catena-Poly[[triaqua­cadmium(II)]-μ-pyridine-2,3-dicarboxyl­ato-κ3N,O2:O3]

Aghabozorg, H.; Motyeian, E.; Khadivi, R.; Ghadermazi, M.; Manteghi, F.

doi:10.1107/S160053680706850X

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 2| February 2008| Pages m320-m321

doi:10.1107/S160053680706850X

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catena-Poly[[triaquacadmium(II)]-μ-pyridine-2,3-dicarboxylato-κ³N,O²:O³]

Hossein Aghabozorg,^a ^* Elham Motyeian,^a Ramona Khadivi,^b Mohammad Ghadermazi ^c and Faranak Manteghi ^a

^aFaculty of Chemistry, Teacher Training University, 49 Mofateh Ave., 15614 Tehran, Iran, ^bDepartment of Chemistry, Islamic Azad University, North Tehran Branch, Tehran, Iran, and ^cDepartment of Chemistry, Faculty of Science, University of Kurdistan, Sanandaj, Iran
^*Correspondence e-mail: haghabozorg@yahoo.com

(Received 17 November 2007; accepted 27 December 2007; online 9 January 2008)

The title polymeric compound, [Cd(C₇H₃NO₄)(H₂O)₃]_n or [Cd(py-2,3-dc)(H₂O)₃]_n, where py-2,3-dcH₂ is pyridine-2,3-dicarboxylic acid, was obtained by the reaction of cadmium(II) nitrate hexahydrate with (pipzH₂)(py-2,3-dc) as a proton-transfer compound in aqueous solution (pipz is piperazine). The molecular structure shows that only the anionic fragment of the starting proton-transfer compound is present in the complex, while the (pipzH₂)²⁺ dication has been lost. Each (py-2,3-dc)²⁻ ligand bridges two Cd^II atoms in two different coordination modes, i.e. one end acts as a monodentate and the other end as a bidentate ligand. The three remaining coordination sites on the metal center are occupied by water molecules. The geometric arrangement of the six donor atoms around the Cd^II atom is distorted octahedral. In the crystal structure, O—H⋯O and C—H⋯O hydrogen bonds play an important role in stabilizing the supramolecular structure.

Related literature

For related ion pairs or complexes, see: Aghabozorg, Daneshvar, Motyeian et al. (2007 ); Aghabozorg et al. (2008 ); Manteghi et al. (2007 ); Aghabozorg, Sadr-khanlou et al. (2007 ); Li et al. (2004 ).

Experimental

Crystal data

[Cd(C₇H₃NO₄)(H₂O)₃]
M_r = 331.55
Orthorhombic, P c a 2₁
a = 16.820 (3) Å
b = 6.8076 (14) Å
c = 8.6658 (17) Å
V = 992.3 (3) Å³
Z = 4
Mo Kα radiation
μ = 2.22 mm⁻¹
T = 100 (2) K
0.40 × 0.08 × 0.05 mm

Data collection

Bruker APEX 1000 CCD area-detector diffractometer
Absorption correction: multi-scan (APEX2; Bruker, 2005 ) T_min = 0.810, T_max = 0.901
8990 measured reflections
2255 independent reflections
1848 reflections with I > 2σ(I)
R_int = 0.060

Refinement

R[F² > 2σ(F²)] = 0.029
wR(F²) = 0.056
S = 1.01
2255 reflections
151 parameters
7 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.61 e Å⁻³
Δρ_min = −0.84 e Å⁻³
Absolute structure: Flack (1983), 1042 Friedel pairs
Flack parameter: 0.05 (4)

Table 1
Selected geometric parameters (Å, °)

Cd1—O1W	2.254 (4)
Cd1—O2ⁱ	2.259 (3)
Cd1—O3W	2.274 (3)
Cd1—O4	2.279 (3)
Cd1—N1ⁱ	2.302 (4)
Cd1—O2W	2.385 (3)

O3W—Cd1—O4	156.89 (12)
O1W—Cd1—N1ⁱ	163.70 (14)
O2ⁱ—Cd1—O2W	171.30 (12)
Symmetry code: (i) $[-x+{\script{3\over 2}}, y, z-{\script{1\over 2}}]$ .

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1⋯O2Wⁱⁱ	0.85 (2)	1.99 (2)	2.782 (5)	155.61
O1W—H2⋯O3ⁱⁱⁱ	0.87 (2)	1.86 (2)	2.702 (5)	163.55
O2W—H3⋯O1ⁱⁱⁱ	0.88 (2)	1.85 (2)	2.731 (5)	177.88
O2W—H4⋯O3^iv	0.87 (2)	1.84 (2)	2.687 (5)	164.45
O3W—H5⋯O4ⁱⁱⁱ	0.86 (2)	1.86 (2)	2.712 (4)	171.29
O3W—H6⋯O1^v	0.87 (2)	1.89 (2)	2.735 (8)	164.32
C3—H3A⋯O1W^vi	0.95 (2)	2.49 (2)	3.420 (6)	165
Symmetry codes: (ii) $[-x+1, -y+1, z+{\script{1\over 2}}]$ ; (iii) $[-x+1, -y+1, z-{\script{1\over 2}}]$ ; (iv) $[-x+1, -y+2, z-{\script{1\over 2}}]$ ; (v) x, y, z-1; (vi) x, y+1, z.

Data collection: APEX2 (Bruker, 2005); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXTL (Sheldrick, 1998 ); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680706850X/su2028sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053680706850X/su2028Isup2.hkl

checkCIF report

Comment top

Recently, ion pairs or complexes related to the title compound have been reported (Aghabozorg, Daneshvar, Motyeian et al., 2007). Proton transfer from pyridine-2,3-dicarboxylic acid (py-2,3-dcH₂) to amines, such as piperazine (pipz) and propane-1,3-diamine (pn), resulted in the formation of novel systems (Aghabozorg, Manteghi et al., 2007 submitted; Manteghi et al., 2007). The resulting compounds, with some remaining sites as electron donors, can coordinate to metallic ions (Aghabozorg, Sadr-khanlou et al., 2007). The molecular structure of the title compound shows that only the anionic fragment of starting proton transfer compound is incorporated into the complex and that the (pipzH₂)²⁺ dication has been lost. Each cadmium(II) atom is coordinated by five O-atoms and one N-atom. The asymmetric unit consists of one cadmium, one bridging (py-2,3-dc)^2-and three coordinated water molecules (Fig. 1). The (py-2,3-dc)^2-groups bridge two cadmium ions by adopting two different coordination modes, bidentate and monodentate. The existance of both coordination modes is seldom found in pyridine multicarboxylate coordination polymers (Li et al. 2004). The bond lengths and bond angles of the equatorial bonds around the metal center with atoms N1A, O2A, O1W and O2W, and the axial bonds with atoms O4 and O3W, indicate that the geometric arrangement of the six donor atoms around the cadmium(II) atom is distorted octahedral (Table 1). It is noticeable that one of the carboxylate groups is almost coplannar with the pyridine ring and the other is perpendicular to it (Fig. 1). The formation of the polymeric chains along the c axis is illustrated in Fig. 2. There are a number of O—H···O hydrogen bonds (Table 2) involving the coordinated water molecules and other O-atoms, [D···A distances ranging from 2.685 (5) to 2.789 (5) Å], and a C—H···O bond [D···A distance of 3.430 (6) Å], that give rise to the formation of a three-dimensional network (Fig. 3).

Related literature top

For related ion pairs or complexes, see: Aghabozorg, Daneshvar, Motyeian et al. (2007); Aghabozorg et al. (2008); Manteghi et al. (2007); Aghabozorg, Sadr-khanlou et al. (2007); Li et al. (2004).

Experimental top

The proton transfer ion pair was prepared according to the literature (Aghabozorg et al., 2008, in press). A solution of Cd(NO₃)₂. 6H₂O (158 mg, 0.5 mmol) in water (20 ml) was added to a solution of (pipzH₂)(py- 2,3-dc) (253 mg, 1.0 mmol) in water (20 ml), in a 1:2 molar ratio. Colorless crystals of the title compound suitable for X-ray characterization were obtained after a few days at room temperature.

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: APEX2 (Bruker, 2005); data reduction: APEX2 (Bruker, 2005); program(s) used to solve structure: SHELXTL (Sheldrick, 1998); program(s) used to refine structure: SHELXTL (Sheldrick, 1998); molecular graphics: SHELXTL (Sheldrick, 1998); software used to prepare material for publication: SHELXTL (Sheldrick, 1998).

Figures top

	Fig. 1. Molecular structure of the title compound, showing the atom-numbering scheme and displacement ellipsoids at the 50% probability level. Hydrogen bonds are shown as dashed lines. Atoms marked with suffixes A—E are related by the symmetry codes (A) -x + 3/2, y, z - 1/2; (B) -x + 1, -y + 1, z + 1/2; (C) -x + 1, -y + 1, z - 1/2; (D) -x + 1, -y + 2, z - 1/2; (E) x, y, z - 1).
	Fig. 2. A view of the polymeric chain of the title compound extending along the c axis.
	Fig. 3. A view along the b axis of the crystal packing of the title compound [the hydrogen bonds are shown as dashed lines and the hydrogen atoms of the pyridine-2,3-dicarboxylates ligands are omitted for clarity].

catena-Poly[[triaquacadmium(II)]-µ-pyridine-2,3-dicarboxylato- κ³N,O²:O³] top

Crystal data top

[Cd(C₇H₃NO₄)(H₂O)₃]	F(000) = 648
M_r = 331.55	D_x = 2.219 Mg m⁻³
Orthorhombic, Pca2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2ac	Cell parameters from 1136 reflections
a = 16.820 (3) Å	θ = 3.0–24.6°
b = 6.8076 (14) Å	µ = 2.22 mm⁻¹
c = 8.6658 (17) Å	T = 100 K
V = 992.3 (3) Å³	Needle, colourless
Z = 4	0.40 × 0.08 × 0.05 mm

Data collection top

Bruker APEX 1000 CCD area-detector diffractometer	2255 independent reflections
Radiation source: fine-focus sealed tube	1848 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.060
ω scans	θ_max = 27.5°, θ_min = 2.4°
Absorption correction: multi-scan (APEX2; Bruker, 2005)	h = −21→21
T_min = 0.810, T_max = 0.901	k = −8→8
8990 measured reflections	l = −11→11

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F² > 2σ(F²)] = 0.029	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.056	w = 1/[σ²(F_o²) + (0.02P)²] where P = (F_o² + 2F_c²)/3
S = 1.01	(Δ/σ)_max = 0.001
2255 reflections	Δρ_max = 0.61 e Å⁻³
151 parameters	Δρ_min = −0.84 e Å⁻³
7 restraints	Absolute structure: Flack (1983), 1042 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.05 (4)

Crystal data top

[Cd(C₇H₃NO₄)(H₂O)₃]	V = 992.3 (3) Å³
M_r = 331.55	Z = 4
Orthorhombic, Pca2₁	Mo Kα radiation
a = 16.820 (3) Å	µ = 2.22 mm⁻¹
b = 6.8076 (14) Å	T = 100 K
c = 8.6658 (17) Å	0.40 × 0.08 × 0.05 mm

Data collection top

Bruker APEX 1000 CCD area-detector diffractometer	2255 independent reflections
Absorption correction: multi-scan (APEX2; Bruker, 2005)	1848 reflections with I > 2σ(I)
T_min = 0.810, T_max = 0.901	R_int = 0.060
8990 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.029	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.056	Δρ_max = 0.61 e Å⁻³
S = 1.01	Δρ_min = −0.84 e Å⁻³
2255 reflections	Absolute structure: Flack (1983), 1042 Friedel pairs
151 parameters	Absolute structure parameter: 0.05 (4)
7 restraints

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
Cd1	0.602315 (16)	0.57263 (4)	1.12348 (5)	0.01148 (8)
O1	0.64375 (15)	0.5438 (4)	1.6269 (10)	0.0146 (4)
O2	0.77114 (19)	0.4893 (5)	1.6812 (4)	0.0146 (4)
O3	0.55536 (18)	0.9159 (5)	1.5507 (4)	0.0139 (7)
O4	0.56140 (18)	0.7169 (5)	1.3472 (4)	0.0131 (8)
C1	0.7384 (3)	0.7512 (7)	1.5083 (6)	0.0114 (10)
C2	0.6813 (3)	0.8656 (7)	1.4333 (6)	0.0120 (11)
C3	0.7065 (3)	1.0220 (8)	1.3431 (7)	0.0110 (11)
H3A	0.6685	1.1023	1.2920	0.013*
C4	0.7868 (3)	1.0616 (8)	1.3272 (7)	0.0149 (11)
H4A	0.8050	1.1660	1.2636	0.018*
C5	0.8403 (3)	0.9424 (8)	1.4080 (6)	0.0168 (11)
H5A	0.8956	0.9694	1.4001	0.020*
C6	0.7166 (2)	0.5813 (6)	1.6146 (9)	0.0146 (4)
C7	0.5934 (3)	0.8271 (7)	1.4475 (5)	0.0113 (10)
N1	0.8168 (2)	0.7919 (6)	1.4961 (5)	0.0125 (9)
O1W	0.5482 (2)	0.2964 (6)	1.2211 (4)	0.0145 (8)
H1	0.526 (3)	0.302 (9)	1.309 (4)	0.022*
H2	0.509 (2)	0.227 (7)	1.183 (5)	0.022*
O2W	0.47743 (19)	0.6981 (5)	1.0383 (4)	0.0134 (7)
H3	0.439 (2)	0.618 (6)	1.065 (6)	0.020*
H4	0.464 (3)	0.818 (4)	1.060 (6)	0.020*
O3W	0.59058 (19)	0.3963 (5)	0.9018 (4)	0.0147 (8)
H5	0.5445 (19)	0.350 (8)	0.879 (7)	0.022*
H6	0.609 (3)	0.420 (8)	0.811 (3)	0.022*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.00902 (12)	0.01505 (14)	0.01036 (13)	−0.00047 (13)	0.0004 (3)	0.0018 (3)
O1	0.0109 (8)	0.0186 (11)	0.0144 (10)	0.0005 (8)	0.0029 (11)	0.0048 (12)
O2	0.0109 (8)	0.0186 (11)	0.0144 (10)	0.0005 (8)	0.0029 (11)	0.0048 (12)
O3	0.0112 (16)	0.0158 (18)	0.0146 (16)	−0.0006 (14)	0.0041 (13)	−0.0032 (16)
O4	0.0077 (16)	0.023 (2)	0.0084 (17)	−0.0019 (14)	0.0004 (14)	−0.0031 (16)
C1	0.011 (2)	0.012 (3)	0.011 (2)	−0.0042 (19)	−0.0063 (19)	−0.001 (2)
C2	0.010 (2)	0.014 (3)	0.012 (3)	−0.0018 (19)	0.000 (2)	−0.005 (2)
C3	0.009 (3)	0.013 (3)	0.011 (3)	0.004 (2)	0.000 (2)	−0.002 (2)
C4	0.014 (3)	0.016 (3)	0.014 (3)	−0.002 (2)	−0.001 (2)	0.005 (3)
C5	0.012 (3)	0.020 (3)	0.017 (3)	−0.004 (2)	0.000 (2)	−0.004 (3)
C6	0.0109 (8)	0.0186 (11)	0.0144 (10)	0.0005 (8)	0.0029 (11)	0.0048 (12)
C7	0.013 (2)	0.011 (3)	0.010 (2)	−0.001 (2)	−0.003 (2)	0.0057 (19)
N1	0.011 (2)	0.016 (2)	0.010 (2)	−0.0057 (17)	0.0018 (16)	−0.0007 (18)
O1W	0.0142 (18)	0.022 (2)	0.0070 (17)	−0.0081 (15)	0.0020 (14)	−0.0012 (16)
O2W	0.0127 (17)	0.0119 (19)	0.0156 (19)	0.0014 (14)	−0.0030 (14)	−0.0008 (17)
O3W	0.0113 (18)	0.023 (2)	0.0093 (16)	−0.0033 (15)	0.0003 (14)	−0.0040 (16)

Geometric parameters (Å, º) top

Cd1—O1W	2.254 (4)	C2—C7	1.506 (6)
Cd1—O2ⁱ	2.259 (3)	C3—C4	1.385 (6)
Cd1—O3W	2.274 (3)	C3—H3A	0.9500
Cd1—O4	2.279 (3)	C4—C5	1.400 (7)
Cd1—N1ⁱ	2.302 (4)	C4—H4A	0.9500
Cd1—O2W	2.385 (3)	C5—N1	1.338 (7)
O1—C6	1.256 (4)	C5—H5A	0.9500
O2—C6	1.252 (6)	N1—Cd1ⁱⁱ	2.302 (4)
O2—Cd1ⁱⁱ	2.259 (3)	O1W—H1	0.850 (19)
O3—C7	1.255 (6)	O1W—H2	0.869 (19)
O4—C7	1.268 (6)	O2W—H3	0.88 (2)
C1—N1	1.351 (6)	O2W—H4	0.866 (19)
C1—C2	1.397 (7)	O3W—H5	0.858 (19)
C1—C6	1.523 (7)	O3W—H6	0.87 (2)
C2—C3	1.387 (7)

O1W—Cd1—O2ⁱ	95.06 (13)	C2—C3—H3A	119.9
O1W—Cd1—O3W	80.89 (13)	C3—C4—C5	117.7 (5)
O2ⁱ—Cd1—O3W	97.84 (12)	C3—C4—H4A	121.1
O1W—Cd1—O4	85.31 (13)	C5—C4—H4A	121.1
O2ⁱ—Cd1—O4	101.79 (12)	N1—C5—C4	122.6 (5)
O3W—Cd1—O4	156.89 (12)	N1—C5—H5A	118.7
O1W—Cd1—N1ⁱ	163.70 (14)	C4—C5—H5A	118.7
O2ⁱ—Cd1—N1ⁱ	73.25 (13)	O2—C6—O1	125.0 (6)
O3W—Cd1—N1ⁱ	89.34 (14)	O2—C6—C1	118.8 (4)
O4—Cd1—N1ⁱ	107.87 (14)	O1—C6—C1	116.2 (5)
O1W—Cd1—O2W	93.38 (13)	O3—C7—O4	123.9 (4)
O2ⁱ—Cd1—O2W	171.30 (12)	O3—C7—C2	118.3 (4)
O3W—Cd1—O2W	81.44 (12)	O4—C7—C2	117.6 (4)
O4—Cd1—O2W	80.96 (12)	C5—N1—C1	119.4 (4)
N1ⁱ—Cd1—O2W	98.06 (13)	C5—N1—Cd1ⁱⁱ	126.5 (3)
C6—O2—Cd1ⁱⁱ	117.6 (3)	C1—N1—Cd1ⁱⁱ	114.0 (3)
C7—O4—Cd1	135.2 (3)	Cd1—O1W—H1	118 (4)
N1—C1—C2	121.3 (5)	Cd1—O1W—H2	128 (3)
N1—C1—C6	116.0 (4)	H1—O1W—H2	92 (5)
C2—C1—C6	122.6 (4)	Cd1—O2W—H3	110 (3)
C3—C2—C1	118.7 (4)	Cd1—O2W—H4	120 (4)
C3—C2—C7	118.6 (4)	H3—O2W—H4	110 (5)
C1—C2—C7	122.7 (4)	Cd1—O3W—H5	118 (4)
C4—C3—C2	120.2 (5)	Cd1—O3W—H6	130 (4)
C4—C3—H3A	119.9	H5—O3W—H6	101 (5)

O1W—Cd1—O4—C7	131.6 (5)	C2—C1—C6—O2	−177.9 (5)
O2ⁱ—Cd1—O4—C7	37.4 (5)	N1—C1—C6—O1	179.6 (6)
O3W—Cd1—O4—C7	−175.1 (4)	C2—C1—C6—O1	2.7 (9)
N1ⁱ—Cd1—O4—C7	−38.6 (5)	Cd1—O4—C7—O3	168.0 (3)
O2W—Cd1—O4—C7	−134.3 (5)	Cd1—O4—C7—C2	−7.0 (7)
N1—C1—C2—C3	0.9 (7)	C3—C2—C7—O3	−87.1 (6)
C6—C1—C2—C3	177.6 (5)	C1—C2—C7—O3	92.4 (6)
N1—C1—C2—C7	−178.5 (4)	C3—C2—C7—O4	88.2 (6)
C6—C1—C2—C7	−1.8 (8)	C1—C2—C7—O4	−92.3 (6)
C1—C2—C3—C4	0.6 (9)	C4—C5—N1—C1	0.2 (8)
C7—C2—C3—C4	−179.9 (5)	C4—C5—N1—Cd1ⁱⁱ	176.0 (4)
C2—C3—C4—C5	−1.7 (9)	C2—C1—N1—C5	−1.3 (7)
C3—C4—C5—N1	1.3 (9)	C6—C1—N1—C5	−178.3 (5)
Cd1ⁱⁱ—O2—C6—O1	175.2 (6)	C2—C1—N1—Cd1ⁱⁱ	−177.7 (4)
Cd1ⁱⁱ—O2—C6—C1	−4.1 (7)	C6—C1—N1—Cd1ⁱⁱ	5.4 (6)
N1—C1—C6—O2	−1.0 (8)

Symmetry codes: (i) −x+3/2, y, z−1/2; (ii) −x+3/2, y, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1···O2Wⁱⁱⁱ	0.85 (2)	1.99 (2)	2.782 (5)	156
O1W—H2···O3^iv	0.87 (2)	1.86 (2)	2.702 (5)	164
O2W—H3···O1^iv	0.88 (2)	1.85 (2)	2.731 (5)	178
O2W—H4···O3^v	0.87 (2)	1.84 (2)	2.687 (5)	165
O3W—H5···O4^iv	0.86 (2)	1.86 (2)	2.712 (4)	171
O3W—H6···O1^vi	0.87 (2)	1.89 (2)	2.735 (8)	164
C3—H3A···O1W^vii	0.95 (2)	2.49 (2)	3.420 (6)	165

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

Experimental details

Crystal data
Chemical formula	[Cd(C₇H₃NO₄)(H₂O)₃]
M_r	331.55
Crystal system, space group	Orthorhombic, Pca2₁
Temperature (K)	100
a, b, c (Å)	16.820 (3), 6.8076 (14), 8.6658 (17)
V (Å³)	992.3 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.22
Crystal size (mm)	0.40 × 0.08 × 0.05

Data collection
Diffractometer	Bruker APEX 1000 CCD area-detector diffractometer
Absorption correction	Multi-scan (APEX2; Bruker, 2005)
T_min, T_max	0.810, 0.901
No. of measured, independent and observed [I > 2σ(I)] reflections	8990, 2255, 1848
R_int	0.060
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.029, 0.056, 1.01
No. of reflections	2255
No. of parameters	151
No. of restraints	7
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.61, −0.84
Absolute structure	Flack (1983), 1042 Friedel pairs
Absolute structure parameter	0.05 (4)

Computer programs: APEX2 (Bruker, 2005), SHELXTL (Sheldrick, 1998).

Selected geometric parameters (Å, º) top

Cd1—O1W	2.254 (4)	Cd1—O4	2.279 (3)
Cd1—O2ⁱ	2.259 (3)	Cd1—N1ⁱ	2.302 (4)
Cd1—O3W	2.274 (3)	Cd1—O2W	2.385 (3)

O3W—Cd1—O4	156.89 (12)	O2ⁱ—Cd1—O2W	171.30 (12)
O1W—Cd1—N1ⁱ	163.70 (14)

N1—C1—C6—O2	−1.0 (8)	C3—C2—C7—O4	88.2 (6)
N1—C1—C6—O1	179.6 (6)	C1—C2—C7—O4	−92.3 (6)

Symmetry code: (i) −x+3/2, y, z−1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1···O2Wⁱⁱ	0.85 (2)	1.99 (2)	2.782 (5)	155.61
O1W—H2···O3ⁱⁱⁱ	0.87 (2)	1.86 (2)	2.702 (5)	163.55
O2W—H3···O1ⁱⁱⁱ	0.88 (2)	1.85 (2)	2.731 (5)	177.88
O2W—H4···O3^iv	0.87 (2)	1.84 (2)	2.687 (5)	164.45
O3W—H5···O4ⁱⁱⁱ	0.86 (2)	1.86 (2)	2.712 (4)	171.29
O3W—H6···O1^v	0.87 (2)	1.89 (2)	2.735 (8)	164.32
C3—H3A···O1W^vi	0.95 (2)	2.49 (2)	3.420 (6)	165

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

References

Aghabozorg, H., Daneshvar, S., Motyeian, E., Ghadermazi, M. & Attar Gharamaleki, J. (2007). Acta Cryst. E63, m2468–m2469. Web of Science CSD CrossRef IUCr Journals Google Scholar
Aghabozorg, H., Manteghi, F. & Ghadermazi, M. (2008). Acta Cryst. E64. Submitted for publication. CrossRef IUCr Journals Google Scholar
Aghabozorg, H., Sadr-khanlou, E., Soleimannejad, J. & Adams, H. (2007). Acta Cryst. E63, m1769. Web of Science CSD CrossRef IUCr Journals Google Scholar
Bruker (2005). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Li, L. J. & Li, Y. (2004). J. Mol. Struct. 694, 199–203. Web of Science CSD CrossRef CAS Google Scholar
Manteghi, F., Ghadermazi, M. & Aghabozorg, H. (2007). Acta Cryst. E63, o2809. Web of Science CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (1998). SHELXTL. Version. 5.10. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar

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Volume 64| Part 2| February 2008| Pages m320-m321

doi:10.1107/S160053680706850X

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