A one-dimensional zigzag coordination polymer: catena-poly[[[triaqua­cadmium(II)]-[μ-2,2′-(5-methyl-1,3-phenyl­enedi­oxy)diacetato-κ4O,O′:O′′,O′′′]] monohydrate]

Lin, Y.; Wei, Y.; Wei, X.-W.; Zhang, H.-T.

doi:10.1107/S1600536807068031

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 2| February 2008| Pages m280-m281

doi:10.1107/S1600536807068031

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A one-dimensional zigzag coordination polymer: catena-poly[[[triaquacadmium(II)]-[μ-2,2′-(5-methyl-1,3-phenylenedioxy)diacetato-κ⁴O,O′:O′′,O′′′]] monohydrate]

Ying Lin,^a Yun Wei,^a Xian-Wen Wei ^a and Hong-Tao Zhang ^a ^*

^aCollege of Chemistry and Materials Science, Anhui Key Laboratory of Functional Molecular Solids, Anhui Normal University, Wuhu 241000, People's Republic of China
^*Correspondence e-mail: zht2006@mail.ahnu.edu.cn

(Received 21 November 2007; accepted 21 December 2007; online 4 January 2008)

In the title one-dimensional coordination polymer, {[Cd(C₁₁H₁₀O₆)(H₂O)₃]·H₂O}_n, the 2,2′-(5-methyl-1,3-phenylenedioxy)diacetate dianions connect Cd^II ions in a head-to-tail fashion to generate zigzag chains. The coordination geometry of the Cd atom is distorted pentagonal bipyramidal. There are O—H⋯O hydrogen bonds between the carboxyl O atoms, the aqua ligands and the uncoordinated water molecules.

Related literature

For related literature on coordination polymers, see: Burrows et al. (2004 ); Hong et al. (2006 ); Janiak (2000 , 2003 ); Kitagawa et al. (2004 ); Moulton & Zaworotko (2001 ); Russell et al. (2001 ).

Experimental

Crystal data

[Cd(C₁₁H₁₀O₆)(H₂O)₃]·H₂O
M_r = 422.66
Triclinic, $[P \overline 1]$
a = 7.3792 (11) Å
b = 8.6946 (12) Å
c = 11.9495 (17) Å
α = 85.294 (19)°
β = 82.52 (2)°
γ = 88.44 (2)°
V = 757.47 (19) Å³
Z = 2
Mo Kα radiation
μ = 1.49 mm⁻¹
T = 298 (2) K
0.24 × 0.08 × 0.02 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.717, T_max = 0.971
5397 measured reflections
2647 independent reflections
2121 reflections with I > 2σ(I)
R_int = 0.037

Refinement

R[F² > 2σ(F²)] = 0.040
wR(F²) = 0.093
S = 0.98
2647 reflections
200 parameters
H-atom parameters constrained
Δρ_max = 0.41 e Å⁻³
Δρ_min = −0.75 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Cd—O9	2.262 (4)
Cd—O7	2.297 (4)
Cd—O1	2.303 (3)
Cd—O6ⁱ	2.331 (4)
Cd—O8	2.381 (4)
Cd—O5ⁱ	2.432 (4)
Cd—O2	2.573 (4)

O9—Cd—O7	167.09 (14)
O9—Cd—O1	85.66 (14)
O9—Cd—O8	92.24 (14)
O7—Cd—O8	88.31 (14)
O1—Cd—O8	130.96 (13)
O6ⁱ—Cd—O8	80.48 (13)
O9—Cd—O5ⁱ	88.92 (13)
O9—Cd—O2	83.86 (14)
O8—Cd—O2	77.69 (12)
O5ⁱ—Cd—O2	146.90 (12)
Symmetry code: (i) x-1, y, z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7B⋯O8ⁱⁱ	0.85	2.08	2.875 (5)	156
O7—H7C⋯O5ⁱⁱⁱ	0.85	2.00	2.846 (5)	174
O8—H8C⋯O9^iv	0.85	2.51	3.263 (5)	148
O8—H8C⋯O10^v	0.85	2.38	3.008 (7)	131
O8—H8D⋯O2^iv	0.85	2.14	2.808 (5)	136
O9—H9E⋯O1^vi	0.85	1.92	2.752 (5)	165
O9—H9F⋯O10^vii	0.85	2.10	2.659 (6)	123
O10—H10C⋯O6	0.85	2.08	2.731 (6)	133
O10—H10D⋯O2^v	0.85	1.95	2.793 (6)	170
Symmetry codes: (ii) -x-1, -y, -z+2; (iii) -x, -y+1, -z+1; (iv) -x, -y, -z+2; (v) -x, -y, -z+1; (vi) -x, -y+1, -z+2; (vii) x, y, z+1.

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 (Sheldrick, 2000 ); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807068031/ob2104sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536807068031/ob2104Isup2.hkl

checkCIF report

Comment top

Supramolecular self-assembly of coordination polymers have been one of the areas of rapid growth in chemistry recently, owing to their intriguing molecular topologies and useful properties, such as molecular recognition, electronic, optical, magnetic and catalytic properties (Janiak, 2003; Kitagawa et al., 2004). Generally, the structure of such a molecular architecture is governed by coordination interaction and other non-covalent interactions such as hydrogen bonding and π-π stacking as well as the conformations of ligands depending on their rigidity and flexibility (Russell et al., 2001; Moulton & Zaworotko, 2001; Burrows et al., 2004). To date, there is a great research interest focused on the coordination interaction, hydrogen bonding and π-π stacking as well as the rigidity of ligands, whereas there is scant attention to the influence of the flexibility of ligands on the structure of coordination polymer. In order to further understand the role of the flexibility of ligands in the self-assembly of coordination polymers, we have designed and synthesized a ligand bearing the flexible group, 2,2'-(5-methyl-1,3-phenylenedioxy)diacetic acid (abbreviated to H₂5-mpdoa), and employed it with Cd^II ion to assemble the title coordination polymer, (I), [Cd(5-mpdoa)(H₂O)₃]_n^.nH₂O.

As shown in Fig. 1, the coordination geometry of the Cd^II atom is a distorted pentagonal bipyramid. The equatorial positions are occupied by four carboxyl O atoms (O1, O2, O5ⁱ, O6ⁱ, symmetry code (i) x - 1, y, z + 1) from two symmetry related 5-mpdoa ligands and the aqua O8 atom. The aqua O7 and O9 atoms are located at the axial vertices of the pentagonal bipyramid. Both two carboxylate groups of the 5-mpdoa ligands, O1/C1/O2 and O5ⁱ/C11ⁱ/O6ⁱ, chelate the Cd^IIatom in the same mode. The O5/C11/O6 carboxylate is almost coplanar with the benzene ring C3—C8, whereas the O1/C1/O2 carboxylate has a slightly twisted from the benzene ring with the dihedral angle of 10.7 (7)°. Due to the flexibility of the molecule induced by the σ-rotation of the C—O bond (selected torsion angles are listed in Table 1), the 5-mpdoa ligand adopts a W-shape conformation.

The 5-mpdoa ligands connect the neighbouring Cd^II atoms in a head-to-tail mode to construct an infinite zigzag chain which runs along the [101] direction. Such a supramolecular geometry could be regarded as a result of the cooperation of coordination interaction, the symmetry and the flexibility of ligand molecule as well as the hydrogen bonds. All zigzag chains are packing together through an amount of hydrogen bonding interactions between the carboxyl O atoms, the aqua ligands and the lattice water molecules (Fig. 2, Table 2). The shortest center-center distance between two adjacent benzene rings of the different chains is 4.997 (15) Å, indicating no interchain π-π interaction of 5-mpdoa (Janiak et al., 2000).

Related literature top

For related literature on coordination polymers, see: Burrows et al. (2004); Hong et al. (2006); Janiak (2000, 2003); Kitagawa et al. (2004); Moulton & Zaworotko (2001); Russell et al. (2001).

Experimental top

The H₂5-mpdoa ligand, 2,2'-(5-methyl-1,3-phenylenedioxy)diacetic acid, was synthesized from 5-methylbenzene-1,3-diol and 2-chloroacetic acid according to a literature method reported by Hong et al. (2006). Cd(CH₃COO)₂^.2(H₂O) (26.8 mg, 0.10 mmol) and H₂5-mpdoa (24.0 mg, 0.10 mmol) were dissolved in 10 ml water. The resulting yellow solution was filtered and the filtrate was left at room temperature. Yellow column-like crystals were obtained (25.5 mg, yield ca 60%) after several weeks by slow evaporation of the solvent.

Computing details top

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

Figures top

	Fig. 1. A drawing of the asymmetric unit of (I) (solid line portion) with displacement ellipsoids at the 30% probability level. [symmetry code: (i) x - 1, y, z + 1].
	Fig. 2. A packing diagram of (I) viewed down the c axis. Dotted lines show O—H^···O hydrogen bonds. All hydrogen atoms have been omitted for clarity.

catena-poly[[[triaquacadmium(II)]-[µ-2,2'-(5-methyl-1,3- phenylenedioxy)diacetato-κ⁴O,O':O'',O''']] monohydrate] top

Crystal data top

[Cd(C₁₁H₁₀O₆)(H₂O)₃]·H₂O	Z = 2
M_r = 422.66	F(000) = 424
Triclinic, P1	D_x = 1.853 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.3792 (11) Å	Cell parameters from 1908 reflections
b = 8.6946 (12) Å	θ = 2.4–25.5°
c = 11.9495 (17) Å	µ = 1.49 mm⁻¹
α = 85.294 (19)°	T = 298 K
β = 82.52 (2)°	Column, yellow
γ = 88.44 (2)°	0.24 × 0.08 × 0.02 mm
V = 757.47 (19) Å³

Data collection top

Bruker SMART CCD area-detector diffractometer	2647 independent reflections
Radiation source: fine-focus sealed tube	2121 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.037
ϕ and ω scans	θ_max = 25.0°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −8→8
T_min = 0.717, T_max = 0.971	k = −10→10
5397 measured reflections	l = −14→14

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)] = 0.040	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.093	H-atom parameters constrained
S = 0.98	w = 1/[σ²(F_o²) + (0.0479P)²] where P = (F_o² + 2F_c²)/3
2647 reflections	(Δ/σ)_max = 0.001
200 parameters	Δρ_max = 0.41 e Å⁻³
0 restraints	Δρ_min = −0.75 e Å⁻³

Crystal data top

[Cd(C₁₁H₁₀O₆)(H₂O)₃]·H₂O	γ = 88.44 (2)°
M_r = 422.66	V = 757.47 (19) Å³
Triclinic, P1	Z = 2
a = 7.3792 (11) Å	Mo Kα radiation
b = 8.6946 (12) Å	µ = 1.49 mm⁻¹
c = 11.9495 (17) Å	T = 298 K
α = 85.294 (19)°	0.24 × 0.08 × 0.02 mm
β = 82.52 (2)°

Data collection top

Bruker SMART CCD area-detector diffractometer	2647 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	2121 reflections with I > 2σ(I)
T_min = 0.717, T_max = 0.971	R_int = 0.037
5397 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.040	0 restraints
wR(F²) = 0.093	H-atom parameters constrained
S = 0.98	Δρ_max = 0.41 e Å⁻³
2647 reflections	Δρ_min = −0.75 e Å⁻³
200 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

	x	y	z	U_iso*/U_eq
C1	−0.0333 (7)	0.3276 (6)	0.8172 (4)	0.0364 (12)
C2	0.0773 (7)	0.3784 (6)	0.7048 (4)	0.0357 (12)
H2A	0.2052	0.3511	0.7070	0.043*
H2B	0.0346	0.3267	0.6445	0.043*
C3	0.1556 (6)	0.6127 (6)	0.5904 (4)	0.0304 (11)
C4	0.2445 (6)	0.5368 (5)	0.5016 (4)	0.0289 (11)
H4	0.2422	0.4298	0.5022	0.035*
C5	0.3370 (6)	0.6246 (6)	0.4120 (4)	0.0301 (11)
C6	0.3419 (6)	0.7843 (6)	0.4103 (4)	0.0339 (12)
H6	0.4059	0.8411	0.3491	0.041*
C7	0.2513 (7)	0.8586 (6)	0.4997 (5)	0.0350 (12)
C8	0.1596 (7)	0.7715 (6)	0.5901 (4)	0.0358 (12)
H8	0.0999	0.8201	0.6514	0.043*
C9	0.2558 (8)	1.0326 (6)	0.5005 (5)	0.0515 (15)
H9A	0.1448	1.0770	0.4773	0.061*
H9B	0.3583	1.0715	0.4492	0.061*
H9C	0.2671	1.0595	0.5756	0.061*
C10	0.4195 (7)	0.4039 (5)	0.3083 (4)	0.0348 (12)
H10A	0.2934	0.3767	0.3065	0.042*
H10B	0.4627	0.3468	0.3732	0.042*
C11	0.5344 (6)	0.3625 (7)	0.2014 (4)	0.0363 (13)
Cd	−0.24893 (5)	0.25748 (4)	1.02124 (3)	0.03576 (16)
O1	−0.1211 (5)	0.4250 (4)	0.8748 (3)	0.0411 (9)
O2	−0.0333 (5)	0.1860 (4)	0.8455 (3)	0.0499 (10)
O3	0.0573 (5)	0.5399 (4)	0.6840 (3)	0.0387 (9)
O4	0.4307 (5)	0.5637 (4)	0.3184 (3)	0.0383 (9)
O5	0.6157 (5)	0.4624 (4)	0.1334 (3)	0.0455 (9)
O6	0.5458 (5)	0.2198 (4)	0.1862 (3)	0.0500 (10)
O7	−0.4729 (5)	0.2338 (5)	0.9073 (3)	0.0635 (12)
H7B	−0.5520	0.1705	0.9401	0.076*
H7C	−0.5233	0.3214	0.8950	0.076*
O8	−0.2346 (5)	−0.0167 (4)	1.0480 (3)	0.0570 (11)
H8C	−0.1671	−0.0518	0.9923	0.069*
H8D	−0.1896	−0.0430	1.1088	0.069*
O9	0.0139 (5)	0.2816 (4)	1.0963 (3)	0.0580 (11)
H9E	0.0262	0.3754	1.1086	0.069*
H9F	0.0093	0.2255	1.1580	0.069*
O10	0.2207 (6)	0.0730 (5)	0.1980 (4)	0.0801 (15)
H10C	0.3344	0.0701	0.1748	0.096*
H10D	0.1737	−0.0127	0.1891	0.096*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.028 (3)	0.047 (3)	0.034 (3)	−0.010 (2)	−0.003 (2)	−0.001 (3)
C2	0.040 (3)	0.035 (3)	0.031 (3)	−0.001 (2)	0.000 (2)	−0.002 (2)
C3	0.030 (3)	0.036 (3)	0.024 (3)	−0.004 (2)	−0.001 (2)	0.002 (2)
C4	0.029 (3)	0.027 (3)	0.031 (3)	−0.002 (2)	−0.003 (2)	−0.003 (2)
C5	0.027 (3)	0.039 (3)	0.025 (3)	−0.001 (2)	−0.002 (2)	−0.003 (2)
C6	0.030 (3)	0.037 (3)	0.031 (3)	−0.005 (2)	0.004 (2)	0.000 (2)
C7	0.034 (3)	0.030 (3)	0.043 (3)	−0.003 (2)	−0.010 (2)	−0.003 (2)
C8	0.043 (3)	0.032 (3)	0.032 (3)	0.008 (2)	−0.001 (2)	−0.008 (2)
C9	0.050 (4)	0.035 (3)	0.067 (4)	−0.002 (3)	0.003 (3)	−0.006 (3)
C10	0.034 (3)	0.036 (3)	0.032 (3)	−0.005 (2)	0.004 (2)	−0.001 (2)
C11	0.027 (3)	0.057 (4)	0.026 (3)	0.004 (3)	−0.002 (2)	−0.007 (3)
Cd	0.0367 (2)	0.0382 (2)	0.0297 (2)	−0.00158 (16)	0.00579 (15)	−0.00233 (16)
O1	0.043 (2)	0.046 (2)	0.030 (2)	−0.0051 (18)	0.0085 (17)	0.0003 (17)
O2	0.059 (3)	0.038 (2)	0.050 (3)	−0.0106 (19)	−0.003 (2)	0.0085 (19)
O3	0.047 (2)	0.0324 (19)	0.031 (2)	0.0022 (16)	0.0131 (16)	−0.0004 (16)
O4	0.051 (2)	0.031 (2)	0.029 (2)	−0.0055 (16)	0.0096 (17)	−0.0030 (16)
O5	0.045 (2)	0.053 (2)	0.033 (2)	0.0000 (19)	0.0115 (17)	−0.0003 (18)
O6	0.058 (3)	0.040 (2)	0.050 (3)	−0.0003 (19)	0.0103 (19)	−0.0144 (19)
O7	0.060 (3)	0.059 (3)	0.072 (3)	−0.022 (2)	−0.023 (2)	0.023 (2)
O8	0.047 (2)	0.046 (2)	0.072 (3)	0.0030 (19)	0.006 (2)	0.005 (2)
O9	0.070 (3)	0.048 (2)	0.062 (3)	−0.001 (2)	−0.023 (2)	−0.013 (2)
O10	0.078 (3)	0.047 (3)	0.124 (4)	−0.006 (2)	−0.044 (3)	−0.008 (3)

Geometric parameters (Å, º) top

C1—O1	1.249 (6)	C10—O4	1.409 (5)
C1—O2	1.250 (6)	C10—C11	1.503 (7)
C1—C2	1.517 (7)	C10—H10A	0.9700
C1—Cd	2.766 (5)	C10—H10B	0.9700
C2—O3	1.413 (6)	C11—O5	1.249 (6)
C2—H2A	0.9700	C11—O6	1.268 (6)
C2—H2B	0.9700	C11—Cdⁱ	2.715 (5)
C3—O3	1.370 (6)	Cd—O9	2.262 (4)
C3—C4	1.379 (7)	Cd—O7	2.297 (4)
C3—C8	1.382 (7)	Cd—O1	2.303 (3)
C4—C5	1.378 (7)	Cd—O6ⁱⁱ	2.331 (4)
C4—H4	0.9300	Cd—O8	2.381 (4)
C5—O4	1.374 (5)	Cd—O5ⁱⁱ	2.432 (4)
C5—C6	1.388 (7)	Cd—O2	2.573 (4)
C6—C7	1.382 (7)	O7—H7B	0.8489
C6—H6	0.9300	O7—H7C	0.8491
C7—C8	1.379 (7)	O8—H8C	0.8499
C7—C9	1.515 (7)	O8—H8D	0.8492
C8—H8	0.9300	O9—H9E	0.8495
C9—H9A	0.9600	O9—H9F	0.8482
C9—H9B	0.9600	O10—H10C	0.8492
C9—H9C	0.9600	O10—H10D	0.8499

O1—C1—O2	123.5 (5)	O7—Cd—O1	84.25 (13)
O1—C1—C2	120.1 (5)	O9—Cd—O6ⁱⁱ	100.20 (15)
O2—C1—C2	116.4 (5)	O7—Cd—O6ⁱⁱ	92.61 (15)
O1—C1—Cd	55.6 (3)	O1—Cd—O6ⁱⁱ	148.09 (13)
O2—C1—Cd	68.0 (3)	O9—Cd—O8	92.24 (14)
C2—C1—Cd	175.5 (4)	O7—Cd—O8	88.31 (14)
O3—C2—C1	109.0 (4)	O1—Cd—O8	130.96 (13)
O3—C2—H2A	109.9	O6ⁱⁱ—Cd—O8	80.48 (13)
C1—C2—H2A	109.9	O9—Cd—O5ⁱⁱ	88.92 (13)
O3—C2—H2B	109.9	O7—Cd—O5ⁱⁱ	99.79 (15)
C1—C2—H2B	109.9	O1—Cd—O5ⁱⁱ	93.99 (12)
H2A—C2—H2B	108.3	O6ⁱⁱ—Cd—O5ⁱⁱ	55.16 (12)
O3—C3—C4	123.9 (4)	O8—Cd—O5ⁱⁱ	135.00 (13)
O3—C3—C8	114.8 (4)	O9—Cd—O2	83.86 (14)
C4—C3—C8	121.3 (5)	O7—Cd—O2	83.67 (14)
C3—C4—C5	117.8 (4)	O1—Cd—O2	53.34 (12)
C3—C4—H4	121.1	O6ⁱⁱ—Cd—O2	157.94 (13)
C5—C4—H4	121.1	O8—Cd—O2	77.69 (12)
O4—C5—C4	123.7 (4)	O5ⁱⁱ—Cd—O2	146.90 (12)
O4—C5—C6	114.6 (4)	O9—Cd—C11ⁱⁱ	94.48 (14)
C4—C5—C6	121.7 (5)	O7—Cd—C11ⁱⁱ	97.62 (15)
C5—C6—C7	119.8 (5)	O1—Cd—C11ⁱⁱ	121.12 (15)
C5—C6—H6	120.1	O6ⁱⁱ—Cd—C11ⁱⁱ	27.78 (14)
C7—C6—H6	120.1	O8—Cd—C11ⁱⁱ	107.90 (16)
C8—C7—C6	118.9 (4)	O5ⁱⁱ—Cd—C11ⁱⁱ	27.38 (14)
C8—C7—C9	120.1 (5)	O2—Cd—C11ⁱⁱ	174.26 (15)
C6—C7—C9	120.9 (5)	O9—Cd—C1	84.11 (15)
C7—C8—C3	120.5 (5)	O7—Cd—C1	83.27 (14)
C7—C8—H8	119.7	O1—Cd—C1	26.58 (14)
C3—C8—H8	119.7	O6ⁱⁱ—Cd—C1	173.43 (14)
C7—C9—H9A	109.5	O8—Cd—C1	104.43 (15)
C7—C9—H9B	109.5	O5ⁱⁱ—Cd—C1	120.41 (15)
H9A—C9—H9B	109.5	O2—Cd—C1	26.77 (13)
C7—C9—H9C	109.5	C11ⁱⁱ—Cd—C1	147.67 (18)
H9A—C9—H9C	109.5	C1—O1—Cd	97.9 (3)
H9B—C9—H9C	109.5	C1—O2—Cd	85.3 (3)
O4—C10—C11	109.4 (4)	C3—O3—C2	119.1 (4)
O4—C10—H10A	109.8	C5—O4—C10	118.4 (4)
C11—C10—H10A	109.8	C11—O5—Cdⁱ	89.0 (3)
O4—C10—H10B	109.8	C11—O6—Cdⁱ	93.2 (3)
C11—C10—H10B	109.8	Cd—O7—H7B	109.4
H10A—C10—H10B	108.3	Cd—O7—H7C	109.2
O5—C11—O6	122.5 (5)	H7B—O7—H7C	109.7
O5—C11—C10	121.9 (5)	Cd—O8—H8C	109.3
O6—C11—C10	115.6 (5)	Cd—O8—H8D	109.2
O5—C11—Cdⁱ	63.6 (3)	H8C—O8—H8D	109.6
O6—C11—Cdⁱ	59.0 (3)	Cd—O9—H9E	109.2
C10—C11—Cdⁱ	173.6 (4)	Cd—O9—H9F	109.1
O9—Cd—O7	167.09 (14)	H9E—O9—H9F	109.7
O9—Cd—O1	85.66 (14)	H10C—O10—H10D	109.6

O1—C1—C2—O3	−0.6 (7)	O2—C1—O1—Cd	0.1 (6)
O2—C1—C2—O3	177.9 (4)	C2—C1—O1—Cd	178.5 (4)
O3—C3—C4—C5	179.3 (4)	O9—Cd—O1—C1	85.5 (3)
C8—C3—C4—C5	−0.3 (7)	O7—Cd—O1—C1	−86.4 (3)
C3—C4—C5—O4	−179.9 (4)	O6ⁱⁱ—Cd—O1—C1	−172.1 (3)
C3—C4—C5—C6	0.1 (7)	O8—Cd—O1—C1	−3.7 (4)
O4—C5—C6—C7	179.5 (4)	O5ⁱⁱ—Cd—O1—C1	174.1 (3)
C4—C5—C6—C7	−0.5 (7)	O2—Cd—O1—C1	−0.1 (3)
C5—C6—C7—C8	0.9 (7)	C11ⁱⁱ—Cd—O1—C1	178.1 (3)
C5—C6—C7—C9	179.4 (5)	O1—C1—O2—Cd	−0.1 (5)
C6—C7—C8—C3	−1.1 (7)	C2—C1—O2—Cd	−178.5 (4)
C9—C7—C8—C3	−179.6 (5)	O9—Cd—O2—C1	−89.1 (3)
O3—C3—C8—C7	−178.9 (4)	O7—Cd—O2—C1	87.6 (3)
C4—C3—C8—C7	0.8 (7)	O1—Cd—O2—C1	0.1 (3)
O4—C10—C11—O5	−3.2 (7)	O6ⁱⁱ—Cd—O2—C1	168.9 (3)
O4—C10—C11—O6	175.4 (4)	O8—Cd—O2—C1	177.3 (3)
O1—C1—Cd—O9	−92.1 (3)	O5ⁱⁱ—Cd—O2—C1	−10.6 (4)
O2—C1—Cd—O9	88.0 (3)	C4—C3—O3—C2	14.2 (7)
O1—C1—Cd—O7	90.6 (3)	C8—C3—O3—C2	−166.1 (4)
O2—C1—Cd—O7	−89.3 (3)	C1—C2—O3—C3	175.6 (4)
O2—C1—Cd—O1	−179.9 (5)	C4—C5—O4—C10	5.6 (7)
O1—C1—Cd—O8	177.1 (3)	C6—C5—O4—C10	−174.4 (4)
O2—C1—Cd—O8	−2.8 (3)	C11—C10—O4—C5	−179.0 (4)
O1—C1—Cd—O5ⁱⁱ	−6.8 (4)	O6—C11—O5—Cdⁱ	−2.4 (5)
O2—C1—Cd—O5ⁱⁱ	173.3 (3)	C10—C11—O5—Cdⁱ	176.1 (4)
O1—C1—Cd—O2	179.9 (5)	O5—C11—O6—Cdⁱ	2.5 (5)
O1—C1—Cd—C11ⁱⁱ	−3.0 (5)	C10—C11—O6—Cdⁱ	−176.1 (4)
O2—C1—Cd—C11ⁱⁱ	177.1 (3)

Symmetry codes: (i) x+1, y, z−1; (ii) x−1, y, z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7B···O8ⁱⁱⁱ	0.85	2.08	2.875 (5)	156
O7—H7C···O5^iv	0.85	2.00	2.846 (5)	174
O8—H8C···O9^v	0.85	2.51	3.263 (5)	148
O8—H8C···O10^vi	0.85	2.38	3.008 (7)	131
O8—H8D···O2^v	0.85	2.14	2.808 (5)	136
O9—H9E···O1^vii	0.85	1.92	2.752 (5)	165
O9—H9F···O10^viii	0.85	2.10	2.659 (6)	123
O10—H10C···O6	0.85	2.08	2.731 (6)	133
O10—H10D···O2^vi	0.85	1.95	2.793 (6)	170

Symmetry codes: (iii) −x−1, −y, −z+2; (iv) −x, −y+1, −z+1; (v) −x, −y, −z+2; (vi) −x, −y, −z+1; (vii) −x, −y+1, −z+2; (viii) x, y, z+1.

Experimental details

Crystal data
Chemical formula	[Cd(C₁₁H₁₀O₆)(H₂O)₃]·H₂O
M_r	422.66
Crystal system, space group	Triclinic, P1
Temperature (K)	298
a, b, c (Å)	7.3792 (11), 8.6946 (12), 11.9495 (17)
α, β, γ (°)	85.294 (19), 82.52 (2), 88.44 (2)
V (Å³)	757.47 (19)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.49
Crystal size (mm)	0.24 × 0.08 × 0.02

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.717, 0.971
No. of measured, independent and observed [I > 2σ(I)] reflections	5397, 2647, 2121
R_int	0.037
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.040, 0.093, 0.98
No. of reflections	2647
No. of parameters	200
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.41, −0.75

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Sheldrick, 2000).

Selected geometric parameters (Å, º) top

Cd—O9	2.262 (4)	Cd—O8	2.381 (4)
Cd—O7	2.297 (4)	Cd—O5ⁱ	2.432 (4)
Cd—O1	2.303 (3)	Cd—O2	2.573 (4)
Cd—O6ⁱ	2.331 (4)

O9—Cd—O7	167.09 (14)	O6ⁱ—Cd—O8	80.48 (13)
O9—Cd—O1	85.66 (14)	O9—Cd—O5ⁱ	88.92 (13)
O9—Cd—O8	92.24 (14)	O9—Cd—O2	83.86 (14)
O7—Cd—O8	88.31 (14)	O8—Cd—O2	77.69 (12)
O1—Cd—O8	130.96 (13)	O5ⁱ—Cd—O2	146.90 (12)

O1—C1—C2—O3	−0.6 (7)	C4—C3—O3—C2	14.2 (7)
O4—C10—C11—O5	−3.2 (7)	C4—C5—O4—C10	5.6 (7)

Symmetry code: (i) x−1, y, z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7B···O8ⁱⁱ	0.85	2.08	2.875 (5)	156.4
O7—H7C···O5ⁱⁱⁱ	0.85	2.00	2.846 (5)	173.8
O8—H8C···O9^iv	0.85	2.51	3.263 (5)	148.0
O8—H8C···O10^v	0.85	2.38	3.008 (7)	131.0
O8—H8D···O2^iv	0.85	2.14	2.808 (5)	135.8
O9—H9E···O1^vi	0.85	1.92	2.752 (5)	164.9
O9—H9F···O10^vii	0.85	2.10	2.659 (6)	123.3
O10—H10C···O6	0.85	2.08	2.731 (6)	132.6
O10—H10D···O2^v	0.85	1.95	2.793 (6)	169.5

Symmetry codes: (ii) −x−1, −y, −z+2; (iii) −x, −y+1, −z+1; (iv) −x, −y, −z+2; (v) −x, −y, −z+1; (vi) −x, −y+1, −z+2; (vii) x, y, z+1.

Acknowledgements

This work was funded by the Doctoral Research Launch Foundation of Anhui Normal University and the Youth Research Foundation of Anhui Normal University (grant No. 2006xqn64).

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