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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

Tris(2,2′-bi­pyridine-κ2N,N′)cadmium(II) bis­­(perchlorate) hemihydrate

aKey Laboratory for Soft Chemistry and Functional Materials of the Ministry of Education, Nanjing University of Science and Technology, Nanjing 210094, People's Republic of China
*Correspondence e-mail: zhangweiguang650@sohu.com

(Received 4 November 2008; accepted 7 November 2008; online 3 December 2008)

The asymmetric unit of the title compound, [Cd(C10H8N2)3](ClO4)2·0.5H2O, consists of one complex [Cd(bpy)3]2+ cation (bpy = 2,2′-bipyridine), two perchlorate anions and one water molecule with half-occupancy. The central cadmium(II) ion is bound to six N atoms from three bpy ligands in a distorted octa­hedral coordination, with Cd—N bond distances ranging from 2.304 (3) to 2.395 (2) Å.

Related literature

For applications of metal complexes of 2,2′-bipyridine and its derivatives, see: Kuang et al. (2006[Kuang, D., Klein, C., Snaith, H. J., Moser, J.-E., Humphry-Baker, R., Comte, P., Zakeeruddin, S. M. & Gratzel, M. (2006). Nano Lett. 6, 769-773.]). For cadmium complexes, see: Kundu et al. (2005[Kundu, N., Mandal, D., Chaudhury, M. & Tiekink, E. R. T. (2005). Appl. Organomet. Chem. 19, 1268-1270.]); Ranjbar et al. (2007[Ranjbar, Z. R., Morsali, A. & Zhu, L.-G. (2007). J. Coord. Chem. 6, 667-676.]); Shi et al. (2006[Shi, J.-M., Chen, J.-N. & Liu, L.-D. (2006). Acta Cryst. E62, m2094-m2095.]); Zheng et al. (2005[Zheng, S.-T., Zhang, J., Xu, J.-Q. & Yang, G.-Y. (2005). J. Solid State Chem. 178, 3740-3746.]).

[Scheme 1]

Experimental

Crystal data
  • [Cd(C10H8N2)3](ClO4)2·0.5H2O

  • Mr = 788.87

  • Triclinic, [P \overline 1]

  • a = 8.1704 (3) Å

  • b = 11.0282 (5) Å

  • c = 18.3875 (7) Å

  • α = 104.631 (1)°

  • β = 92.652 (1)°

  • γ = 100.520 (1)°

  • V = 1568.68 (11) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.93 mm−1

  • T = 173 (2) K

  • 0.20 × 0.16 × 0.12 mm

Data collection
  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.82, Tmax = 0.90

  • 19563 measured reflections

  • 6067 independent reflections

  • 5114 reflections with I > 2σ(I)

  • Rint = 0.037

Refinement
  • R[F2 > 2σ(F2)] = 0.034

  • wR(F2) = 0.107

  • S = 1.01

  • 6067 reflections

  • 434 parameters

  • H-atom parameters constrained

  • Δρmax = 0.44 e Å−3

  • Δρmin = −0.54 e Å−3

Table 1
Selected geometric parameters (Å, °)

Cd1—N4 2.304 (3)
Cd1—N2 2.312 (3)
Cd1—N6 2.330 (3)
Cd1—N3 2.329 (3)
Cd1—N5 2.383 (3)
Cd1—N1 2.395 (2)

Data collection: SMART (Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. 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


Comment top

Metal complexes of 2,2'-bipyridine and its derivatives have several applications, for example, in dye-sensitized solar cells (Kuang et al., 2006). Among these reported complexes, only a few structurally characterized examples are of cadmium ion (Kundu et al., 2005; Ranjbar et al., 2007; Shi et al., 2006; Zheng et al., 2005). For these cadmium complexes, the coordination scheme gives rise to monomeric species. Here we report a new monomeric cadmium(II) complex, viz. the title compound, [Cd(C10H8N2)3](ClO4)2.0.5H2O (I).

The structure of (I) consists of monomeric [Cd(bpy)3]2+ cations (bpy = 2,2'-bipyridine) and perchlorate anions and non-coordinating water molecules. The cadmium(II) ion is bound to six nitrogen atoms from three bpy ligands, giving a distorted CdN6 octahedral geometry. Of the six Cd—N bond distances ranging from 2.304 (3) to 2.395 (2) Å, the two cis bonds, Cd1—N1 and Cd1—N5, are longer than the other four bonds. The three 2,2'-bipyridine ligands are bent, with dihedral angles between the mean planes of two pyridine rings of the same bipyridine ligand ranging from 11.0 (2) to 27.6 (2)°.

Related literature top

For applications of metal complexes of 2,2'-bipyridine and its derivatives, see: Kuang et al., (2006). For cadmium complexes, see: Kundu et al. (2005); Ranjbar et al. (2007); Shi et al. (2006); Zheng et al. (2005).

Experimental top

The title complex was obtained as light red crystals by the hydrothermal reaction of Cd(ClO4)2.6H2O (0.10 mmol) and 2,2'-bipyridine (0.10 mmol) in water (7 ml) at 160°C for 48 hr.

Refinement top

H atoms bonded to O atoms of water molecules were located in a difference map and refined with O—H bonds = 0.85 Å, and with Uiso(H) = 1.2Ueq(O). Other H atoms were positioned geometrically and refined using a riding model, with C—H bonds = 0.95 Å and with Uiso (H) = 1.2Ueq (C).

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SMART (Bruker, 2000); data reduction: SAINT (Bruker, 2000); 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. View of the title compound. Displacement ellipsoids for non-H atoms are drawn at the 30% probability level.
Tris(2,2'-bipyridine-κ2N,N')cadmium(II) bis(perchlorate) hemihydrate top
Crystal data top
[Cd(C10H8N2)3](ClO4)2·0.5H2OZ = 2
Mr = 788.87F(000) = 794
Triclinic, P1Dx = 1.670 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.1704 (3) ÅCell parameters from 5350 reflections
b = 11.0282 (5) Åθ = 2.3–24.2°
c = 18.3875 (7) ŵ = 0.93 mm1
α = 104.631 (1)°T = 173 K
β = 92.652 (1)°Block, light red
γ = 100.520 (1)°0.20 × 0.16 × 0.12 mm
V = 1568.68 (11) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
6067 independent reflections
Radiation source: fine-focus sealed tube5114 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
ϕ and ω scansθmax = 26.0°, θmin = 1.2°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 910
Tmin = 0.82, Tmax = 0.90k = 1313
19563 measured reflectionsl = 2222
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)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0692P)2]
where P = (Fo2 + 2Fc2)/3
6067 reflections(Δ/σ)max = 0.001
434 parametersΔρmax = 0.44 e Å3
0 restraintsΔρmin = 0.54 e Å3
Crystal data top
[Cd(C10H8N2)3](ClO4)2·0.5H2Oγ = 100.520 (1)°
Mr = 788.87V = 1568.68 (11) Å3
Triclinic, P1Z = 2
a = 8.1704 (3) ÅMo Kα radiation
b = 11.0282 (5) ŵ = 0.93 mm1
c = 18.3875 (7) ÅT = 173 K
α = 104.631 (1)°0.20 × 0.16 × 0.12 mm
β = 92.652 (1)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
6067 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
5114 reflections with I > 2σ(I)
Tmin = 0.82, Tmax = 0.90Rint = 0.037
19563 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0340 restraints
wR(F2) = 0.107H-atom parameters constrained
S = 1.01Δρmax = 0.44 e Å3
6067 reflectionsΔρmin = 0.54 e Å3
434 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*/UeqOcc. (<1)
Cd10.49907 (3)0.73554 (2)0.243298 (12)0.03097 (10)
N10.6598 (3)0.6830 (2)0.33902 (14)0.0294 (6)
N20.6508 (3)0.5860 (2)0.18631 (14)0.0301 (6)
N30.3534 (3)0.7832 (3)0.14562 (14)0.0322 (6)
N40.6676 (3)0.8972 (3)0.20701 (14)0.0317 (6)
N50.2893 (3)0.5889 (3)0.28060 (15)0.0343 (6)
N60.3367 (3)0.8481 (3)0.32562 (14)0.0336 (6)
C10.7042 (3)0.5700 (3)0.31281 (16)0.0275 (6)
C20.7179 (4)0.4891 (3)0.35877 (18)0.0348 (7)
H20.74760.40860.33900.042*
C30.6876 (4)0.5275 (3)0.43375 (19)0.0402 (8)
H30.69490.47330.46610.048*
C40.6469 (4)0.6444 (4)0.46057 (19)0.0399 (8)
H40.62840.67350.51220.048*
C50.6330 (4)0.7198 (3)0.41210 (17)0.0336 (7)
H50.60340.80060.43100.040*
C60.7320 (4)0.5340 (3)0.23180 (17)0.0280 (6)
C70.8391 (4)0.4527 (3)0.20353 (19)0.0373 (8)
H70.89510.41540.23600.045*
C80.8633 (4)0.4266 (3)0.1278 (2)0.0411 (8)
H80.93690.37180.10770.049*
C90.7789 (4)0.4813 (3)0.08131 (19)0.0398 (8)
H90.79340.46510.02900.048*
C100.6737 (4)0.5596 (3)0.11315 (18)0.0352 (7)
H100.61460.59650.08150.042*
C110.4207 (4)0.8910 (3)0.12777 (17)0.0312 (7)
C120.3271 (5)0.9441 (4)0.0842 (2)0.0444 (9)
H120.37541.02100.07230.053*
C130.1647 (5)0.8857 (4)0.0582 (2)0.0491 (9)
H130.09980.92170.02820.059*
C140.0970 (4)0.7748 (4)0.07580 (19)0.0447 (9)
H140.01490.73200.05800.054*
C150.1953 (4)0.7269 (3)0.12003 (19)0.0414 (8)
H150.14850.65050.13290.050*
C160.5991 (4)0.9476 (3)0.15684 (17)0.0330 (7)
C170.6922 (5)1.0456 (4)0.1331 (2)0.0464 (9)
H170.64151.08390.09960.056*
C180.8591 (5)1.0872 (4)0.1585 (2)0.0555 (11)
H180.92491.15410.14230.067*
C190.9301 (4)1.0308 (4)0.2077 (2)0.0468 (9)
H191.04601.05560.22440.056*
C200.8297 (4)0.9392 (3)0.23142 (19)0.0409 (8)
H200.87690.90300.26710.049*
C210.2114 (4)0.6420 (3)0.34008 (17)0.0365 (8)
C220.1362 (4)0.5700 (4)0.3857 (2)0.0515 (11)
H220.08520.60960.42830.062*
C230.1353 (5)0.4418 (5)0.3693 (2)0.0656 (14)
H230.08320.39160.40010.079*
C240.2102 (5)0.3873 (4)0.3083 (3)0.0612 (13)
H240.20920.29810.29500.073*
C250.2881 (4)0.4648 (3)0.2658 (2)0.0450 (9)
H250.34320.42700.22410.054*
C260.2157 (4)0.7800 (3)0.35443 (17)0.0357 (8)
C270.0983 (4)0.8389 (5)0.3950 (2)0.0543 (11)
H270.01240.79010.41490.065*
C280.1078 (5)0.9681 (5)0.4058 (2)0.0625 (13)
H280.02981.00980.43390.075*
C290.2321 (6)1.0361 (4)0.3754 (2)0.0587 (12)
H290.23981.12510.38140.070*
C300.3449 (5)0.9735 (4)0.3362 (2)0.0434 (9)
H300.43171.02090.31590.052*
Cl10.30915 (10)0.28250 (8)0.06302 (4)0.03444 (19)
O10.2886 (4)0.4107 (3)0.07130 (16)0.0558 (7)
O20.4439 (3)0.2792 (3)0.11403 (16)0.0599 (8)
O30.3387 (6)0.2297 (4)0.01150 (18)0.1051 (14)
O40.1617 (4)0.2129 (3)0.0806 (2)0.0909 (13)
Cl20.75289 (11)0.16580 (8)0.41261 (5)0.0389 (2)
O50.7279 (3)0.0316 (2)0.40528 (15)0.0488 (6)
O60.6449 (3)0.2223 (3)0.46332 (17)0.0605 (8)
O70.9241 (3)0.2243 (3)0.44150 (15)0.0558 (7)
O80.7206 (4)0.1863 (2)0.34000 (15)0.0639 (8)
O90.4144 (9)0.1855 (6)0.2510 (3)0.0752 (19)0.50
H9A0.43230.21350.21250.090*0.50
H9B0.50800.18810.27410.090*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.03118 (15)0.03525 (17)0.03679 (15)0.01384 (10)0.01081 (10)0.02177 (11)
N10.0266 (13)0.0319 (15)0.0321 (13)0.0070 (11)0.0015 (10)0.0123 (11)
N20.0314 (14)0.0286 (14)0.0346 (14)0.0091 (11)0.0050 (11)0.0136 (11)
N30.0347 (14)0.0329 (15)0.0339 (14)0.0088 (12)0.0074 (11)0.0158 (12)
N40.0332 (14)0.0316 (15)0.0331 (14)0.0070 (11)0.0079 (11)0.0123 (12)
N50.0298 (14)0.0376 (17)0.0343 (14)0.0015 (12)0.0016 (11)0.0144 (12)
N60.0276 (13)0.0422 (17)0.0334 (14)0.0115 (12)0.0054 (11)0.0108 (12)
C10.0245 (15)0.0268 (16)0.0332 (15)0.0059 (12)0.0013 (12)0.0115 (13)
C20.0365 (17)0.0321 (18)0.0413 (18)0.0124 (14)0.0049 (14)0.0155 (15)
C30.044 (2)0.044 (2)0.0403 (18)0.0098 (16)0.0021 (15)0.0245 (16)
C40.0398 (19)0.052 (2)0.0304 (16)0.0107 (16)0.0043 (14)0.0142 (16)
C50.0330 (17)0.0354 (19)0.0342 (16)0.0093 (14)0.0040 (13)0.0104 (14)
C60.0260 (15)0.0258 (16)0.0349 (16)0.0062 (12)0.0033 (12)0.0120 (13)
C70.0389 (18)0.0336 (18)0.0431 (18)0.0155 (15)0.0008 (14)0.0117 (15)
C80.0415 (19)0.0353 (19)0.048 (2)0.0167 (15)0.0110 (15)0.0067 (16)
C90.048 (2)0.038 (2)0.0345 (17)0.0082 (16)0.0124 (15)0.0109 (15)
C100.0399 (18)0.0368 (19)0.0338 (17)0.0095 (15)0.0081 (14)0.0163 (14)
C110.0402 (18)0.0288 (17)0.0295 (15)0.0120 (14)0.0088 (13)0.0123 (13)
C120.053 (2)0.042 (2)0.047 (2)0.0158 (17)0.0025 (17)0.0229 (17)
C130.055 (2)0.054 (2)0.049 (2)0.0261 (19)0.0013 (17)0.0233 (19)
C140.0367 (19)0.056 (2)0.0426 (19)0.0150 (17)0.0029 (15)0.0124 (17)
C150.0425 (19)0.039 (2)0.0441 (19)0.0038 (15)0.0016 (15)0.0179 (16)
C160.0432 (18)0.0288 (17)0.0329 (16)0.0102 (14)0.0127 (14)0.0153 (14)
C170.054 (2)0.044 (2)0.048 (2)0.0061 (17)0.0139 (17)0.0257 (17)
C180.059 (3)0.042 (2)0.065 (3)0.0041 (19)0.023 (2)0.020 (2)
C190.0372 (19)0.045 (2)0.053 (2)0.0009 (16)0.0099 (16)0.0086 (18)
C200.041 (2)0.038 (2)0.0427 (19)0.0066 (16)0.0029 (15)0.0106 (16)
C210.0248 (16)0.053 (2)0.0295 (16)0.0026 (14)0.0019 (12)0.0162 (15)
C220.0375 (19)0.074 (3)0.0388 (19)0.0165 (19)0.0037 (15)0.0289 (19)
C230.050 (2)0.088 (4)0.054 (3)0.028 (2)0.015 (2)0.044 (3)
C240.061 (3)0.047 (2)0.071 (3)0.018 (2)0.025 (2)0.035 (2)
C250.043 (2)0.039 (2)0.051 (2)0.0024 (16)0.0087 (16)0.0181 (17)
C260.0251 (16)0.056 (2)0.0271 (15)0.0074 (15)0.0023 (12)0.0129 (15)
C270.0343 (19)0.097 (4)0.0361 (19)0.026 (2)0.0081 (15)0.016 (2)
C280.053 (3)0.103 (4)0.041 (2)0.050 (3)0.0073 (18)0.011 (2)
C290.075 (3)0.057 (3)0.047 (2)0.041 (2)0.010 (2)0.003 (2)
C300.043 (2)0.040 (2)0.048 (2)0.0144 (16)0.0003 (16)0.0095 (17)
Cl10.0324 (4)0.0375 (5)0.0363 (4)0.0062 (3)0.0032 (3)0.0155 (3)
O10.0639 (18)0.0448 (16)0.0671 (18)0.0208 (14)0.0003 (14)0.0238 (14)
O20.0509 (16)0.0511 (17)0.080 (2)0.0109 (13)0.0190 (14)0.0257 (15)
O30.184 (4)0.103 (3)0.0511 (19)0.082 (3)0.038 (2)0.0193 (19)
O40.0405 (16)0.090 (3)0.167 (4)0.0002 (16)0.0150 (19)0.087 (3)
Cl20.0446 (5)0.0342 (5)0.0418 (4)0.0122 (4)0.0064 (4)0.0137 (4)
O50.0504 (15)0.0356 (14)0.0681 (17)0.0119 (11)0.0114 (13)0.0242 (13)
O60.0511 (16)0.0616 (18)0.0702 (19)0.0283 (14)0.0178 (14)0.0060 (15)
O70.0423 (14)0.0619 (18)0.0617 (17)0.0040 (13)0.0091 (12)0.0235 (14)
O80.109 (2)0.0407 (16)0.0478 (15)0.0232 (16)0.0063 (15)0.0195 (13)
O90.105 (5)0.075 (4)0.066 (4)0.045 (4)0.018 (3)0.036 (3)
Geometric parameters (Å, º) top
Cd1—N42.304 (3)C13—H130.9500
Cd1—N22.312 (3)C14—C151.377 (5)
Cd1—N62.330 (3)C14—H140.9500
Cd1—N32.329 (3)C15—H150.9500
Cd1—N52.383 (3)C16—C171.380 (5)
Cd1—N12.395 (2)C17—C181.375 (5)
N1—C11.340 (4)C17—H170.9500
N1—C51.343 (4)C18—C191.382 (6)
N2—C101.332 (4)C18—H180.9500
N2—C61.341 (4)C19—C201.356 (5)
N3—C151.334 (4)C19—H190.9500
N3—C111.341 (4)C20—H200.9500
N4—C201.337 (4)C21—C221.384 (5)
N4—C161.341 (4)C21—C261.471 (5)
N5—C251.325 (4)C22—C231.368 (6)
N5—C211.349 (4)C22—H220.9500
N6—C301.336 (4)C23—C241.362 (7)
N6—C261.342 (4)C23—H230.9500
C1—C21.390 (4)C24—C251.389 (5)
C1—C61.481 (4)C24—H240.9500
C2—C31.384 (5)C25—H250.9500
C2—H20.9500C26—C271.395 (5)
C3—C41.367 (5)C27—C281.375 (6)
C3—H30.9500C27—H270.9500
C4—C51.378 (5)C28—C291.376 (6)
C4—H40.9500C28—H280.9500
C5—H50.9500C29—C301.374 (5)
C6—C71.391 (4)C29—H290.9500
C7—C81.380 (5)C30—H300.9500
C7—H70.9500Cl1—O31.398 (3)
C8—C91.389 (5)Cl1—O41.404 (3)
C8—H80.9500Cl1—O21.425 (2)
C9—C101.374 (5)Cl1—O11.425 (3)
C9—H90.9500Cl2—O61.422 (3)
C10—H100.9500Cl2—O51.427 (3)
C11—C121.384 (4)Cl2—O81.430 (3)
C11—C161.492 (4)Cl2—O71.444 (3)
C12—C131.370 (5)O9—H9A0.8500
C12—H120.9500O9—H9B0.8500
C13—C141.370 (5)
N4—Cd1—N292.41 (9)C11—C12—H12120.0
N4—Cd1—N6101.98 (10)C12—C13—C14119.3 (3)
N2—Cd1—N6162.88 (10)C12—C13—H13120.4
N4—Cd1—N371.23 (9)C14—C13—H13120.4
N2—Cd1—N3106.18 (9)C13—C14—C15118.3 (3)
N6—Cd1—N387.41 (9)C13—C14—H14120.8
N4—Cd1—N5170.37 (9)C15—C14—H14120.8
N2—Cd1—N596.17 (10)N3—C15—C14122.8 (3)
N6—Cd1—N570.34 (10)N3—C15—H15118.6
N3—Cd1—N5102.03 (9)C14—C15—H15118.6
N4—Cd1—N1107.32 (9)N4—C16—C17120.7 (3)
N2—Cd1—N170.96 (9)N4—C16—C11116.7 (3)
N6—Cd1—N195.64 (9)C17—C16—C11122.6 (3)
N3—Cd1—N1176.86 (8)C18—C17—C16119.4 (4)
N5—Cd1—N179.74 (9)C18—C17—H17120.3
C1—N1—C5118.7 (3)C16—C17—H17120.3
C1—N1—Cd1111.40 (18)C17—C18—C19119.4 (4)
C5—N1—Cd1121.4 (2)C17—C18—H18120.3
C10—N2—C6119.4 (3)C19—C18—H18120.3
C10—N2—Cd1123.3 (2)C20—C19—C18118.1 (3)
C6—N2—Cd1116.9 (2)C20—C19—H19120.9
C15—N3—C11119.1 (3)C18—C19—H19120.9
C15—N3—Cd1123.0 (2)N4—C20—C19123.1 (3)
C11—N3—Cd1116.1 (2)N4—C20—H20118.4
C20—N4—C16119.1 (3)C19—C20—H20118.4
C20—N4—Cd1123.3 (2)N5—C21—C22121.2 (4)
C16—N4—Cd1117.5 (2)N5—C21—C26116.2 (3)
C25—N5—C21118.0 (3)C22—C21—C26122.5 (3)
C25—N5—Cd1122.9 (2)C23—C22—C21120.0 (4)
C21—N5—Cd1114.7 (2)C23—C22—H22120.0
C30—N6—C26119.6 (3)C21—C22—H22120.0
C30—N6—Cd1122.2 (2)C24—C23—C22118.9 (4)
C26—N6—Cd1117.6 (2)C24—C23—H23120.5
N1—C1—C2121.6 (3)C22—C23—H23120.5
N1—C1—C6116.5 (3)C23—C24—C25118.6 (4)
C2—C1—C6121.8 (3)C23—C24—H24120.7
C3—C2—C1119.0 (3)C25—C24—H24120.7
C3—C2—H2120.5N5—C25—C24123.2 (4)
C1—C2—H2120.5N5—C25—H25118.4
C4—C3—C2119.0 (3)C24—C25—H25118.4
C4—C3—H3120.5N6—C26—C27120.6 (4)
C2—C3—H3120.5N6—C26—C21117.1 (3)
C3—C4—C5119.4 (3)C27—C26—C21122.2 (3)
C3—C4—H4120.3C28—C27—C26119.5 (4)
C5—C4—H4120.3C28—C27—H27120.2
N1—C5—C4122.2 (3)C26—C27—H27120.2
N1—C5—H5118.9C27—C28—C29119.0 (4)
C4—C5—H5118.9C27—C28—H28120.5
N2—C6—C7120.9 (3)C29—C28—H28120.5
N2—C6—C1116.6 (3)C30—C29—C28119.1 (4)
C7—C6—C1122.5 (3)C30—C29—H29120.4
C8—C7—C6119.4 (3)C28—C29—H29120.4
C8—C7—H7120.3N6—C30—C29122.2 (4)
C6—C7—H7120.3N6—C30—H30118.9
C7—C8—C9119.2 (3)C29—C30—H30118.9
C7—C8—H8120.4O3—Cl1—O4110.3 (3)
C9—C8—H8120.4O3—Cl1—O2110.4 (2)
C10—C9—C8118.1 (3)O4—Cl1—O2108.31 (19)
C10—C9—H9120.9O3—Cl1—O1109.2 (2)
C8—C9—H9120.9O4—Cl1—O1108.11 (19)
N2—C10—C9123.0 (3)O2—Cl1—O1110.55 (16)
N2—C10—H10118.5O6—Cl2—O5110.51 (17)
C9—C10—H10118.5O6—Cl2—O8109.87 (19)
N3—C11—C12120.6 (3)O5—Cl2—O8109.15 (16)
N3—C11—C16116.4 (3)O6—Cl2—O7108.97 (17)
C12—C11—C16123.0 (3)O5—Cl2—O7109.12 (16)
C13—C12—C11120.0 (3)O8—Cl2—O7109.20 (17)
C13—C12—H12120.0H9A—O9—H9B108.6

Experimental details

Crystal data
Chemical formula[Cd(C10H8N2)3](ClO4)2·0.5H2O
Mr788.87
Crystal system, space groupTriclinic, P1
Temperature (K)173
a, b, c (Å)8.1704 (3), 11.0282 (5), 18.3875 (7)
α, β, γ (°)104.631 (1), 92.652 (1), 100.520 (1)
V3)1568.68 (11)
Z2
Radiation typeMo Kα
µ (mm1)0.93
Crystal size (mm)0.20 × 0.16 × 0.12
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2000)
Tmin, Tmax0.82, 0.90
No. of measured, independent and
observed [I > 2σ(I)] reflections
19563, 6067, 5114
Rint0.037
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.107, 1.01
No. of reflections6067
No. of parameters434
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.44, 0.54

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top
Cd1—N42.304 (3)Cd1—N32.329 (3)
Cd1—N22.312 (3)Cd1—N52.383 (3)
Cd1—N62.330 (3)Cd1—N12.395 (2)
N4—Cd1—N292.41 (9)N6—Cd1—N570.34 (10)
N4—Cd1—N6101.98 (10)N3—Cd1—N5102.03 (9)
N2—Cd1—N6162.88 (10)N4—Cd1—N1107.32 (9)
N4—Cd1—N371.23 (9)N2—Cd1—N170.96 (9)
N2—Cd1—N3106.18 (9)N6—Cd1—N195.64 (9)
N6—Cd1—N387.41 (9)N3—Cd1—N1176.86 (8)
N4—Cd1—N5170.37 (9)N5—Cd1—N179.74 (9)
N2—Cd1—N596.17 (10)
 

Acknowledgements

This work was supported financially by the National Natural Science Foundation of China (grant No. 50572039) and the Natural Science Foundation of Jiangsu Province (BK2006199).

References

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First citationRanjbar, Z. R., Morsali, A. & Zhu, L.-G. (2007). J. Coord. Chem. 6, 667–676.  Web of Science CSD CrossRef
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals
First citationShi, J.-M., Chen, J.-N. & Liu, L.-D. (2006). Acta Cryst. E62, m2094–m2095.  Web of Science CSD CrossRef IUCr Journals
First citationZheng, S.-T., Zhang, J., Xu, J.-Q. & Yang, G.-Y. (2005). J. Solid State Chem. 178, 3740–3746.  Web of Science CSD CrossRef CAS

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