Cd1—C1127.26 (8)O4—C2—C7119.9 (3)
O1i—Cd1—C1182.55 (8)O3—C2—Cd3vi57.25 (16)
O5ii—Cd2—O19164.72 (9)O4—C2—Cd3vi64.73 (16)
O5ii—Cd2—O7iii89.68 (9)C7—C2—Cd3vi170.8 (2)
O19—Cd2—O7iii85.15 (9)O6—C3—O5123.4 (3)
O5ii—Cd2—O1386.30 (9)O6—C3—C8118.0 (3)
O19—Cd2—O1388.23 (9)O5—C3—C8118.6 (3)
O7iii—Cd2—O13139.19 (8)O8—C4—O7122.8 (3)
O5ii—Cd2—O16iv92.31 (10)O8—C4—C10120.2 (3)
O19—Cd2—O16iv101.56 (10)O7—C4—C10117.0 (3)
O7iii—Cd2—O16iv85.25 (9)C6—C5—C10119.0 (3)
O13—Cd2—O16iv135.45 (8)C6—C5—C1116.3 (3)
O5ii—Cd2—O15iv82.85 (8)C10—C5—C1124.2 (3)
O19—Cd2—O15iv110.44 (8)C5—C6—C7121.5 (3)
O7iii—Cd2—O15iv138.17 (8)C5—C6—H6A119.3
O13—Cd2—O15iv81.52 (8)C7—C6—H6A119.3
O16iv—Cd2—O15iv54.23 (8)C8—C7—C6119.6 (3)
O5ii—Cd2—C14iv86.15 (9)C8—C7—C2124.5 (3)
O19—Cd2—C14iv109.13 (9)C6—C7—C2115.7 (3)
O7iii—Cd2—C14iv111.38 (9)C7—C8—C9118.7 (3)
O13—Cd2—C14iv108.83 (9)C7—C8—C3122.5 (3)
O16iv—Cd2—C14iv26.93 (9)C9—C8—C3118.8 (3)
O15iv—Cd2—C14iv27.35 (8)C10—C9—C8122.1 (3)
O20—Cd3—O14109.96 (10)C10—C9—H9A118.9
O20—Cd3—O12v104.98 (11)C8—C9—H9A118.9
O14—Cd3—O12v118.76 (9)C9—C10—C5118.9 (3)
O20—Cd3—O3vi128.71 (10)C9—C10—C4119.1 (3)
O14—Cd3—O3vi106.24 (9)C5—C10—C4121.9 (3)
O12v—Cd3—O3vi87.43 (9)O10—C11—O9122.8 (3)
O20—Cd3—O4vi86.79 (10)O10—C11—C15119.2 (3)
O14—Cd3—O4vi94.92 (8)O9—C11—C15117.8 (3)
O12v—Cd3—O4vi136.12 (8)O10—C11—Cd162.26 (16)
O3vi—Cd3—O4vi54.72 (8)O9—C11—Cd160.59 (16)
O20—Cd3—O11v82.73 (10)C15—C11—Cd1172.2 (2)
O14—Cd3—O11v83.20 (8)O11—C12—O12121.6 (3)
O12v—Cd3—O11v53.26 (8)O11—C12—C16119.7 (3)
O3vi—Cd3—O11v137.20 (8)O12—C12—C16118.8 (3)
O4vi—Cd3—O11v167.97 (7)O13—C13—O14125.0 (3)
O20—Cd3—C2vi108.01 (10)O13—C13—C18116.1 (3)
O14—Cd3—C2vi103.16 (9)O14—C13—C18118.7 (2)
O12v—Cd3—C2vi111.66 (9)O16—C14—O15122.6 (3)
O3vi—Cd3—C2vi27.23 (9)O16—C14—C19118.7 (3)
O4vi—Cd3—C2vi27.55 (8)O15—C14—C19118.7 (3)
O11v—Cd3—C2vi164.19 (8)O16—C14—Cd2iv59.12 (17)
C1—O1—Cd1127.97 (19)O15—C14—Cd2iv63.63 (16)
C1—O1—Cd1i124.46 (19)C19—C14—Cd2iv176.1 (2)
Cd1—O1—Cd1i102.14 (9)C20—C15—C16119.4 (3)
C1—O2—H2109.5C20—C15—C11117.3 (3)
C2—O3—Cd3vi95.52 (19)C16—C15—C11123.2 (3)
C2—O4—Cd3vi87.72 (18)C17—C16—C15119.0 (3)
C3—O5—Cd2vii133.2 (2)C17—C16—C12119.9 (3)
C4—O7—Cd2iii103.09 (19)C15—C16—C12121.0 (3)
C11—O9—Cd191.98 (18)C18—C17—C16122.0 (3)
C11—O10—Cd190.47 (18)C18—C17—H17A119.0
C12—O11—Cd3v85.03 (18)C16—C17—H17A119.0
C12—O11—H11108.1C17—C18—C19118.8 (3)
Cd3v—O11—H11132.4C17—C18—C13117.2 (3)
C12—O12—Cd3v100.07 (19)C19—C18—C13124.1 (2)
C13—O13—Cd2130.86 (19)C20—C19—C18119.3 (3)
C13—O14—Cd3127.86 (18)C20—C19—C14117.8 (3)
C14—O15—Cd2iv89.03 (18)C18—C19—C14122.9 (3)
C14—O16—Cd2iv93.95 (19)C15—C20—C19121.5 (3)
Cd1—O17—H17B112.3C15—C20—H20A119.2
Cd1—O17—H17C110.8C19—C20—H20A119.2
O18—Cd1—O1—C164.7 (3)C6—C5—C10—C4173.8 (3)
O17—Cd1—O1—C143.4 (3)C1—C5—C10—C414.6 (4)
O9—Cd1—O1—C1128.0 (2)O8—C4—C10—C9153.6 (3)
O10—Cd1—O1—C1132.8 (2)O7—C4—C10—C924.4 (4)
O1i—Cd1—O1—C1154.4 (3)O8—C4—C10—C524.0 (4)
C11—Cd1—O1—C1130.6 (2)O7—C4—C10—C5158.0 (3)
O18—Cd1—O1—Cd1i89.68 (14)Cd1—O10—C11—O92.9 (3)
O17—Cd1—O1—Cd1i162.14 (11)Cd1—O10—C11—C15171.3 (2)
O9—Cd1—O1—Cd1i77.54 (9)Cd1—O9—C11—O103.0 (3)
O10—Cd1—O1—Cd1i72.77 (15)Cd1—O9—C11—C15171.3 (2)
O1i—Cd1—O1—Cd1i0.0O18—Cd1—C11—O1014.6 (2)
C11—Cd1—O1—Cd1i74.97 (11)O1—Cd1—C11—O10177.20 (16)
O18—Cd1—O9—C1121.0 (4)O17—Cd1—C11—O1092.60 (19)
O1—Cd1—O9—C11175.02 (18)O9—Cd1—C11—O10177.2 (3)
O17—Cd1—O9—C1193.29 (19)O1i—Cd1—C11—O10104.99 (18)
O10—Cd1—O9—C111.57 (16)O18—Cd1—C11—O9168.2 (2)
O1i—Cd1—O9—C1197.41 (18)O1—Cd1—C11—O95.6 (2)
O18—Cd1—O10—C11168.1 (2)O17—Cd1—C11—O984.60 (19)
O1—Cd1—O10—C114.3 (2)O10—Cd1—C11—O9177.2 (3)
O17—Cd1—O10—C1186.19 (19)O1i—Cd1—C11—O977.82 (18)
O9—Cd1—O10—C111.58 (16)O18—Cd1—C11—C1588.0 (16)
O1i—Cd1—O10—C1173.30 (18)O1—Cd1—C11—C1574.6 (16)
O5ii—Cd2—O13—C13154.2 (3)O17—Cd1—C11—C15164.8 (16)
O19—Cd2—O13—C1340.1 (3)O9—Cd1—C11—C1580.2 (16)
O7iii—Cd2—O13—C13120.6 (3)O10—Cd1—C11—C15102.6 (16)
O16iv—Cd2—O13—C1364.6 (3)O1i—Cd1—C11—C152.4 (16)
O15iv—Cd2—O13—C1370.9 (3)Cd3v—O11—C12—O122.5 (3)
C14iv—Cd2—O13—C1369.5 (3)Cd3v—O11—C12—C16178.1 (3)
O20—Cd3—O14—C13156.7 (2)Cd3v—O12—C12—O112.9 (4)
O12v—Cd3—O14—C1335.8 (3)Cd3v—O12—C12—C16177.7 (2)
O3vi—Cd3—O14—C1360.3 (2)Cd2—O13—C13—O147.2 (4)
O4vi—Cd3—O14—C13115.0 (2)Cd2—O13—C13—C18177.81 (18)
O11v—Cd3—O14—C1377.0 (2)Cd3—O14—C13—O13157.5 (2)
C2vi—Cd3—O14—C1388.3 (2)Cd3—O14—C13—C1817.3 (4)
Cd1—O1—C1—O2163.6 (2)Cd2iv—O16—C14—O155.0 (3)
Cd1i—O1—C1—O247.2 (4)Cd2iv—O16—C14—C19176.2 (2)
Cd1—O1—C1—C521.1 (4)Cd2iv—O15—C14—O164.8 (3)
Cd1i—O1—C1—C5128.2 (2)Cd2iv—O15—C14—C19176.4 (2)
Cd3vi—O3—C2—O45.3 (3)O10—C11—C15—C2073.4 (4)
Cd3vi—O3—C2—C7170.8 (2)O9—C11—C15—C20101.0 (3)
Cd3vi—O4—C2—O34.9 (3)Cd1—C11—C15—C2025.0 (17)
Cd3vi—O4—C2—C7171.1 (2)O10—C11—C15—C16109.7 (3)
Cd2vii—O5—C3—O694.5 (4)O9—C11—C15—C1675.8 (4)
Cd2vii—O5—C3—C886.6 (3)Cd1—C11—C15—C16151.9 (14)
Cd2iii—O7—C4—O83.3 (4)C20—C15—C16—C171.2 (4)
Cd2iii—O7—C4—C10178.7 (2)C11—C15—C16—C17175.6 (3)
O2—C1—C5—C6116.5 (3)C20—C15—C16—C12177.0 (3)
O1—C1—C5—C659.1 (4)C11—C15—C16—C126.2 (4)
O2—C1—C5—C1055.2 (4)O11—C12—C16—C17153.6 (3)
O1—C1—C5—C10129.1 (3)O12—C12—C16—C1725.8 (5)
C10—C5—C6—C73.8 (4)O11—C12—C16—C1524.6 (5)
C1—C5—C6—C7168.4 (3)O12—C12—C16—C15155.9 (3)
C5—C6—C7—C80.7 (4)C15—C16—C17—C181.2 (5)
C5—C6—C7—C2174.6 (3)C12—C16—C17—C18177.0 (3)
O3—C2—C7—C8143.9 (3)C16—C17—C18—C190.3 (5)
O4—C2—C7—C839.9 (4)C16—C17—C18—C13179.2 (3)
Cd3vi—C2—C7—C8158.4 (12)O13—C13—C18—C1779.5 (3)
O3—C2—C7—C641.1 (4)O14—C13—C18—C1795.8 (3)
O4—C2—C7—C6135.1 (3)O13—C13—C18—C19101.0 (3)
Cd3vi—C2—C7—C616.6 (15)O14—C13—C18—C1983.7 (4)
C6—C7—C8—C92.3 (4)C17—C18—C19—C200.5 (4)
C2—C7—C8—C9177.2 (3)C13—C18—C19—C20179.9 (3)
C6—C7—C8—C3177.5 (3)C17—C18—C19—C14179.3 (3)
C2—C7—C8—C32.7 (5)C13—C18—C19—C141.2 (4)
O6—C3—C8—C7132.8 (3)O16—C14—C19—C2011.6 (4)
O5—C3—C8—C746.2 (4)O15—C14—C19—C20167.3 (3)
O6—C3—C8—C947.1 (4)Cd2iv—C14—C19—C2067 (3)
O5—C3—C8—C9133.9 (3)O16—C14—C19—C18169.6 (3)
C7—C8—C9—C102.3 (4)O15—C14—C19—C1811.5 (4)
C3—C8—C9—C10177.5 (3)Cd2iv—C14—C19—C18114 (3)
C8—C9—C10—C50.8 (4)C16—C15—C20—C190.4 (4)
C8—C9—C10—C4176.9 (3)C11—C15—C20—C19176.6 (3)
C6—C5—C10—C93.8 (4)C18—C19—C20—C150.5 (4)
C1—C5—C10—C9167.7 (3)C14—C19—C20—C15179.4 (3)
Symmetry codes: (i) x, y, z; (ii) x, y+1, z1; (iii) x, y+1, z; (iv) x+1, y+1, z1; (v) x+1, y+1, z; (vi) x+1, y, z; (vii) x, y1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O11—H11···O220.822.162.895 (4)149
O17—H17C···O80.842.323.158 (4)179
O18—H18B···O30.852.503.292 (4)156
O2—H2···O10i0.822.533.237 (3)145
O18—H18A···O10vi0.852.193.031 (4)168
O24—H24B···O15v0.852.092.841 (4)147
O19—H19A···O23ii0.851.922.720 (4)157
O17—H17B···O23viii0.852.293.073 (5)155
O19—H19B···O6ix0.851.852.698 (3)173
O20—H20B···O6ix0.852.182.996 (4)160
O20—H20C···O13x0.852.233.047 (4)161
O22—H22A···O2x0.852.052.807 (4)147
O23—H23B···O7x0.852.092.894 (4)158
O24—H24A···O4xi0.851.942.783 (4)173
O21—H21A···O9xii0.851.912.748 (4)168
O21—H21B···O12xiii0.851.942.765 (4)163
O22—H22B···O21xiv0.851.992.825 (4)166
O23—H23A···O2xv0.852.202.944 (4)147
Symmetry codes: (i) x, y, z; (ii) x, y+1, z1; (v) x+1, y+1, z; (vi) x+1, y, z; (viii) x+1, y, z+1; (ix) x+1, y+1, z1; (x) x+1, y, z; (xi) x+1, y+1, z; (xii) x, y+1, z+1; (xiii) x, y, z+1; (xiv) x+1, y+1, z+1; (xv) x, y, z+1.

Experimental details

Crystal data
Chemical formula[Cd3(C10H3O8)2(H2O)4]·4H2O
Mr983.58
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)8.3244 (17), 12.992 (3), 13.540 (3)
α, β, γ (°)85.79 (3), 84.67 (3), 87.17 (3)
V3)1452.6 (5)
Z2
Radiation typeMo Kα
µ (mm1)2.28
Crystal size (mm)0.20 × 0.17 × 0.16
Data collection
DiffractometerRigaku Saturn
diffractometer
Absorption correctionMulti-scan
(CrystalClear; Rigaku/MSC, 2004)
Tmin, Tmax0.658, 0.712
No. of measured, independent and
observed [I > 2σ(I)] reflections
18101, 6873, 6308
Rint0.022
(sin θ/λ)max1)0.658
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.029, 0.068, 1.05
No. of reflections6873
No. of parameters424
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.64, 0.84

Computer programs: CrystalClear (Rigaku/MSC, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008), publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O11—H11···O220.822.162.895 (4)149.1
O17—H17C···O80.842.323.158 (4)179.4
O18—H18B···O30.852.503.292 (4)155.7
O2—H2···O10i0.822.533.237 (3)145.3
O18—H18A···O10ii0.852.193.031 (4)167.7
O24—H24B···O15iii0.852.092.841 (4)147.3
O19—H19A···O23iv0.851.922.720 (4)157.1
O17—H17B···O23v0.852.293.073 (5)154.7
O19—H19B···O6vi0.851.852.698 (3)172.6
O20—H20B···O6vi0.852.182.996 (4)160.2
O20—H20C···O13vii0.852.233.047 (4)161.1
O22—H22A···O2vii0.852.052.807 (4)147.3
O23—H23B···O7vii0.852.092.894 (4)158.3
O24—H24A···O4viii0.851.942.783 (4)173.3
O21—H21A···O9ix0.851.912.748 (4)168.1
O21—H21B···O12x0.851.942.765 (4)162.7
O22—H22B···O21xi0.851.992.825 (4)166.1
O23—H23A···O2xii0.852.202.944 (4)146.9
Symmetry codes: (i) x, y, z; (ii) x+1, y, z; (iii) x+1, y+1, z; (iv) x, y+1, z1; (v) x+1, y, z+1; (vi) x+1, y+1, z1; (vii) x+1, y, z; (viii) x+1, y+1, z; (ix) x, y+1, z+1; (x) x, y, z+1; (xi) x+1, y+1, z+1; (xii) x, y, z+1.
 

Acknowledgements

The study was supported by the Science and Technology Department of Henan Province (082102330003).

References

First citationLin, J.-D., Cheng, J.-W. & Du, S.-W. (2008). Cryst. Growth Des. 8, 3345–3353.  Web of Science CrossRef CAS Google Scholar
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ISSN: 2056-9890
Volume 68| Part 6| June 2012| Pages m801-m802
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