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Acta Cryst. (2007). E63, m2893    [ doi:10.1107/S1600536807053792 ]

Di-[mu]-nitrato-[kappa]3O,O':O'';[kappa]3O:O',O''-bis[bis(3-nitrobenzohydrazide-[kappa]2N',O)cadmium(II)] dinitrate

S. Y. Chundak, L. Y. Lukachinec and M. Daszkiewicz

Abstract top

The title compound, [Cd2(NO3)2(C7H7N3O3)2](NO3)2, contains centrosymmetric dimeric cations in which two nitrate anions each serve as a bidentate ligand to one Cd atom and a bridge to the other. The other anion in the asymmetric unit (half the formula unit) is uncoordinated. The ligands form an atypical seven-coordinated augmented trigonal prism around the CdII atom, with a displacement from the centre of the polyhedron in the direction of the uncoordinated nitrate anion. The crystal structure displays numerous N-H...O hydrogen bonds.

Comment top

In the dimeric structure of bis((µ2-nitrato-O,O',O'')-cis-bis(m-nitrobenzoylhydrazino-N,O)cadmium(II)) bis(nitrate), two cis coordinated organic ligands and two bridging nitrate anions form atypical seven coordinated arrangement around the Cd-atom. Because the dimer lies on the inversion centre the asymmetric unit contains only half of the dimer. Therefore, two cadmium(II) ions and their coordination spheres are symmetrically dependent. By the same reason two bridging nitrate anions are also symmetrically dependent. Although bridging coordination mode of nitrate anion is clearly seen, it is worth noticing that this anion donates three oxygen atoms to the cadmium(II) and monodentate and bidentate coordination can be specified. In the former mode, the Cd—Onitrate bond lenghts difference, Co—O—N angles difference and Co—N—Oterminal angle for one nitrate are 0.38 Å, 17.3° and 160.4° respectively and correlate well with the anisobidentate coordination mode (Kleywegt et al., 1985; Dowling et al., 1996). In the latter mode, respective parameters distinctly indicates monodentate coordination (0.93 Å, 45.9° and 139.3°).

Intriguingly, the Cd-atom is displaced from the centre of the coordination polyhedron (augmented trigonal prism) in the direction of one face (0.54 Å). However, it seems that this displacement is caused by free NO3− anion. In spite of the Cd···ONO2 distance (3.184 Å) which is too long for a bond, indeed it is worth considering as a weak interaction. The position of the free nitrate anion is stabillized by several hydrogen bonding interactions both NH and NH2 groups from organic ligand.

Related literature top

For geometric studies of the coordination mode of the nitrate anion, see: Kleywegt et al. (1985); Dowling et al. (1996).

Experimental top

1.8 g (1 mmol) of m-nitrobenzoylhydrazine was dissolved in 25 ml hot ethanol and mixed with 3 ml e thanolic solution of Cd(NO3)2 (3.1 g; 1 mmol). Colourless crystals were formed after 24 h, then filtered, washed with ethanol and dried on air.

Refinement top

All the hydrogen atoms were visible in the difference maps and were refined with isotropic displacement parameters correlated with the anisotropic displacement parameters of the atoms to which they were bonded [C—H 0.93 Å and Uiso(H) = 1.2Ueq(C)]. The positions of hydrogen atoms from hydrazine group were determined from the difference maps and were not refined [Uiso(H) = 1.5Ueq(N,O)].

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: publCIF (Version 1.9.0_c; Westrip, 2007).

Figures top
[Figure 1] Fig. 1. Dimeric structure of the title compound with elipsoids drawn at the 50% probability level. [Symmetry code: (i) −x, −y + 2, −z.].
Di-µ-nitrato-κ3O,O':O'';κ3O:O',O''-bis[bis(3-nitrobenzohydrazide- κ2N',O)cadmium(II)] dinitrate top
Crystal data top
[Cd2(NO3)2(C7H7N3O3)2](NO3)2F000 = 1192
Mr = 598.73Dx = 1.922 Mg m−3
Monoclinic, P21/cMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3275 reflections
a = 7.9218 (16) Åθ = 3.2–28.3º
b = 7.6237 (15) ŵ = 1.14 mm−1
c = 34.325 (7) ÅT = 293 (2) K
β = 93.67 (3)ºPlate, colourless
V = 2068.7 (7) Å30.38 × 0.35 × 0.10 mm
Z = 4
Data collection top
Kuma KM-4 with CCD area-detector
diffractometer		5111 independent reflections
Radiation source: fine-focus sealed tube3275 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.060
Detector resolution: 1024x1024 with blocks 2x2, 33.133pixel/mm pixels mm-1θmax = 28.3º
T = 293(2) Kθmin = 3.2º
ω scansh = −10→7
Absorption correction: numerical
(CrysAlis; Oxford Diffraction, 2006)		k = −10→10
Tmin = 0.672, Tmax = 0.871l = −45→45
26291 measured reflections
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)] = 0.041H-atom parameters constrained
wR(F2) = 0.064  w = 1/[σ2(Fo2) + (0.0233P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.94(Δ/σ)max = 0.001
5111 reflectionsΔρmax = 0.63 e Å−3
316 parametersΔρmin = −0.76 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Cd2(NO3)2(C7H7N3O3)2](NO3)2V = 2068.7 (7) Å3
Mr = 598.73Z = 4
Monoclinic, P21/cMo Kα
a = 7.9218 (16) ŵ = 1.14 mm−1
b = 7.6237 (15) ÅT = 293 (2) K
c = 34.325 (7) Å0.38 × 0.35 × 0.10 mm
β = 93.67 (3)º
Data collection top
Kuma KM-4 with CCD area-detector
diffractometer		5111 independent reflections
Absorption correction: numerical
(CrysAlis; Oxford Diffraction, 2006)		3275 reflections with I > 2σ(I)
Tmin = 0.672, Tmax = 0.871Rint = 0.060
26291 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.041316 parameters
wR(F2) = 0.064H-atom parameters constrained
S = 0.94Δρmax = 0.63 e Å−3
5111 reflectionsΔρmin = −0.76 e Å−3
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*/Ueq
Cd10.21123 (3)0.91697 (3)0.065750 (7)0.03871 (9)
C1A0.3993 (3)1.3516 (4)0.14429 (8)0.0283 (7)
C11A0.3681 (4)1.2144 (4)0.11357 (8)0.0299 (7)
O11A0.2649 (3)1.0959 (3)0.11856 (6)0.0420 (5)
N11A0.4532 (3)1.2260 (3)0.08142 (7)0.0325 (6)
H11A0.52541.31010.07740.049*
N12A0.4232 (3)1.0998 (3)0.05130 (7)0.0348 (6)
H21A0.38161.15280.02960.052*
H22A0.52211.04560.05030.052*
C2A0.4693 (3)1.5141 (4)0.13664 (9)0.0305 (7)
H2A0.50501.54020.11200.037*
C3A0.4847 (4)1.6360 (4)0.16640 (9)0.0320 (7)
N31A0.5536 (4)1.8102 (4)0.15805 (9)0.0488 (7)
O31A0.5797 (4)1.8452 (3)0.12432 (8)0.0784 (9)
O32A0.5794 (4)1.9129 (3)0.18495 (8)0.0781 (8)
C4A0.4352 (4)1.6029 (4)0.20352 (9)0.0406 (8)
H4A0.44741.68730.22310.049*
C5A0.3668 (4)1.4395 (4)0.21075 (9)0.0431 (8)
H5A0.33321.41330.23560.052*
C6A0.3481 (3)1.3157 (4)0.18157 (8)0.0351 (8)
H6A0.30091.20720.18680.042*
C1B−0.0259 (3)0.4933 (4)0.13333 (8)0.0280 (7)
C11B0.0584 (3)0.6052 (4)0.10467 (8)0.0292 (7)
O11B0.1456 (3)0.7319 (3)0.11554 (6)0.0422 (6)
N11B0.0386 (3)0.5559 (3)0.06711 (7)0.0345 (6)
H11B−0.04800.49300.05750.052*
N12B0.1088 (3)0.6642 (3)0.03862 (7)0.0342 (6)
H21B0.02770.69930.02070.051*
H22B0.15900.59650.02330.051*
C2B−0.0491 (3)0.5612 (4)0.16999 (9)0.0345 (7)
H2B−0.01520.67500.17640.041*
C3B−0.1232 (4)0.4572 (4)0.19677 (9)0.0383 (8)
N31B−0.1504 (4)0.5325 (5)0.23589 (9)0.0575 (9)
O31B−0.1058 (4)0.6833 (5)0.24205 (8)0.0936 (10)
O32B−0.2169 (4)0.4419 (4)0.25973 (8)0.0890 (10)
C4B−0.1743 (4)0.2890 (5)0.18912 (10)0.0467 (9)
H4B−0.22440.22220.20790.056*
C5B−0.1495 (4)0.2211 (4)0.15282 (10)0.0461 (9)
H5B−0.18310.10670.14690.055*
C6B−0.0751 (4)0.3213 (4)0.12507 (9)0.0365 (8)
H6B−0.05780.27350.10070.044*
N1A−0.1265 (3)1.0524 (3)0.03837 (8)0.0355 (6)
O1A0.0176 (3)1.1213 (3)0.03396 (6)0.0446 (6)
O2A−0.1387 (3)0.9443 (3)0.06509 (7)0.0578 (7)
O3A−0.2493 (3)1.0939 (3)0.01617 (6)0.0458 (6)
N1B0.6356 (3)0.5968 (4)0.03179 (7)0.0369 (6)
O1B0.6860 (3)0.4722 (3)0.05402 (6)0.0470 (6)
O2B0.7298 (3)0.6450 (3)0.00571 (6)0.0483 (6)
O3B0.4979 (3)0.6670 (3)0.03588 (7)0.0605 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.04042 (14)0.03565 (13)0.03968 (14)−0.01622 (13)−0.00052 (10)0.00128 (13)
C1A0.0280 (17)0.0297 (16)0.0271 (17)−0.0040 (13)0.0012 (13)0.0007 (14)
C11A0.0264 (17)0.0321 (17)0.0312 (17)−0.0060 (14)0.0024 (14)0.0046 (15)
O11A0.0475 (13)0.0426 (13)0.0373 (12)−0.0235 (12)0.0136 (10)−0.0040 (11)
N11A0.0346 (14)0.0320 (14)0.0317 (14)−0.0172 (12)0.0087 (12)−0.0054 (12)
N12A0.0315 (14)0.0403 (15)0.0331 (14)−0.0098 (12)0.0048 (11)−0.0078 (13)
C2A0.0310 (17)0.0341 (17)0.0268 (17)−0.0051 (14)0.0044 (13)−0.0005 (14)
C3A0.0350 (18)0.0246 (16)0.0360 (18)−0.0058 (13)0.0010 (15)0.0018 (14)
N31A0.064 (2)0.0316 (17)0.052 (2)−0.0115 (15)0.0120 (16)−0.0047 (16)
O31A0.136 (3)0.0435 (15)0.0596 (18)−0.0336 (16)0.0397 (18)−0.0036 (14)
O32A0.124 (2)0.0463 (15)0.0645 (17)−0.0368 (17)0.0137 (16)−0.0237 (15)
C4A0.047 (2)0.040 (2)0.0349 (18)−0.0032 (17)−0.0005 (15)−0.0081 (17)
C5A0.055 (2)0.047 (2)0.0272 (17)−0.0048 (18)0.0063 (15)−0.0014 (17)
C6A0.0384 (19)0.0339 (18)0.0333 (18)−0.0077 (14)0.0043 (15)0.0025 (15)
C1B0.0251 (16)0.0306 (16)0.0280 (17)−0.0036 (13)0.0000 (13)−0.0003 (14)
C11B0.0258 (16)0.0279 (17)0.0334 (17)−0.0009 (14)−0.0007 (13)0.0023 (15)
O11B0.0552 (14)0.0336 (12)0.0365 (12)−0.0221 (11)−0.0070 (10)0.0011 (10)
N11B0.0397 (15)0.0324 (15)0.0321 (14)−0.0174 (12)0.0086 (12)−0.0052 (12)
N12B0.0394 (15)0.0357 (14)0.0284 (14)−0.0065 (12)0.0096 (12)−0.0019 (12)
C2B0.0298 (17)0.0353 (18)0.0381 (18)0.0000 (15)−0.0008 (14)−0.0034 (16)
C3B0.0340 (19)0.053 (2)0.0281 (17)0.0029 (16)0.0049 (14)−0.0035 (16)
N31B0.051 (2)0.077 (3)0.046 (2)0.0013 (18)0.0094 (16)−0.0077 (19)
O31B0.123 (3)0.098 (2)0.063 (2)−0.031 (2)0.0344 (17)−0.0359 (19)
O32B0.112 (2)0.109 (3)0.0502 (17)−0.011 (2)0.0390 (17)0.0055 (18)
C4B0.047 (2)0.052 (2)0.042 (2)−0.0091 (18)0.0073 (17)0.0115 (19)
C5B0.055 (2)0.0328 (19)0.051 (2)−0.0122 (17)0.0038 (18)0.0057 (18)
C6B0.0411 (19)0.0340 (19)0.0347 (19)−0.0056 (15)0.0046 (15)−0.0031 (16)
N1A0.0381 (17)0.0395 (17)0.0295 (15)−0.0003 (13)0.0081 (13)−0.0109 (14)
O1A0.0268 (12)0.0586 (16)0.0487 (14)−0.0106 (11)0.0053 (10)−0.0038 (12)
O2A0.0754 (18)0.0577 (17)0.0405 (14)−0.0121 (14)0.0046 (12)0.0137 (13)
O3A0.0289 (12)0.0581 (15)0.0502 (14)0.0012 (12)0.0011 (11)0.0049 (13)
N1B0.0352 (16)0.0401 (17)0.0349 (15)−0.0143 (14)−0.0018 (13)−0.0052 (14)
O1B0.0386 (14)0.0502 (15)0.0520 (15)−0.0163 (11)0.0007 (11)0.0178 (12)
O2B0.0522 (15)0.0548 (15)0.0391 (13)−0.0167 (12)0.0121 (11)0.0088 (11)
O3B0.0341 (14)0.0755 (18)0.0716 (18)0.0063 (13)0.0002 (13)−0.0077 (15)
Geometric parameters (Å, °) top
Cd1—O11A2.287 (2)C6A—H6A0.9300
Cd1—O11B2.301 (2)C1B—C2B1.384 (4)
Cd1—N12A2.262 (2)C1B—C6B1.392 (4)
Cd1—N12B2.268 (2)C1B—C11B1.492 (4)
Cd1—O1A2.399 (2)C11B—O11B1.232 (3)
Cd1—O2A2.778 (2)C11B—N11B1.342 (3)
Cd1—O3Ai2.848 (2)N11B—N12B1.420 (3)
Cd1—O3B3.184 (3)N11B—H11B0.8831
C1A—C2A1.389 (4)N12B—H21B0.9017
C1A—C6A1.394 (4)N12B—H22B0.8532
C1A—C11A1.494 (4)C2B—C3B1.374 (4)
C11A—O11A1.238 (3)C2B—H2B0.9300
C11A—N11A1.333 (3)C3B—C4B1.365 (4)
N11A—N12A1.421 (3)C3B—N31B1.489 (4)
N11A—H11A0.8760N31B—O32B1.216 (4)
N12A—H21A0.8908N31B—O31B1.217 (4)
N12A—H22A0.8890C4B—C5B1.375 (4)
C2A—C3A1.381 (4)C4B—H4B0.9300
C2A—H2A0.9300C5B—C6B1.382 (4)
C3A—C4A1.380 (4)C5B—H5B0.9300
C3A—N31A1.471 (4)C6B—H6B0.9300
N31A—O32A1.218 (3)N1A—O3A1.238 (3)
N31A—O31A1.219 (3)N1A—O2A1.241 (3)
C4A—C5A1.387 (4)N1A—O1A1.274 (3)
C4A—H4A0.9300N1B—O3B1.232 (3)
C5A—C6A1.377 (4)N1B—O2B1.256 (3)
C5A—H5A0.9300N1B—O1B1.267 (3)
N12A—Cd1—N12B133.23 (9)C1A—C6A—H6A119.7
N12A—Cd1—O11A72.73 (8)C2B—C1B—C6B119.1 (3)
N12A—Cd1—O11B138.33 (8)C2B—C1B—C11B118.4 (3)
N12A—Cd1—O1A87.82 (8)C6B—C1B—C11B122.4 (3)
N12B—Cd1—O11B72.07 (8)O11B—C11B—N11B122.6 (3)
N12B—Cd1—O11A151.16 (8)O11B—C11B—C1B121.0 (3)
N12B—Cd1—O1A99.40 (8)N11B—C11B—C1B116.3 (3)
O11A—Cd1—O11B79.41 (7)C11B—O11B—Cd1113.88 (18)
O11A—Cd1—O1A93.12 (8)C11B—N11B—N12B118.2 (2)
O11B—Cd1—O1A124.58 (8)C11B—N11B—H11B123.3
C2A—C1A—C6A119.5 (3)N12B—N11B—H11B112.9
C2A—C1A—C11A122.7 (3)N11B—N12B—Cd1110.89 (16)
C6A—C1A—C11A117.8 (3)N11B—N12B—H21B110.5
O11A—C11A—N11A122.5 (3)Cd1—N12B—H21B104.4
O11A—C11A—C1A119.6 (3)N11B—N12B—H22B107.0
N11A—C11A—C1A117.9 (3)Cd1—N12B—H22B126.8
C11A—O11A—Cd1114.63 (18)H21B—N12B—H22B95.6
C11A—N11A—N12A119.2 (2)C3B—C2B—C1B118.6 (3)
C11A—N11A—H11A123.3C3B—C2B—H2B120.7
N12A—N11A—H11A117.5C1B—C2B—H2B120.7
N11A—N12A—Cd1110.48 (16)C4B—C3B—C2B123.2 (3)
N11A—N12A—H21A109.7C4B—C3B—N31B118.5 (3)
Cd1—N12A—H21A102.8C2B—C3B—N31B118.2 (3)
N11A—N12A—H22A103.7O32B—N31B—O31B123.6 (4)
Cd1—N12A—H22A113.0O32B—N31B—C3B118.8 (3)
H21A—N12A—H22A117.3O31B—N31B—C3B117.7 (3)
C3A—C2A—C1A118.5 (3)C3B—C4B—C5B118.0 (3)
C3A—C2A—H2A120.7C3B—C4B—H4B121.0
C1A—C2A—H2A120.7C5B—C4B—H4B121.0
C4A—C3A—C2A122.9 (3)C4B—C5B—C6B120.6 (3)
C4A—C3A—N31A118.4 (3)C4B—C5B—H5B119.7
C2A—C3A—N31A118.7 (3)C6B—C5B—H5B119.7
O32A—N31A—O31A123.3 (3)C5B—C6B—C1B120.4 (3)
O32A—N31A—C3A118.6 (3)C5B—C6B—H6B119.8
O31A—N31A—C3A118.1 (3)C1B—C6B—H6B119.8
C3A—C4A—C5A117.8 (3)O3A—N1A—O2A122.0 (3)
C3A—C4A—H4A121.1O3A—N1A—O1A119.8 (3)
C5A—C4A—H4A121.1O2A—N1A—O1A118.3 (3)
C6A—C5A—C4A120.7 (3)N1A—O1A—Cd1103.30 (18)
C6A—C5A—H5A119.7O3B—N1B—O2B121.6 (3)
C4A—C5A—H5A119.7O3B—N1B—O1B120.3 (3)
C5A—C6A—C1A120.6 (3)O2B—N1B—O1B118.0 (3)
C5A—C6A—H6A119.7
C2A—C1A—C11A—O11A−159.5 (3)C6B—C1B—C11B—N11B20.1 (4)
C6A—C1A—C11A—O11A17.5 (4)N11B—C11B—O11B—Cd115.5 (3)
C2A—C1A—C11A—N11A20.1 (4)C1B—C11B—O11B—Cd1−167.0 (2)
C6A—C1A—C11A—N11A−162.9 (3)N12A—Cd1—O11B—C11B−149.64 (19)
N11A—C11A—O11A—Cd1−6.3 (4)N12B—Cd1—O11B—C11B−13.7 (2)
C1A—C11A—O11A—Cd1173.26 (19)O11A—Cd1—O11B—C11B162.0 (2)
N12A—Cd1—O11A—C11A6.32 (19)O1A—Cd1—O11B—C11B75.5 (2)
N12B—Cd1—O11A—C11A163.6 (2)O11B—C11B—N11B—N12B−5.8 (4)
O11B—Cd1—O11A—C11A155.0 (2)C1B—C11B—N11B—N12B176.6 (2)
O1A—Cd1—O11A—C11A−80.4 (2)C11B—N11B—N12B—Cd1−7.1 (3)
O11A—C11A—N11A—N12A1.1 (4)N12A—Cd1—N12B—N11B150.76 (16)
C1A—C11A—N11A—N12A−178.5 (2)O11A—Cd1—N12B—N11B1.2 (3)
C11A—N11A—N12A—Cd14.7 (3)O11B—Cd1—N12B—N11B10.11 (16)
N12B—Cd1—N12A—N11A−170.52 (15)O1A—Cd1—N12B—N11B−113.34 (17)
O11A—Cd1—N12A—N11A−5.34 (16)C6B—C1B—C2B—C3B−1.3 (4)
O11B—Cd1—N12A—N11A−55.6 (2)C11B—C1B—C2B—C3B−178.6 (3)
O1A—Cd1—N12A—N11A88.61 (17)C1B—C2B—C3B—C4B0.5 (5)
C6A—C1A—C2A—C3A−0.5 (4)C1B—C2B—C3B—N31B−178.9 (2)
C11A—C1A—C2A—C3A176.5 (3)C4B—C3B—N31B—O32B0.1 (5)
C1A—C2A—C3A—C4A0.7 (4)C2B—C3B—N31B—O32B179.5 (3)
C1A—C2A—C3A—N31A−178.1 (3)C4B—C3B—N31B—O31B−179.2 (3)
C4A—C3A—N31A—O32A6.8 (4)C2B—C3B—N31B—O31B0.3 (5)
C2A—C3A—N31A—O32A−174.4 (3)C2B—C3B—C4B—C5B0.2 (5)
C4A—C3A—N31A—O31A−172.1 (3)N31B—C3B—C4B—C5B179.6 (3)
C2A—C3A—N31A—O31A6.7 (4)C3B—C4B—C5B—C6B−0.1 (5)
C2A—C3A—C4A—C5A−0.2 (5)C4B—C5B—C6B—C1B−0.8 (5)
N31A—C3A—C4A—C5A178.5 (3)C2B—C1B—C6B—C5B1.4 (4)
C3A—C4A—C5A—C6A−0.5 (5)C11B—C1B—C6B—C5B178.6 (3)
C4A—C5A—C6A—C1A0.7 (5)O3A—N1A—O1A—Cd1−158.5 (2)
C2A—C1A—C6A—C5A−0.2 (4)O2A—N1A—O1A—Cd121.3 (3)
C11A—C1A—C6A—C5A−177.3 (3)N12A—Cd1—O1A—N1A−178.19 (17)
C2B—C1B—C11B—O11B19.6 (4)N12B—Cd1—O1A—N1A48.31 (17)
C6B—C1B—C11B—O11B−157.6 (3)O11A—Cd1—O1A—N1A−105.62 (16)
C2B—C1B—C11B—N11B−162.8 (3)O11B—Cd1—O1A—N1A−26.34 (19)
Symmetry codes: (i) −x, −y+2, −z.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N11A—H11A···O1Bii0.881.982.833 (3)164.5
N12A—H21A···O2Biii0.892.122.963 (3)157.8
N12A—H22A···O3Aiv0.892.252.931 (3)133.3
N11B—H11B···O1Bv0.882.112.872 (3)144.3
N12B—H21B···O1Ai0.902.333.093 (3)142.2
N12B—H21B···O2Bv0.902.423.143 (3)137.5
N12B—H22B···O2Bvi0.852.303.124 (3)163.6
Symmetry codes: (ii) x, y+1, z; (iii) −x+1, −y+2, −z; (iv) x+1, y, z; (v) x−1, y, z; (i) −x, −y+2, −z; (vi) −x+1, −y+1, −z.
Table 1
Selected geometric parameters (Å, °) top
Cd1—O11A2.287 (2)Cd1—O1A2.399 (2)
Cd1—O11B2.301 (2)Cd1—O2A2.778 (2)
Cd1—N12A2.262 (2)Cd1—O3Ai2.848 (2)
Cd1—N12B2.268 (2)Cd1—O3B3.184 (3)
N12A—Cd1—N12B133.23 (9)N12B—Cd1—O11A151.16 (8)
N12A—Cd1—O11A72.73 (8)N12B—Cd1—O1A99.40 (8)
N12A—Cd1—O11B138.33 (8)O11A—Cd1—O11B79.41 (7)
N12A—Cd1—O1A87.82 (8)O11A—Cd1—O1A93.12 (8)
N12B—Cd1—O11B72.07 (8)O11B—Cd1—O1A124.58 (8)
Symmetry codes: (i) −x, −y+2, −z.
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N11A—H11A···O1Bii0.881.982.833 (3)164.5
N12A—H21A···O2Biii0.892.122.963 (3)157.8
N12A—H22A···O3Aiv0.892.252.931 (3)133.3
N11B—H11B···O1Bv0.882.112.872 (3)144.3
N12B—H21B···O1Ai0.902.333.093 (3)142.2
N12B—H21B···O2Bv0.902.423.143 (3)137.5
N12B—H22B···O2Bvi0.852.303.124 (3)163.6
Symmetry codes: (ii) x, y+1, z; (iii) −x+1, −y+2, −z; (iv) x+1, y, z; (v) x−1, y, z; (i) −x, −y+2, −z; (vi) −x+1, −y+1, −z.
references
References top

Brandenburg, K. (2005). DIAMOND. Release 3.0e. Crystal Impact GbR, Bonn, Germany.

Dowling, C., Murphy, V. J. & Parkin, G. (1996). Inorg. Chem. 35, 2415–2420.

Kleywegt, G. J., Wiesmeijer, W. G. R., Van Driel, G. J., Driessen, W. L., Reedijk, J. & Noordik, J. H. (1985). J. Chem. Soc. Dalton Trans. pp. 2177–2184.

Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Versions 1.171.30.3. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Westrip, S. P. (2007). PublCIF. In preparation.