metal-organic compounds
catena-Poly[(trans-diaquacadmium)-bis{μ-5-[4-(1H-imidazol-1-yl)phenyl]tetrazol-1-ido}]
aCollege of Food Science and Technology, Guangdong Ocean University, Zhanjiang 524088, People's Republic of China, bSchool of Enviroment Science and Engineering, Donghua University, Shanghai 200051, People's Republic of China, and cCollege of Science, Guangdong Ocean University, Zhanjiang 524088, People's Republic of China
*Correspondence e-mail: songwd60@163.com
In the title compound, [Cd(C10H7N6)2(H2O)2], the CdII atom lies on an inversion centre and is coordinated by four N atoms from 5-[4-(1H-imidazol-1-yl)phenyl]tetrazol-1-ide ligands and two O atoms from the coordinated water molecules in an octahedral arrangement. The complex polymeric chains are interconnected via intermolecular water O—H⋯N hydrogen bonds into a three-dimensional network.
Related literature
For our previous work based on imidazole derivatives as ligands, see: Tong, Li et al. (2011); Li et al. (2010). For related structures, see: Huang et al. (2009); Cheng (2011).
Experimental
Crystal data
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Refinement
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Data collection: SMART (Bruker, 2007); cell SAINT (Bruker, 2007); data reduction: SAINT; 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.
Supporting information
10.1107/S1600536812014626/kp2399sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536812014626/kp2399Isup2.hkl
A mixture of cadmium nitrate (0.1 mmol, 0.020 g) and 1-tetrazole-4-imidazole-benzene (0.2 mmol, 0.043 g) in 12 mL of water and 3 mL of alcohol was sealed in an autoclave equipped with a Teflon liner (25 mL) and then heated at 413 K for 3 days. Crystals of the title compound were obtained by slow evaporation of the solvent at room temperature.
H atoms of the water molecule were located in a difference-Fourier map and refined as riding with an O—H distance restraint of 0.85 Å, with Uiso(H) = 1.5 Ueq. The imidazolyl and phenyl H atoms were located in a difference-Fourier but were refined as riding with C—H = 0.93 Å and Uiso(H) = 1.5Ueq(C).
Data collection: SMART (Bruker, 2007); cell
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).[Cd(C10H7N6)2(H2O)2] | Z = 1 |
Mr = 570.86 | F(000) = 286 |
Triclinic, P1 | Dx = 1.841 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.6070 (6) Å | Cell parameters from 1702 reflections |
b = 8.0621 (8) Å | θ = 2.5–25.9° |
c = 9.1509 (9) Å | µ = 1.11 mm−1 |
α = 102.762 (1)° | T = 298 K |
β = 97.495 (1)° | Block, colourless |
γ = 106.073 (2)° | 0.22 × 0.21 × 0.15 mm |
V = 514.84 (8) Å3 |
Bruker SMART 1000 CCD area-detector diffractometer | 1768 independent reflections |
Radiation source: fine-focus sealed tube | 1708 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.015 |
ϕ and ω scans | θmax = 25.0°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Bruker, 2007) | h = −5→9 |
Tmin = 0.792, Tmax = 0.851 | k = −9→8 |
2591 measured reflections | l = −10→8 |
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)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.065 | H-atom parameters constrained |
S = 1.14 | w = 1/[σ2(Fo2) + (0.0345P)2 + 0.1705P] where P = (Fo2 + 2Fc2)/3 |
1768 reflections | (Δ/σ)max < 0.001 |
160 parameters | Δρmax = 0.48 e Å−3 |
3 restraints | Δρmin = −0.62 e Å−3 |
[Cd(C10H7N6)2(H2O)2] | γ = 106.073 (2)° |
Mr = 570.86 | V = 514.84 (8) Å3 |
Triclinic, P1 | Z = 1 |
a = 7.6070 (6) Å | Mo Kα radiation |
b = 8.0621 (8) Å | µ = 1.11 mm−1 |
c = 9.1509 (9) Å | T = 298 K |
α = 102.762 (1)° | 0.22 × 0.21 × 0.15 mm |
β = 97.495 (1)° |
Bruker SMART 1000 CCD area-detector diffractometer | 1768 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2007) | 1708 reflections with I > 2σ(I) |
Tmin = 0.792, Tmax = 0.851 | Rint = 0.015 |
2591 measured reflections |
R[F2 > 2σ(F2)] = 0.027 | 3 restraints |
wR(F2) = 0.065 | H-atom parameters constrained |
S = 1.14 | Δρmax = 0.48 e Å−3 |
1768 reflections | Δρmin = −0.62 e Å−3 |
160 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Cd1 | 0.5000 | 0.5000 | 0.5000 | 0.02370 (13) | |
N1 | 0.2660 (3) | 0.6294 (3) | 0.4304 (3) | 0.0252 (6) | |
N2 | 0.3282 (3) | 0.8094 (3) | 0.4926 (3) | 0.0280 (6) | |
N3 | 0.2042 (3) | 0.8776 (3) | 0.4406 (3) | 0.0278 (6) | |
N4 | 0.0567 (3) | 0.7454 (3) | 0.3421 (3) | 0.0274 (6) | |
N5 | 0.3041 (3) | 0.1036 (3) | 0.0476 (3) | 0.0218 (5) | |
N6 | 0.4348 (3) | 0.3262 (3) | 0.2564 (3) | 0.0242 (5) | |
O1W | 0.6896 (3) | 0.7364 (3) | 0.4031 (3) | 0.0297 (5) | |
H2W | 0.7079 | 0.8454 | 0.4492 | 0.045* | |
H1W | 0.7919 | 0.7268 | 0.3806 | 0.045* | |
C1 | 0.0999 (4) | 0.5951 (4) | 0.3384 (3) | 0.0215 (6) | |
C2 | −0.0149 (4) | 0.4151 (4) | 0.2423 (3) | 0.0214 (6) | |
C3 | 0.0003 (4) | 0.2630 (4) | 0.2830 (4) | 0.0258 (7) | |
H3 | 0.0763 | 0.2756 | 0.3757 | 0.031* | |
C4 | −0.0950 (4) | 0.0934 (4) | 0.1889 (3) | 0.0259 (7) | |
H4 | −0.0818 | −0.0071 | 0.2173 | 0.031* | |
C5 | −0.2105 (4) | 0.0742 (4) | 0.0518 (3) | 0.0207 (6) | |
C6 | −0.2325 (4) | 0.2233 (4) | 0.0103 (4) | 0.0284 (7) | |
H6 | −0.3123 | 0.2100 | −0.0806 | 0.034* | |
C7 | −0.1346 (4) | 0.3928 (4) | 0.1053 (4) | 0.0284 (7) | |
H7 | −0.1489 | 0.4931 | 0.0773 | 0.034* | |
C8 | 0.3743 (4) | 0.1495 (4) | 0.2001 (3) | 0.0241 (6) | |
H8 | 0.3793 | 0.0683 | 0.2573 | 0.029* | |
C9 | 0.4018 (4) | 0.3952 (4) | 0.1350 (4) | 0.0272 (7) | |
H9 | 0.4304 | 0.5167 | 0.1406 | 0.033* | |
C10 | 0.3218 (4) | 0.2606 (4) | 0.0065 (4) | 0.0272 (7) | |
H10 | 0.2857 | 0.2717 | −0.0910 | 0.033* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.02649 (19) | 0.02043 (18) | 0.02061 (19) | 0.00771 (13) | −0.00038 (12) | 0.00108 (12) |
N1 | 0.0254 (14) | 0.0177 (12) | 0.0279 (14) | 0.0069 (10) | −0.0013 (11) | 0.0009 (11) |
N2 | 0.0273 (14) | 0.0175 (12) | 0.0335 (15) | 0.0036 (11) | 0.0016 (11) | 0.0025 (11) |
N3 | 0.0287 (14) | 0.0188 (13) | 0.0337 (15) | 0.0072 (11) | 0.0035 (11) | 0.0043 (11) |
N4 | 0.0273 (14) | 0.0208 (13) | 0.0311 (15) | 0.0078 (11) | 0.0007 (11) | 0.0040 (11) |
N5 | 0.0237 (13) | 0.0185 (12) | 0.0198 (13) | 0.0049 (10) | 0.0007 (10) | 0.0026 (10) |
N6 | 0.0262 (13) | 0.0199 (12) | 0.0237 (14) | 0.0065 (10) | 0.0030 (10) | 0.0028 (10) |
O1W | 0.0283 (11) | 0.0214 (11) | 0.0388 (13) | 0.0080 (9) | 0.0079 (10) | 0.0061 (10) |
C1 | 0.0202 (14) | 0.0209 (14) | 0.0228 (16) | 0.0075 (12) | 0.0042 (12) | 0.0039 (12) |
C2 | 0.0183 (14) | 0.0210 (14) | 0.0234 (16) | 0.0061 (11) | 0.0045 (12) | 0.0028 (12) |
C3 | 0.0248 (16) | 0.0256 (16) | 0.0215 (16) | 0.0034 (12) | −0.0035 (12) | 0.0058 (13) |
C4 | 0.0295 (16) | 0.0213 (15) | 0.0241 (16) | 0.0037 (12) | 0.0004 (13) | 0.0084 (13) |
C5 | 0.0216 (15) | 0.0183 (14) | 0.0203 (15) | 0.0060 (11) | 0.0038 (12) | 0.0020 (12) |
C6 | 0.0288 (17) | 0.0259 (16) | 0.0246 (17) | 0.0085 (13) | −0.0067 (13) | 0.0024 (13) |
C7 | 0.0315 (17) | 0.0214 (15) | 0.0312 (18) | 0.0124 (13) | −0.0035 (13) | 0.0052 (13) |
C8 | 0.0288 (16) | 0.0217 (15) | 0.0206 (16) | 0.0072 (12) | 0.0010 (12) | 0.0066 (12) |
C9 | 0.0359 (17) | 0.0188 (15) | 0.0265 (17) | 0.0064 (13) | 0.0050 (13) | 0.0093 (13) |
C10 | 0.0383 (18) | 0.0202 (15) | 0.0213 (16) | 0.0067 (13) | 0.0001 (13) | 0.0087 (13) |
Cd1—N6 | 2.264 (2) | O1W—H1W | 0.8500 |
Cd1—N6i | 2.264 (2) | C1—C2 | 1.475 (4) |
Cd1—N1 | 2.385 (2) | C2—C3 | 1.387 (4) |
Cd1—N1i | 2.385 (2) | C2—C7 | 1.395 (4) |
Cd1—O1Wi | 2.461 (2) | C3—C4 | 1.380 (4) |
Cd1—O1W | 2.461 (2) | C3—H3 | 0.9300 |
N1—C1 | 1.345 (4) | C4—C5 | 1.387 (4) |
N1—N2 | 1.356 (3) | C4—H4 | 0.9300 |
N2—N3 | 1.306 (4) | C5—C6 | 1.383 (4) |
N3—N4 | 1.363 (3) | C5—N5ii | 1.442 (3) |
N4—C1 | 1.335 (4) | C6—C7 | 1.386 (4) |
N5—C8 | 1.356 (4) | C6—H6 | 0.9300 |
N5—C10 | 1.375 (4) | C7—H7 | 0.9300 |
N5—C5ii | 1.442 (3) | C8—H8 | 0.9300 |
N6—C8 | 1.326 (4) | C9—C10 | 1.347 (4) |
N6—C9 | 1.373 (4) | C9—H9 | 0.9300 |
O1W—H2W | 0.8500 | C10—H10 | 0.9300 |
N6—Cd1—N6i | 180.000 (1) | N4—C1—N1 | 111.2 (2) |
N6—Cd1—N1 | 89.45 (8) | N4—C1—C2 | 125.0 (2) |
N6i—Cd1—N1 | 90.55 (8) | N1—C1—C2 | 123.8 (2) |
N6—Cd1—N1i | 90.55 (8) | C3—C2—C7 | 118.3 (3) |
N6i—Cd1—N1i | 89.45 (8) | C3—C2—C1 | 120.5 (3) |
N1—Cd1—N1i | 180.000 (1) | C7—C2—C1 | 121.2 (3) |
N6—Cd1—O1Wi | 94.50 (8) | C4—C3—C2 | 121.4 (3) |
N6i—Cd1—O1Wi | 85.50 (8) | C4—C3—H3 | 119.3 |
N1—Cd1—O1Wi | 98.76 (8) | C2—C3—H3 | 119.3 |
N1i—Cd1—O1Wi | 81.24 (8) | C3—C4—C5 | 119.4 (3) |
N6—Cd1—O1W | 85.50 (8) | C3—C4—H4 | 120.3 |
N6i—Cd1—O1W | 94.50 (8) | C5—C4—H4 | 120.3 |
N1—Cd1—O1W | 81.24 (8) | C6—C5—C4 | 120.4 (3) |
N1i—Cd1—O1W | 98.76 (8) | C6—C5—N5ii | 120.9 (3) |
O1Wi—Cd1—O1W | 180.00 (7) | C4—C5—N5ii | 118.7 (2) |
C1—N1—N2 | 105.4 (2) | C5—C6—C7 | 119.5 (3) |
C1—N1—Cd1 | 143.60 (19) | C5—C6—H6 | 120.3 |
N2—N1—Cd1 | 110.51 (17) | C7—C6—H6 | 120.3 |
N3—N2—N1 | 108.8 (2) | C6—C7—C2 | 120.9 (3) |
N2—N3—N4 | 110.0 (2) | C6—C7—H7 | 119.5 |
C1—N4—N3 | 104.6 (2) | C2—C7—H7 | 119.5 |
C8—N5—C10 | 106.9 (2) | N6—C8—N5 | 110.7 (3) |
C8—N5—C5ii | 127.3 (2) | N6—C8—H8 | 124.7 |
C10—N5—C5ii | 125.5 (2) | N5—C8—H8 | 124.7 |
C8—N6—C9 | 106.0 (2) | C10—C9—N6 | 109.8 (3) |
C8—N6—Cd1 | 131.1 (2) | C10—C9—H9 | 125.1 |
C9—N6—Cd1 | 120.68 (19) | N6—C9—H9 | 125.1 |
Cd1—O1W—H2W | 118.8 | C9—C10—N5 | 106.6 (3) |
Cd1—O1W—H1W | 117.9 | C9—C10—H10 | 126.7 |
H2W—O1W—H1W | 108.2 | N5—C10—H10 | 126.7 |
N6—Cd1—N1—C1 | 32.7 (4) | Cd1—N1—C1—N4 | −170.3 (2) |
N6i—Cd1—N1—C1 | −147.3 (4) | N2—N1—C1—C2 | 177.5 (3) |
N1i—Cd1—N1—C1 | 139 (100) | Cd1—N1—C1—C2 | 7.6 (5) |
O1Wi—Cd1—N1—C1 | −61.8 (4) | N4—C1—C2—C3 | −156.3 (3) |
O1W—Cd1—N1—C1 | 118.2 (4) | N1—C1—C2—C3 | 26.0 (4) |
N6—Cd1—N1—N2 | −136.9 (2) | N4—C1—C2—C7 | 26.6 (5) |
N6i—Cd1—N1—N2 | 43.1 (2) | N1—C1—C2—C7 | −151.0 (3) |
N1i—Cd1—N1—N2 | −30 (100) | C7—C2—C3—C4 | 2.2 (5) |
O1Wi—Cd1—N1—N2 | 128.65 (19) | C1—C2—C3—C4 | −175.0 (3) |
O1W—Cd1—N1—N2 | −51.35 (19) | C2—C3—C4—C5 | −0.9 (5) |
C1—N1—N2—N3 | 0.4 (3) | C3—C4—C5—C6 | −0.9 (5) |
Cd1—N1—N2—N3 | 174.02 (19) | C3—C4—C5—N5ii | 177.9 (3) |
N1—N2—N3—N4 | −0.2 (3) | C4—C5—C6—C7 | 1.5 (5) |
N2—N3—N4—C1 | −0.1 (3) | N5ii—C5—C6—C7 | −177.3 (3) |
N6i—Cd1—N6—C8 | −60 (100) | C5—C6—C7—C2 | −0.3 (5) |
N1—Cd1—N6—C8 | −119.3 (3) | C3—C2—C7—C6 | −1.5 (5) |
N1i—Cd1—N6—C8 | 60.7 (3) | C1—C2—C7—C6 | 175.6 (3) |
O1Wi—Cd1—N6—C8 | −20.6 (3) | C9—N6—C8—N5 | 0.0 (3) |
O1W—Cd1—N6—C8 | 159.4 (3) | Cd1—N6—C8—N5 | 162.55 (19) |
N6i—Cd1—N6—C9 | 101 (100) | C10—N5—C8—N6 | 0.0 (3) |
N1—Cd1—N6—C9 | 41.1 (2) | C5ii—N5—C8—N6 | −174.1 (2) |
N1i—Cd1—N6—C9 | −138.9 (2) | C8—N6—C9—C10 | 0.0 (3) |
O1Wi—Cd1—N6—C9 | 139.9 (2) | Cd1—N6—C9—C10 | −164.8 (2) |
O1W—Cd1—N6—C9 | −40.1 (2) | N6—C9—C10—N5 | 0.0 (4) |
N3—N4—C1—N1 | 0.3 (3) | C8—N5—C10—C9 | 0.0 (3) |
N3—N4—C1—C2 | −177.6 (3) | C5ii—N5—C10—C9 | 174.3 (3) |
N2—N1—C1—N4 | −0.5 (3) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···N4iii | 0.85 | 2.06 | 2.903 (3) | 171 |
O1W—H2W···N3iv | 0.85 | 2.11 | 2.953 (3) | 171 |
Symmetry codes: (iii) x+1, y, z; (iv) −x+1, −y+2, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C10H7N6)2(H2O)2] |
Mr | 570.86 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 298 |
a, b, c (Å) | 7.6070 (6), 8.0621 (8), 9.1509 (9) |
α, β, γ (°) | 102.762 (1), 97.495 (1), 106.073 (2) |
V (Å3) | 514.84 (8) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.11 |
Crystal size (mm) | 0.22 × 0.21 × 0.15 |
Data collection | |
Diffractometer | Bruker SMART 1000 CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2007) |
Tmin, Tmax | 0.792, 0.851 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 2591, 1768, 1708 |
Rint | 0.015 |
(sin θ/λ)max (Å−1) | 0.594 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.027, 0.065, 1.14 |
No. of reflections | 1768 |
No. of parameters | 160 |
No. of restraints | 3 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.48, −0.62 |
Computer programs: SMART (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···N4i | 0.85 | 2.06 | 2.903 (3) | 171.2 |
O1W—H2W···N3ii | 0.85 | 2.11 | 2.953 (3) | 171.2 |
Symmetry codes: (i) x+1, y, z; (ii) −x+1, −y+2, −z+1. |
Acknowledgements
We acknowledge the Public Science and Technology Research Funds Projects of Ocean (grant No. 2000905021), the Guangdong Oceanic Fisheries Technology Promotion Project [grant No. A2009003–018(c)], the Guangdong Chinese Academy of Science Comprehensive Strategic Cooperation Project (grant No. 2009B091300121) and the Guangdong Province Key Project in the Field of Social Development [grant No. A2009011–007(c)].
References
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The ligands having more N atoms can be used to synthesize complexes of variety of cordination modes. Our research group has show great interest in the metal-organic complexes with imidazole and tetrazole derivatives, such as 2-propyl-imidazole-4,5-dicarboxylic acid (Tong, Li et al., 2011; Li et al., 2010) and 1-tetrazole-4-imidazolebenzene. In this paper, we report the synthesis and structure of a new CdII complex, [Cd(C8H9N2O4)4(H2O)2]n obtained under hydrothermal conditions. An asymmmetric unit of the title complex molecule includes one CdII, 1-tetrazole-4-imidazolebenzene ligand and a coordinated water molecule (Fig. 1). The CdII atom is octahedrally coordinated and lies on an inversion centre, connected with four ligands [two imidazole N and two tetrazole N, Cd—N =2.264 (2) and 2.385 (2) Å] and two coordinated water molecules [Cd—O=2.461 (2) Å] (Table 1). The polymer chains (Fig. 2) are interconnected via water O—H···O and O—H···N hydrogen bonds (Table 2). For related structures of complexes with this ligand, see Huang et al. (2009) and Cheng (2011).