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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 64| Part 5| May 2008| Pages m714-m715
doi:10.1107/S1600536808011331

Aqua­bis­(1H-imidazole-κN3)bis­­(4-methyl­benzoato-κ2O,O′)cadmium(II)

Wen-Dong Song,a* Li-Li Jia and Xiang-Hu Huangb

aCollege of Science, Guangdong Ocean University, Zhanjiang 524088, People's Republic of China, and bCollege of Fisheries, Guangdong Ocean University, ZhanJiang 524088, People's Republic of China
*Correspondence e-mail: songwd60@126.com

(Received 11 April 2008; accepted 21 April 2008; online 26 April 2008)

In the title compound, [Cd(C8H7O2)2(C3H4N2)2(H2O)], the CdII atom is coordinated by four carboxyl­ate O atoms from two bidentate chelating 4-methyl­benzoate ligands, two N atoms from two imidazole ligands and one water mol­ecule in a distorted penta­gonal bipyramidal geometry. Inter­molecular O—H⋯O hydrogen bonds between the coordinated water mol­ecule and the carboxyl­ate O atoms of 4-methyl­benzoate lead to an infinite chain. These chains are further self-assembled into a two-dimensional layer through N—H⋯O hydrogen bonds between the imidazole ligands and carboxyl­ate groups. One of the imidazole ligands is disordered over two positions with site-occupancy factors of 0.737 (4) and 0.263 (4).

Related literature

For related literature, see: Song et al. (2007[Song, W.-D., Gu, C.-S., Hao, X.-M. & Liu, J.-W. (2007). Acta Cryst. E63, m1023-m1024.]).

[Scheme 1]

Experimental

Crystal data

  • [Cd(C8H7O2)2(C3H4N2)2(H2O)]

  • Mr = 536.85

  • Triclinic, [P \overline 1]

  • a = 6.1355 (1) Å

  • b = 12.4338 (3) Å

  • c = 15.4771 (3) Å

  • α = 91.396 (1)°

  • β = 97.765 (1)°

  • γ = 98.304 (1)°

  • V = 1156.46 (4) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.98 mm−1

  • T = 296 (2) K

  • 0.26 × 0.23 × 0.20 mm
Data collection

  • Bruker SMART APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.784, Tmax = 0.828

  • 14653 measured reflections

  • 4764 independent reflections

  • 4515 reflections with I > 2σ(I)

  • Rint = 0.037
Refinement

  • R[F2 > 2σ(F2)] = 0.023

  • wR(F2) = 0.059

  • S = 1.08

  • 4764 reflections

  • 314 parameters

  • 37 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.27 e Å−3

  • Δρmin = −0.46 e Å−3

Table 1
Selected geometric parameters (Å, °)

Cd1—N3 2.257 (13)
Cd1—N1 2.2805 (15)
Cd1—O1W 2.3514 (13)
Cd1—O4 2.3842 (16)
Cd1—O1 2.4128 (14)
Cd1—O2 2.4788 (15)
Cd1—O3 2.5507 (16)
N3—Cd1—N1 174.2 (3)
N3—Cd1—O1W 85.9 (3)
N1—Cd1—O1W 88.49 (6)
N3—Cd1—O4 88.0 (5)
N1—Cd1—O4 92.50 (6)
O1W—Cd1—O4 81.32 (5)
N3—Cd1—O1 96.7 (5)
N1—Cd1—O1 86.88 (5)
O1W—Cd1—O1 141.36 (5)
O4—Cd1—O1 137.19 (5)
N3—Cd1—O2 88.6 (4)
N1—Cd1—O2 89.81 (5)
O1W—Cd1—O2 88.32 (5)
O4—Cd1—O2 169.31 (5)
O1—Cd1—O2 53.35 (5)
N3—Cd1—O3 89.8 (3)
N1—Cd1—O3 95.21 (5)
O1W—Cd1—O3 134.30 (5)
O4—Cd1—O3 53.05 (5)
O1—Cd1—O3 84.34 (5)
O2—Cd1—O3 137.09 (4)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O1W—H1W⋯O3i 0.82 (2) 2.104 (14) 2.881 (2) 157 (2)
O1W—H2W⋯O1i 0.82 (2) 1.943 (13) 2.723 (2) 160 (2)
N2—H2⋯O3ii 0.86 2.06 2.905 (3) 167
N4—H4A⋯O2iii 0.86 1.98 2.813 (8) 163
Symmetry codes: (i) x-1, y, z; (ii) -x+2, -y+1, -z+1; (iii) -x+1, -y+1, -z.

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2007[Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; 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: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808011331/hy2128sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808011331/hy2128Isup2.hkl

checkCIF report


Comment top

In the structural investigation of 4-methylbenzoate complexes, it has been found that the 4-methylbenzoate functions as bidentate and monodentate ligands (Song et al., 2007). In this paper, we report the crystal structure of the title compound, a new Cd complex obtained by the reaction of 4-methylbenzoic acid, imidazole and cadmium chloride in alkaline aqueous solution.

As illustrated in Fig. 1, the CdII atom exists in a distorted pentagonal bipyramidal geometry, defined by four carboxylate O atoms from two bidentate chelating 4-methylbenzoate ligands, two N atoms from two imidazole ligands and one water molecule (Table 1). One of the imidazole ligands is disordered over two positions with site occupancy factors of 0.737 (4) and 0.263 (4). Intermolecular O—H···O hydrogen bonds (Table 2) lead to infinite chains, involving the coordinated water molecules as donors and the O atoms of 4-methylbenzoate ligands as acceptors. These chains are further self-assembled into a two-dimensional supramolecular network through intermolecular N—H···O hydrogen bonds between the imidazole ligands and carboxylate groups (Fig. 2).

Related literature top

For related literature, see: Song et al. (2007).

Experimental top

A mixture of cadmium chloride (0.183 g, 1 mmol), 4-methylbenzoic acid (0.136 g, 1 mmol), imidazole (0.068 g, 1 mmol), NaOH (0.06 g, 1.5 mmol) and H2O (12 ml) was sealed in a 23 ml Teflon-lined reactor, which was heated at 433 K for 3 d and then cooled to room temperature at a rate of 10 K h-1. The crystals obtained were washed with water and dried in air.

Refinement top

H atoms attached to C and N atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93 (aromatic) and 0.96 (methyl) Å and N—H = 0.86 Å and with Uiso(H) = 1.2Ueq(C,N). H atoms of the water molecule were located in a difference Fourier map and refined with restraints of O—H = 0.82 (1) Å and H···H= 1.34 (2) Å and with Uiso(H) = 1.5Ueq(O). Site occupancy factors of the disordered imidazole ligand were refined.

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); 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: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound. Displacement ellipsoids are drawn as the 30% probability level. H atoms have been omitted for clarity.
[Figure 2] Fig. 2. A view of the two-dimensional layer in the title compound.
Aquabis(1H-imidazole-κN3)bis(4-methylbenzoato- κ2O,O')cadmium(II) top
Crystal data top
[Cd(C8H7O2)2(C3H4N2)2(H2O)]Z = 2
Mr = 536.85F(000) = 544
Triclinic, P1Dx = 1.542 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.1355 (1) ÅCell parameters from 3600 reflections
b = 12.4338 (3) Åθ = 1.4–28°
c = 15.4771 (3) ŵ = 0.98 mm−1
α = 91.396 (1)°T = 296 K
β = 97.765 (1)°Block, colorless
γ = 98.304 (1)°0.26 × 0.23 × 0.20 mm
V = 1156.46 (4) Å3
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		4764 independent reflections
Radiation source: fine-focus sealed tube4515 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
ϕ and ω scansθmax = 26.5°, θmin = 1.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −7→7
Tmin = 0.784, Tmax = 0.828k = −15→15
14653 measured reflectionsl = −18→19
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.023H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.059 w = 1/[σ2(Fo2) + (0.0265P)2 + 0.2332P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.010
4764 reflectionsΔρmax = 0.27 e Å−3
314 parametersΔρmin = −0.46 e Å−3
37 restraintsExtinction correction: SHELXTL (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0610 (16)
Crystal data top
[Cd(C8H7O2)2(C3H4N2)2(H2O)]γ = 98.304 (1)°
Mr = 536.85V = 1156.46 (4) Å3
Triclinic, P1Z = 2
a = 6.1355 (1) ÅMo Kα radiation
b = 12.4338 (3) ŵ = 0.98 mm−1
c = 15.4771 (3) ÅT = 296 K
α = 91.396 (1)°0.26 × 0.23 × 0.20 mm
β = 97.765 (1)°
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		4764 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		4515 reflections with I > 2σ(I)
Tmin = 0.784, Tmax = 0.828Rint = 0.037
14653 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02337 restraints
wR(F2) = 0.059H atoms treated by a mixture of independent and constrained refinement
S = 1.08Δρmax = 0.27 e Å−3
4764 reflectionsΔρmin = −0.46 e Å−3
314 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C10.9109 (3)0.68747 (15)0.20150 (12)0.0325 (4)
C21.0359 (3)0.79413 (16)0.18052 (12)0.0360 (4)
C31.2641 (4)0.81996 (19)0.20736 (15)0.0462 (5)
H31.34050.77050.23830.055*
C41.3774 (5)0.9190 (2)0.18814 (17)0.0616 (7)
H41.52960.93540.20650.074*
C51.2686 (6)0.9941 (2)0.14216 (18)0.0694 (9)
C61.0429 (6)0.9680 (2)0.11549 (17)0.0636 (7)
H60.96711.01770.08440.076*
C70.9270 (4)0.86914 (19)0.13418 (15)0.0483 (5)
H70.77490.85310.11540.058*
C81.3923 (9)1.1036 (3)0.1231 (3)0.1242 (18)
H8A1.46161.09640.07170.186*
H8B1.50411.12890.17170.186*
H8C1.28951.15490.11390.186*
C90.7907 (3)0.29695 (15)0.32072 (12)0.0339 (4)
C100.8303 (3)0.18454 (15)0.34383 (12)0.0327 (4)
C111.0249 (3)0.14673 (16)0.33053 (14)0.0393 (4)
H111.13660.19250.30890.047*
C121.0542 (4)0.04120 (17)0.34930 (15)0.0422 (5)
H121.18430.01650.33840.051*
C130.8944 (4)−0.02866 (16)0.38390 (13)0.0388 (4)
C140.7012 (4)0.01078 (17)0.39875 (15)0.0460 (5)
H140.5927−0.03380.42320.055*
C150.6680 (4)0.11496 (17)0.37780 (15)0.0429 (5)
H150.53550.13890.38650.052*
C160.9287 (5)−0.14287 (18)0.40544 (17)0.0559 (6)
H16A1.0697−0.15600.39050.084*
H16B0.8119−0.19350.37280.084*
H16C0.9265−0.15190.46670.084*
C200.4871 (4)0.61585 (18)0.41076 (14)0.0424 (5)
H200.35090.62070.37770.051*
C210.5421 (4)0.64415 (19)0.49653 (15)0.0517 (6)
H210.45210.67090.53320.062*
C220.8214 (4)0.58717 (17)0.44726 (13)0.0396 (4)
H220.96190.56840.44510.047*
Cd10.68370 (2)0.491827 (10)0.250662 (8)0.02905 (7)
N10.6629 (3)0.57885 (13)0.38005 (10)0.0330 (3)
N20.7550 (4)0.62584 (15)0.51870 (12)0.0487 (5)
H20.83260.63720.56950.058*
O11.0144 (2)0.62012 (12)0.24245 (10)0.0424 (3)
O20.7032 (2)0.66821 (12)0.17868 (10)0.0408 (3)
O30.9568 (3)0.36908 (11)0.31565 (10)0.0420 (3)
O40.5945 (3)0.31678 (12)0.30732 (11)0.0468 (4)
O1W0.2938 (2)0.47353 (12)0.22005 (10)0.0395 (3)
H1W0.221 (4)0.4298 (14)0.2482 (15)0.059*
H2W0.228 (4)0.5262 (13)0.2184 (17)0.059*
C170.8273 (6)0.3438 (4)0.0917 (2)0.0580 (10)0.737 (4)
H170.95760.33150.12570.070*0.737 (4)
C180.7560 (6)0.3045 (4)0.0092 (2)0.0633 (11)0.737 (4)
H180.83120.2643−0.02510.076*0.737 (4)
C190.508 (3)0.3921 (12)0.0535 (6)0.0420 (16)0.737 (4)
H190.37280.41790.05380.050*0.737 (4)
N30.668 (2)0.4081 (12)0.1184 (10)0.0411 (13)0.737 (4)
N40.5551 (7)0.3347 (5)−0.0138 (5)0.0450 (11)0.737 (4)
H4A0.47190.3196−0.06320.054*0.737 (4)
C17'0.8520 (17)0.4185 (11)0.0683 (6)0.0580 (10)0.263 (4)
H17'0.99190.45710.08830.070*0.263 (4)
C18'0.7834 (18)0.3789 (12)−0.0139 (6)0.0633 (11)0.263 (4)
H18'0.87120.3675−0.05680.076*0.263 (4)
C19'0.512 (7)0.379 (4)0.0592 (19)0.0420 (16)0.263 (4)
H19'0.36900.38110.07210.050*0.263 (4)
N3'0.690 (7)0.394 (4)0.117 (3)0.0411 (13)0.263 (4)
N4'0.561 (2)0.3591 (18)−0.0207 (18)0.0450 (11)0.263 (4)
H4'0.46830.3381−0.06700.054*0.263 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0379 (10)0.0348 (10)0.0259 (9)0.0070 (8)0.0076 (8)−0.0024 (7)
C20.0439 (11)0.0367 (10)0.0281 (9)0.0036 (8)0.0108 (8)−0.0024 (8)
C30.0432 (11)0.0526 (13)0.0419 (12)0.0010 (10)0.0103 (9)−0.0041 (10)
C40.0575 (15)0.0704 (17)0.0511 (14)−0.0175 (13)0.0183 (12)−0.0110 (13)
C50.097 (2)0.0552 (15)0.0481 (15)−0.0246 (15)0.0208 (15)−0.0025 (12)
C60.095 (2)0.0448 (13)0.0475 (14)0.0013 (14)0.0059 (14)0.0121 (11)
C70.0587 (14)0.0435 (12)0.0412 (12)0.0043 (10)0.0039 (10)0.0052 (10)
C80.179 (5)0.079 (2)0.092 (3)−0.065 (3)0.025 (3)0.011 (2)
C90.0439 (11)0.0332 (10)0.0256 (9)0.0082 (8)0.0060 (8)0.0000 (7)
C100.0386 (10)0.0293 (9)0.0291 (9)0.0033 (7)0.0032 (8)−0.0003 (7)
C110.0404 (11)0.0339 (10)0.0454 (12)0.0041 (8)0.0138 (9)0.0038 (8)
C120.0431 (11)0.0362 (11)0.0506 (13)0.0127 (9)0.0113 (10)0.0007 (9)
C130.0500 (12)0.0281 (9)0.0363 (10)0.0036 (8)0.0023 (9)−0.0014 (8)
C140.0474 (12)0.0357 (11)0.0548 (13)−0.0016 (9)0.0135 (10)0.0081 (9)
C150.0363 (10)0.0381 (11)0.0554 (13)0.0048 (8)0.0108 (9)0.0032 (9)
C160.0824 (18)0.0313 (11)0.0546 (14)0.0106 (11)0.0091 (13)0.0045 (10)
C200.0400 (11)0.0468 (12)0.0405 (11)0.0038 (9)0.0100 (9)−0.0049 (9)
C210.0681 (16)0.0471 (12)0.0410 (12)−0.0028 (11)0.0259 (12)−0.0112 (10)
C220.0473 (11)0.0346 (10)0.0341 (11)0.0025 (8)−0.0010 (9)0.0037 (8)
Cd10.03054 (9)0.03191 (10)0.02451 (9)0.00588 (5)0.00252 (5)−0.00215 (5)
N10.0391 (8)0.0324 (8)0.0271 (8)0.0045 (6)0.0050 (7)−0.0009 (6)
N20.0710 (14)0.0416 (10)0.0264 (9)−0.0088 (9)0.0009 (8)−0.0006 (7)
O10.0410 (8)0.0393 (8)0.0496 (9)0.0120 (6)0.0089 (7)0.0074 (6)
O20.0381 (8)0.0463 (8)0.0358 (8)0.0026 (6)0.0008 (6)0.0045 (6)
O30.0522 (9)0.0313 (7)0.0417 (8)0.0018 (6)0.0085 (7)0.0054 (6)
O40.0481 (9)0.0409 (8)0.0545 (10)0.0159 (7)0.0080 (7)0.0059 (7)
O1W0.0303 (7)0.0441 (8)0.0447 (8)0.0086 (6)0.0041 (6)0.0038 (7)
C170.0427 (15)0.089 (3)0.0413 (17)0.0138 (19)0.0016 (13)−0.0240 (18)
C180.0542 (18)0.092 (3)0.0433 (18)0.013 (2)0.0090 (14)−0.0268 (19)
C190.0507 (14)0.040 (4)0.0335 (17)0.008 (2)−0.0013 (14)0.001 (2)
N30.040 (3)0.053 (4)0.0312 (11)0.0127 (18)0.0034 (19)−0.013 (2)
N40.0624 (13)0.041 (3)0.0262 (17)−0.0024 (13)−0.0035 (9)−0.002 (2)
C17'0.0427 (15)0.089 (3)0.0413 (17)0.0138 (19)0.0016 (13)−0.0240 (18)
C18'0.0542 (18)0.092 (3)0.0433 (18)0.013 (2)0.0090 (14)−0.0268 (19)
C19'0.0507 (14)0.040 (4)0.0335 (17)0.008 (2)−0.0013 (14)0.001 (2)
N3'0.040 (3)0.053 (4)0.0312 (11)0.0127 (18)0.0034 (19)−0.013 (2)
N4'0.0624 (13)0.041 (3)0.0262 (17)−0.0024 (13)−0.0035 (9)−0.002 (2)
Geometric parameters (Å, º) top
C1—O11.256 (2)C20—N11.369 (3)
C1—O21.262 (3)C20—H200.9300
C1—C21.499 (3)C21—N21.358 (3)
C2—C71.383 (3)C21—H210.9300
C2—C31.393 (3)C22—N11.315 (3)
C3—C41.384 (3)C22—N21.331 (3)
C3—H30.9300C22—H220.9300
C4—C51.381 (5)Cd1—N32.257 (13)
C4—H40.9300Cd1—N12.2805 (15)
C5—C61.379 (5)Cd1—O1W2.3514 (13)
C5—C81.516 (4)Cd1—O42.3842 (16)
C6—C71.386 (3)Cd1—O12.4128 (14)
C6—H60.9300Cd1—O22.4788 (15)
C7—H70.9300Cd1—O32.5507 (16)
C8—H8A0.9600N2—H20.8600
C8—H8B0.9600O1W—H1W0.82 (2)
C8—H8C0.9600O1W—H2W0.82 (2)
C9—O41.254 (3)C17—C181.347 (4)
C9—O31.269 (2)C17—N31.444 (10)
C9—C101.496 (3)C17—H170.9300
C10—C111.383 (3)C18—N41.345 (5)
C10—C151.390 (3)C18—H180.9300
C11—C121.382 (3)C19—N31.298 (4)
C11—H110.9300C19—N41.337 (6)
C12—C131.386 (3)C19—H190.9300
C12—H120.9300N4—H4A0.8600
C13—C141.391 (3)C17'—N3'1.33 (5)
C13—C161.504 (3)C17'—C18'1.343 (8)
C14—C151.380 (3)C17'—H17'0.9300
C14—H140.9300C18'—N4'1.343 (9)
C15—H150.9300C18'—H18'0.9300
C16—H16A0.9600C19'—N3'1.300 (9)
C16—H16B0.9600C19'—N4'1.337 (10)
C16—H16C0.9600C19'—H19'0.9300
C20—C211.350 (3)N4'—H4'0.8600
O1—C1—O2121.53 (18)N3—Cd1—O196.7 (5)
O1—C1—C2119.37 (18)N1—Cd1—O186.88 (5)
O2—C1—C2119.09 (18)O1W—Cd1—O1141.36 (5)
C7—C2—C3118.6 (2)O4—Cd1—O1137.19 (5)
C7—C2—C1120.66 (19)N3—Cd1—O288.6 (4)
C3—C2—C1120.8 (2)N1—Cd1—O289.81 (5)
C4—C3—C2120.2 (2)O1W—Cd1—O288.32 (5)
C4—C3—H3119.9O4—Cd1—O2169.31 (5)
C2—C3—H3119.9O1—Cd1—O253.35 (5)
C5—C4—C3121.2 (3)N3—Cd1—O389.8 (3)
C5—C4—H4119.4N1—Cd1—O395.21 (5)
C3—C4—H4119.4O1W—Cd1—O3134.30 (5)
C6—C5—C4118.4 (2)O4—Cd1—O353.05 (5)
C6—C5—C8120.6 (4)O1—Cd1—O384.34 (5)
C4—C5—C8121.0 (3)O2—Cd1—O3137.09 (4)
C5—C6—C7121.1 (3)C22—N1—C20105.43 (17)
C5—C6—H6119.4C22—N1—Cd1123.23 (14)
C7—C6—H6119.4C20—N1—Cd1130.55 (14)
C2—C7—C6120.5 (2)C22—N2—C21107.39 (19)
C2—C7—H7119.8C22—N2—H2126.3
C6—C7—H7119.8C21—N2—H2126.3
O4—C9—O3122.22 (19)C1—O1—Cd194.15 (12)
O4—C9—C10118.90 (18)C1—O2—Cd190.92 (12)
O3—C9—C10118.88 (18)C9—O3—Cd187.86 (12)
C11—C10—C15118.59 (18)C9—O4—Cd195.91 (13)
C11—C10—C9121.38 (17)Cd1—O1W—H1W117.5 (18)
C15—C10—C9120.02 (18)Cd1—O1W—H2W121.9 (18)
C10—C11—C12120.31 (18)H1W—O1W—H2W103.8 (15)
C10—C11—H11119.8C18—C17—N3108.7 (6)
C12—C11—H11119.8C18—C17—H17125.6
C11—C12—C13121.63 (19)N3—C17—H17125.6
C11—C12—H12119.2C17—C18—N4106.7 (5)
C13—C12—H12119.2C17—C18—H18126.6
C12—C13—C14117.65 (19)N4—C18—H18126.6
C12—C13—C16121.4 (2)N3—C19—N4113.3 (12)
C14—C13—C16121.0 (2)N3—C19—H19123.3
C15—C14—C13121.05 (19)N4—C19—H19123.3
C15—C14—H14119.5C19—N3—C17102.8 (11)
C13—C14—H14119.5C19—N3—Cd1130.1 (8)
C14—C15—C10120.7 (2)C17—N3—Cd1126.5 (8)
C14—C15—H15119.6C19—N4—C18108.0 (9)
C10—C15—H15119.6C19—N4—H4A126.0
C21—C20—N1109.4 (2)C18—N4—H4A126.0
C21—C20—H20125.3N3'—C17'—C18'110 (2)
N1—C20—H20125.3N3'—C17'—H17'125.1
C20—C21—N2106.33 (19)C18'—C17'—H17'125.1
C20—C21—H21126.8C17'—C18'—N4'105.1 (14)
N2—C21—H21126.8C17'—C18'—H18'127.5
N1—C22—N2111.4 (2)N4'—C18'—H18'127.5
N1—C22—H22124.3N3'—C19'—N4'111 (4)
N2—C22—H22124.3N3'—C19'—H19'124.3
N3—Cd1—N1174.2 (3)N4'—C19'—H19'124.3
N3—Cd1—O1W85.9 (3)C19'—N3'—C17'103 (4)
N1—Cd1—O1W88.49 (6)C19'—N4'—C18'106 (3)
N3—Cd1—O488.0 (5)C19'—N4'—H4'127.1
N1—Cd1—O492.50 (6)C18'—N4'—H4'127.1
O1W—Cd1—O481.32 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O3i0.82 (2)2.104 (14)2.881 (2)157 (2)
O1W—H2W···O1i0.82 (2)1.943 (13)2.723 (2)160 (2)
N2—H2···O3ii0.862.062.905 (3)167
N4—H4A···O2iii0.861.982.813 (8)163
Symmetry codes: (i) x−1, y, z; (ii) −x+2, −y+1, −z+1; (iii) −x+1, −y+1, −z.

Experimental details

Crystal data
Chemical formula[Cd(C8H7O2)2(C3H4N2)2(H2O)]
Mr536.85
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)6.1355 (1), 12.4338 (3), 15.4771 (3)
α, β, γ (°)91.396 (1), 97.765 (1), 98.304 (1)
V (Å3)1156.46 (4)
Z2
Radiation typeMo Kα
µ (mm−1)0.98
Crystal size (mm)0.26 × 0.23 × 0.20
Data collection
DiffractometerBruker SMART APEXII CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.784, 0.828
No. of measured, independent and
observed [I > 2σ(I)] reflections		14653, 4764, 4515
Rint0.037
(sin θ/λ)max (Å−1)0.628
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.023, 0.059, 1.08
No. of reflections4764
No. of parameters314
No. of restraints37
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)0.27, −0.46

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top
Cd1—N32.257 (13)Cd1—O12.4128 (14)
Cd1—N12.2805 (15)Cd1—O22.4788 (15)
Cd1—O1W2.3514 (13)Cd1—O32.5507 (16)
Cd1—O42.3842 (16)
N3—Cd1—N1174.2 (3)N1—Cd1—O289.81 (5)
N3—Cd1—O1W85.9 (3)O1W—Cd1—O288.32 (5)
N1—Cd1—O1W88.49 (6)O4—Cd1—O2169.31 (5)
N3—Cd1—O488.0 (5)O1—Cd1—O253.35 (5)
N1—Cd1—O492.50 (6)N3—Cd1—O389.8 (3)
O1W—Cd1—O481.32 (5)N1—Cd1—O395.21 (5)
N3—Cd1—O196.7 (5)O1W—Cd1—O3134.30 (5)
N1—Cd1—O186.88 (5)O4—Cd1—O353.05 (5)
O1W—Cd1—O1141.36 (5)O1—Cd1—O384.34 (5)
O4—Cd1—O1137.19 (5)O2—Cd1—O3137.09 (4)
N3—Cd1—O288.6 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O3i0.82 (2)2.104 (14)2.881 (2)157 (2)
O1W—H2W···O1i0.82 (2)1.943 (13)2.723 (2)160 (2)
N2—H2···O3ii0.862.062.905 (3)167
N4—H4A···O2iii0.861.982.813 (8)163
Symmetry codes: (i) x−1, y, z; (ii) −x+2, −y+1, −z+1; (iii) −x+1, −y+1, −z.
 

Acknowledgements

The authors acknowledge Guangdong Ocean University for supporting this work.

References

First citationBruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
 First citationSong, W.-D., Gu, C.-S., Hao, X.-M. & Liu, J.-W. (2007). Acta Cryst. E63, m1023–m1024.  Web of Science CSD CrossRef CAS IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

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ISSN: 2056-9890
Volume 64| Part 5| May 2008| Pages m714-m715
doi:10.1107/S1600536808011331
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