supplementary materials
Bis(![[mu]](/logos/entities/mu_rmgif.gif)
-3,5-dinitrosalicylato)hexaimidazoledicadmium(II) dihydrate
The title dinuclear complex, [Cd2(C7H3N2O7)2(C3H4N2)6]·2H2O, lies about an inversion centre. Each CdII atom is coordinated by three O atoms from two 3,5-dinitrosalicylate ligands and the N atoms of three imidazole ligands. Three ligand O atoms and one N atom lie in the equatorial plane with the two other imidazole ligands axial in a distorted octahedral coordination environment. The intramolecular Cd
Cd separation is 3.906 (4) Å. In the crystal structure, a supramolecular network forms through extensive intermolecular hydrogen-bonding interactions. One imidazole ring is disordered over two orientations in ratio of approximately 0.8:0.2.
The title complex was prepared by the addition of a stoichiometric amount of
cadmium nitrate (20 mmol) and imidazole (20 mmol) to a hot aqueous solution
(25 ml) of 3,5-dinitrosalicylic acid (30 mmol). The pH was then adjusted to
7.0 to 8.0 with NaOH (30 mmol). The resulting solution was filtered, and
colorless crystals were obtained at room temperature on slow evaporation of
the solvent over several days.
Atoms C14, N6, C15 and C16 of one of the imidazole rings are disordered over two
positions such that the two disordered rings are inclined at 75.5 (8)° to one
another. The occupancy factor of the major disorder component refined to
0.792 (6). Carbon-bound H atoms were placed at calculated positions and were
treated as riding on the parent C atoms with C—H = 0.93 Å, N—H = 0.86 Å and with Uiso(H) = 1.2 Ueq(C, N). Water H atoms were
tentatively located in a difference Fourier map and were refined with distance
restraints of O–H = 0.85 Å and H···H = 1.39 Å, each within a standard
deviation of 0.01 Å; and Uiso(H) = 1.2 Ueq(O).
Data collection: APEXII (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2004); software used to prepare material for publication: SHELXTL.
Bis(µ-3,5-dinitrosalicylato)hexaimidazoledicadmium(II) dihydrate
top
Crystal data top
| [Cd2(C7H3N2O7)2(C3H4N2)6]·2H2O | Z = 1 |
| Mr = 1121.54 | F(000) = 560 |
| Triclinic, P1 | Dx = 1.791 Mg m−3 |
| Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
| a = 9.6267 (3) Å | Cell parameters from 4650 reflections |
| b = 10.5305 (3) Å | θ = 1.7–28.0° |
| c = 11.9560 (4) Å | µ = 1.11 mm−1 |
| α = 63.967 (2)° | T = 293 K |
| β = 73.013 (2)° | Block, colorless |
| γ = 79.712 (2)° | 0.25 × 0.20 × 0.18 mm |
| V = 1039.75 (6) Å3 | |
Data collection top
Bruker APEXII area-detector
diffractometer | 4797 independent reflections |
| Radiation source: fine-focus sealed tube | 4363 reflections with I > 2σ(I) |
| graphite | Rint = 0.028 |
| φ and ω scans | θmax = 27.6°, θmin = 2.0° |
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996) | h = −12→12 |
| Tmin = 0.768, Tmax = 0.825 | k = −13→13 |
| 17831 measured reflections | l = −15→15 |
Refinement top
| 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)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.063 | H atoms treated by a mixture of independent and constrained refinement |
| S = 1.04 | w = 1/[σ2(Fo2) + (0.0323P)2 + 0.3686P]
where P = (Fo2 + 2Fc2)/3 |
| 4797 reflections | (Δ/σ)max = 0.002 |
| 341 parameters | Δρmax = 0.59 e Å−3 |
| 6 restraints | Δρmin = −0.67 e Å−3 |
Crystal data top
| [Cd2(C7H3N2O7)2(C3H4N2)6]·2H2O | γ = 79.712 (2)° |
| Mr = 1121.54 | V = 1039.75 (6) Å3 |
| Triclinic, P1 | Z = 1 |
| a = 9.6267 (3) Å | Mo Kα radiation |
| b = 10.5305 (3) Å | µ = 1.11 mm−1 |
| c = 11.9560 (4) Å | T = 293 K |
| α = 63.967 (2)° | 0.25 × 0.20 × 0.18 mm |
| β = 73.013 (2)° | |
Data collection top
Bruker APEXII area-detector
diffractometer | 4797 independent reflections |
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996) | 4363 reflections with I > 2σ(I) |
| Tmin = 0.768, Tmax = 0.825 | Rint = 0.028 |
| 17831 measured reflections | θmax = 27.6° |
Refinement top
| R[F2 > 2σ(F2)] = 0.026 | H atoms treated by a mixture of independent and constrained refinement |
| wR(F2) = 0.063 | Δρmax = 0.59 e Å−3 |
| S = 1.04 | Δρmin = −0.67 e Å−3 |
| 4797 reflections | Absolute structure: ? |
| 341 parameters | Flack parameter: ? |
| 6 restraints | Rogers parameter: ? |
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 | Uiso*/Ueq | Occ. (<1) |
| C1 | 1.0356 (2) | 1.0810 (2) | 0.66201 (19) | 0.0293 (4) | |
| C2 | 0.9348 (2) | 1.0536 (2) | 0.79176 (19) | 0.0268 (4) | |
| C3 | 0.8365 (2) | 0.9396 (2) | 0.85829 (18) | 0.0263 (4) | |
| C4 | 0.7447 (2) | 0.9367 (2) | 0.9779 (2) | 0.0301 (4) | |
| C5 | 0.7498 (2) | 1.0257 (2) | 1.0315 (2) | 0.0333 (5) | |
| H5 | 0.6902 | 1.0151 | 1.1116 | 0.040* | |
| C6 | 0.8463 (2) | 1.1323 (2) | 0.9633 (2) | 0.0329 (5) | |
| C7 | 0.9366 (2) | 1.1464 (2) | 0.8448 (2) | 0.0310 (4) | |
| H7 | 0.9996 | 1.2197 | 0.8002 | 0.037* | |
| C8 | 1.0851 (3) | 0.6339 (3) | 0.7404 (2) | 0.0432 (6) | |
| H8 | 1.0668 | 0.6728 | 0.8001 | 0.052* | |
| C9 | 1.1692 (3) | 0.4916 (3) | 0.6460 (3) | 0.0635 (8) | |
| H9 | 1.2188 | 0.4171 | 0.6260 | 0.076* | |
| C10 | 1.0809 (3) | 0.5935 (3) | 0.5818 (3) | 0.0552 (7) | |
| H10 | 1.0582 | 0.6012 | 0.5085 | 0.066* | |
| C11 | 0.7147 (3) | 0.5666 (3) | 0.6729 (3) | 0.0649 (9) | |
| H11 | 0.7910 | 0.5560 | 0.6082 | 0.078* | |
| C12 | 0.6127 (4) | 0.4720 (4) | 0.7488 (4) | 0.0761 (10) | |
| H12 | 0.6052 | 0.3862 | 0.7468 | 0.091* | |
| C13 | 0.5730 (3) | 0.6516 (3) | 0.7986 (2) | 0.0496 (6) | |
| H13 | 0.5295 | 0.7110 | 0.8397 | 0.060* | |
| N5 | 0.6563 (2) | 1.0255 (2) | 0.5937 (2) | 0.0453 (5) | |
| C14 | 0.5098 (3) | 1.0074 (3) | 0.6268 (3) | 0.0427 (9) | 0.792 (6) |
| H14 | 0.4703 | 0.9193 | 0.6660 | 0.051* | 0.792 (6) |
| N6 | 0.4312 (4) | 1.1290 (5) | 0.5968 (5) | 0.0439 (10) | 0.792 (6) |
| H6 | 0.3383 | 1.1403 | 0.6070 | 0.053* | 0.792 (6) |
| C15 | 0.5259 (5) | 1.2320 (5) | 0.5468 (9) | 0.087 (2) | 0.792 (6) |
| H15 | 0.5036 | 1.3291 | 0.5175 | 0.104* | 0.792 (6) |
| C16 | 0.6577 (4) | 1.1664 (4) | 0.5481 (6) | 0.0833 (19) | 0.792 (6) |
| H16 | 0.7424 | 1.2138 | 0.5201 | 0.100* | 0.792 (6) |
| C14' | 0.6515 (15) | 1.1041 (17) | 0.4670 (12) | 0.058 (5) | 0.208 (6) |
| H14' | 0.7160 | 1.1048 | 0.3917 | 0.070* | 0.208 (6) |
| N6' | 0.5244 (17) | 1.1799 (19) | 0.4856 (13) | 0.077 (5) | 0.208 (6) |
| H6' | 0.4813 | 1.2355 | 0.4262 | 0.092* | 0.208 (6) |
| C15' | 0.477 (2) | 1.156 (3) | 0.607 (2) | 0.057 (7) | 0.208 (6) |
| H15' | 0.3909 | 1.1931 | 0.6457 | 0.069* | 0.208 (6) |
| C16' | 0.5808 (16) | 1.0657 (17) | 0.6632 (13) | 0.060 (5) | 0.208 (6) |
| H16' | 0.5879 | 1.0413 | 0.7462 | 0.072* | 0.208 (6) |
| Cd1 | 0.850613 (15) | 0.865319 (15) | 0.612784 (14) | 0.02985 (6) | |
| N1 | 1.0288 (2) | 0.6853 (2) | 0.6410 (2) | 0.0396 (4) | |
| N2 | 1.1718 (3) | 0.5189 (3) | 0.7456 (2) | 0.0532 (6) | |
| H2 | 1.2208 | 0.4706 | 0.8023 | 0.064* | |
| N3 | 0.6910 (2) | 0.6798 (2) | 0.70391 (19) | 0.0419 (5) | |
| N4 | 0.5238 (3) | 0.5281 (3) | 0.8282 (2) | 0.0636 (7) | |
| H4 | 0.4485 | 0.4905 | 0.8874 | 0.076* | |
| N7 | 0.8480 (2) | 1.2320 (2) | 1.0149 (2) | 0.0438 (5) | |
| N8 | 0.6355 (2) | 0.8313 (2) | 1.04896 (19) | 0.0384 (4) | |
| O1 | 0.83206 (16) | 0.84395 (15) | 0.82153 (13) | 0.0322 (3) | |
| O2 | 1.01862 (18) | 1.01829 (18) | 0.59849 (14) | 0.0429 (4) | |
| O3 | 1.13005 (17) | 1.16861 (17) | 0.61858 (16) | 0.0406 (4) | |
| O4 | 0.9334 (2) | 1.3270 (2) | 0.9547 (2) | 0.0656 (6) | |
| O5 | 0.7639 (2) | 1.2197 (2) | 1.1182 (2) | 0.0639 (6) | |
| O6 | 0.6302 (2) | 0.7591 (2) | 1.16355 (17) | 0.0640 (6) | |
| O7 | 0.55420 (19) | 0.8200 (2) | 0.99275 (19) | 0.0528 (5) | |
| O1W | 0.7629 (2) | 0.56782 (18) | 1.00690 (16) | 0.0445 (4) | |
| H2W | 0.783 (3) | 0.6497 (18) | 0.951 (2) | 0.053* | |
| H1W | 0.812 (3) | 0.506 (2) | 0.987 (3) | 0.053* | |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| C1 | 0.0279 (9) | 0.0333 (10) | 0.0255 (10) | −0.0051 (8) | −0.0032 (8) | −0.0117 (8) |
| C2 | 0.0284 (9) | 0.0278 (10) | 0.0236 (9) | −0.0023 (8) | −0.0036 (8) | −0.0114 (8) |
| C3 | 0.0292 (9) | 0.0254 (9) | 0.0231 (9) | −0.0031 (7) | −0.0045 (8) | −0.0093 (7) |
| C4 | 0.0327 (10) | 0.0272 (10) | 0.0275 (10) | −0.0066 (8) | −0.0011 (8) | −0.0107 (8) |
| C5 | 0.0355 (11) | 0.0363 (11) | 0.0268 (10) | −0.0041 (9) | 0.0009 (8) | −0.0164 (9) |
| C6 | 0.0394 (11) | 0.0319 (11) | 0.0325 (11) | −0.0048 (9) | −0.0038 (9) | −0.0198 (9) |
| C7 | 0.0318 (10) | 0.0313 (10) | 0.0307 (11) | −0.0071 (8) | −0.0024 (8) | −0.0147 (8) |
| C8 | 0.0435 (13) | 0.0465 (14) | 0.0406 (13) | −0.0047 (10) | −0.0084 (10) | −0.0191 (11) |
| C9 | 0.0635 (18) | 0.0553 (17) | 0.076 (2) | 0.0171 (14) | −0.0181 (16) | −0.0375 (16) |
| C10 | 0.0565 (16) | 0.0647 (18) | 0.0589 (17) | 0.0114 (13) | −0.0189 (13) | −0.0407 (15) |
| C11 | 0.0561 (16) | 0.0559 (17) | 0.083 (2) | −0.0225 (14) | 0.0106 (15) | −0.0395 (16) |
| C12 | 0.074 (2) | 0.0573 (19) | 0.095 (3) | −0.0318 (17) | −0.0073 (19) | −0.0274 (18) |
| C13 | 0.0445 (13) | 0.0635 (17) | 0.0393 (14) | −0.0131 (12) | −0.0044 (11) | −0.0195 (12) |
| N5 | 0.0478 (12) | 0.0412 (11) | 0.0470 (12) | 0.0005 (9) | −0.0138 (10) | −0.0180 (10) |
| C14 | 0.0361 (15) | 0.0462 (18) | 0.0457 (18) | −0.0083 (13) | −0.0067 (13) | −0.0187 (14) |
| N6 | 0.027 (2) | 0.0531 (19) | 0.055 (2) | −0.0005 (17) | −0.0075 (17) | −0.0273 (16) |
| C15 | 0.042 (2) | 0.043 (2) | 0.146 (6) | −0.0050 (19) | 0.000 (3) | −0.028 (3) |
| C16 | 0.0330 (18) | 0.043 (2) | 0.145 (5) | −0.0088 (15) | −0.002 (2) | −0.021 (2) |
| C14' | 0.049 (7) | 0.080 (10) | 0.026 (6) | 0.009 (7) | −0.003 (5) | −0.012 (6) |
| N6' | 0.086 (11) | 0.080 (11) | 0.053 (8) | 0.042 (8) | −0.046 (8) | −0.015 (7) |
| C15' | 0.026 (10) | 0.09 (2) | 0.062 (11) | 0.026 (11) | −0.017 (9) | −0.044 (12) |
| C16' | 0.061 (9) | 0.081 (11) | 0.037 (7) | 0.024 (8) | −0.027 (6) | −0.023 (7) |
| Cd1 | 0.03198 (9) | 0.03015 (9) | 0.02494 (9) | −0.00745 (6) | −0.00006 (6) | −0.01130 (6) |
| N1 | 0.0387 (10) | 0.0431 (11) | 0.0430 (11) | 0.0020 (8) | −0.0110 (9) | −0.0242 (9) |
| N2 | 0.0506 (13) | 0.0531 (13) | 0.0510 (14) | 0.0052 (10) | −0.0191 (11) | −0.0159 (11) |
| N3 | 0.0392 (10) | 0.0432 (11) | 0.0396 (11) | −0.0135 (8) | 0.0007 (8) | −0.0160 (9) |
| N4 | 0.0557 (14) | 0.0729 (17) | 0.0478 (14) | −0.0376 (13) | −0.0041 (11) | −0.0047 (12) |
| N7 | 0.0494 (11) | 0.0457 (11) | 0.0454 (12) | −0.0090 (9) | −0.0006 (9) | −0.0312 (10) |
| N8 | 0.0416 (10) | 0.0346 (10) | 0.0363 (10) | −0.0113 (8) | 0.0081 (8) | −0.0198 (8) |
| O1 | 0.0429 (8) | 0.0287 (7) | 0.0248 (7) | −0.0106 (6) | 0.0008 (6) | −0.0133 (6) |
| O2 | 0.0507 (9) | 0.0558 (10) | 0.0267 (8) | −0.0256 (8) | 0.0062 (7) | −0.0223 (7) |
| O3 | 0.0363 (8) | 0.0446 (9) | 0.0399 (9) | −0.0175 (7) | 0.0064 (7) | −0.0207 (7) |
| O4 | 0.0769 (13) | 0.0598 (12) | 0.0708 (14) | −0.0355 (11) | 0.0163 (11) | −0.0460 (11) |
| O5 | 0.0726 (13) | 0.0752 (14) | 0.0578 (12) | −0.0262 (11) | 0.0184 (10) | −0.0530 (11) |
| O6 | 0.0927 (15) | 0.0553 (12) | 0.0311 (9) | −0.0352 (11) | 0.0056 (9) | −0.0078 (8) |
| O7 | 0.0407 (9) | 0.0622 (12) | 0.0589 (12) | −0.0179 (8) | −0.0027 (8) | −0.0282 (10) |
| O1W | 0.0536 (10) | 0.0340 (9) | 0.0377 (9) | −0.0083 (8) | −0.0008 (8) | −0.0118 (7) |
Geometric parameters (Å, °) top
| C1—O3 | 1.245 (2) | N5—C14 | 1.373 (4) |
| C1—O2 | 1.262 (3) | N5—C14' | 1.382 (13) |
| C1—C2 | 1.503 (3) | N5—Cd1 | 2.276 (2) |
| C2—C7 | 1.384 (3) | C14—N6 | 1.323 (6) |
| C2—C3 | 1.447 (3) | C14—H14 | 0.9300 |
| C3—O1 | 1.275 (2) | N6—C15 | 1.354 (6) |
| C3—C4 | 1.435 (3) | N6—H6 | 0.8600 |
| C4—C5 | 1.362 (3) | C15—C16 | 1.333 (6) |
| C4—N8 | 1.459 (3) | C15—H15 | 0.9300 |
| C5—C6 | 1.383 (3) | C16—H16 | 0.9300 |
| C5—H5 | 0.9300 | C14'—N6' | 1.353 (19) |
| C6—C7 | 1.388 (3) | C14'—H14' | 0.9300 |
| C6—N7 | 1.437 (3) | N6'—C15' | 1.31 (3) |
| C7—H7 | 0.9300 | N6'—H6' | 0.8600 |
| C8—N1 | 1.305 (3) | C15'—C16' | 1.37 (2) |
| C8—N2 | 1.331 (3) | C15'—H15' | 0.9300 |
| C8—H8 | 0.9300 | C16'—H16' | 0.9300 |
| C9—C10 | 1.340 (4) | Cd1—N1 | 2.2949 (19) |
| C9—N2 | 1.348 (4) | Cd1—O2i | 2.3330 (14) |
| C9—H9 | 0.9300 | Cd1—O1 | 2.3606 (15) |
| C10—N1 | 1.381 (3) | Cd1—N3 | 2.3647 (18) |
| C10—H10 | 0.9300 | Cd1—O2 | 2.4015 (16) |
| C11—C12 | 1.348 (4) | N2—H2 | 0.8600 |
| C11—N3 | 1.360 (4) | N4—H4 | 0.8600 |
| C11—H11 | 0.9300 | N7—O4 | 1.229 (3) |
| C12—N4 | 1.349 (5) | N7—O5 | 1.229 (3) |
| C12—H12 | 0.9300 | N8—O7 | 1.220 (3) |
| C13—N3 | 1.317 (3) | N8—O6 | 1.231 (3) |
| C13—N4 | 1.327 (4) | O2—Cd1i | 2.3330 (14) |
| C13—H13 | 0.9300 | O1W—H2W | 0.839 (16) |
| N5—C16' | 1.115 (15) | O1W—H1W | 0.817 (16) |
| N5—C16 | 1.338 (4) | | |
| | | |
| O3—C1—O2 | 121.97 (18) | C16—C15—H15 | 126.9 |
| O3—C1—C2 | 119.04 (19) | N6—C15—H15 | 126.9 |
| O2—C1—C2 | 118.94 (17) | C15—C16—N5 | 113.4 (3) |
| C7—C2—C3 | 120.54 (18) | C15—C16—H16 | 123.3 |
| C7—C2—C1 | 116.47 (17) | N5—C16—H16 | 123.3 |
| C3—C2—C1 | 122.96 (18) | N6'—C14'—N5 | 98.6 (10) |
| O1—C3—C4 | 120.58 (17) | N6'—C14'—H14' | 130.7 |
| O1—C3—C2 | 125.47 (17) | N5—C14'—H14' | 130.7 |
| C4—C3—C2 | 113.87 (18) | C15'—N6'—C14' | 110.3 (13) |
| C5—C4—C3 | 125.37 (18) | C15'—N6'—H6' | 124.9 |
| C5—C4—N8 | 116.31 (18) | C14'—N6'—H6' | 124.9 |
| C3—C4—N8 | 118.31 (18) | N6'—C15'—C16' | 104.2 (15) |
| C4—C5—C6 | 117.91 (19) | N6'—C15'—H15' | 127.9 |
| C4—C5—H5 | 121.0 | C16'—C15'—H15' | 127.9 |
| C6—C5—H5 | 121.0 | N5—C16'—C15' | 109.0 (14) |
| C5—C6—C7 | 120.9 (2) | N5—C16'—H16' | 125.5 |
| C5—C6—N7 | 118.89 (19) | C15'—C16'—H16' | 125.5 |
| C7—C6—N7 | 120.17 (19) | N5—Cd1—N1 | 173.81 (7) |
| C2—C7—C6 | 121.32 (19) | N5—Cd1—O2i | 94.73 (7) |
| C2—C7—H7 | 119.3 | N1—Cd1—O2i | 89.21 (7) |
| C6—C7—H7 | 119.3 | N5—Cd1—O1 | 90.80 (7) |
| N1—C8—N2 | 111.5 (2) | N1—Cd1—O1 | 89.17 (6) |
| N1—C8—H8 | 124.3 | O2i—Cd1—O1 | 140.55 (5) |
| N2—C8—H8 | 124.3 | N5—Cd1—N3 | 89.69 (7) |
| C10—C9—N2 | 106.2 (3) | N1—Cd1—N3 | 84.13 (7) |
| C10—C9—H9 | 126.9 | O2i—Cd1—N3 | 130.33 (6) |
| N2—C9—H9 | 126.9 | O1—Cd1—N3 | 88.64 (6) |
| C9—C10—N1 | 109.6 (3) | N5—Cd1—O2 | 96.54 (7) |
| C9—C10—H10 | 125.2 | N1—Cd1—O2 | 89.33 (7) |
| N1—C10—H10 | 125.2 | O2i—Cd1—O2 | 68.82 (6) |
| C12—C11—N3 | 110.8 (3) | O1—Cd1—O2 | 71.75 (5) |
| C12—C11—H11 | 124.6 | N3—Cd1—O2 | 159.44 (7) |
| N3—C11—H11 | 124.6 | C8—N1—C10 | 104.9 (2) |
| C11—C12—N4 | 105.4 (3) | C8—N1—Cd1 | 121.98 (17) |
| C11—C12—H12 | 127.3 | C10—N1—Cd1 | 132.17 (18) |
| N4—C12—H12 | 127.3 | C8—N2—C9 | 107.9 (2) |
| N3—C13—N4 | 111.7 (3) | C8—N2—H2 | 126.1 |
| N3—C13—H13 | 124.1 | C9—N2—H2 | 126.1 |
| N4—C13—H13 | 124.1 | C13—N3—C11 | 104.3 (2) |
| C16'—N5—C16 | 69.1 (9) | C13—N3—Cd1 | 131.26 (19) |
| C16'—N5—C14 | 59.9 (9) | C11—N3—Cd1 | 124.20 (16) |
| C16—N5—C14 | 101.4 (2) | C13—N4—C12 | 107.8 (2) |
| C16'—N5—C14' | 115.2 (9) | C13—N4—H4 | 126.1 |
| C16—N5—C14' | 62.3 (7) | C12—N4—H4 | 126.1 |
| C14—N5—C14' | 90.3 (6) | O4—N7—O5 | 121.9 (2) |
| C16'—N5—Cd1 | 131.7 (7) | O4—N7—C6 | 119.18 (19) |
| C16—N5—Cd1 | 127.5 (2) | O5—N7—C6 | 118.9 (2) |
| C14—N5—Cd1 | 131.09 (19) | O7—N8—O6 | 123.7 (2) |
| C14'—N5—Cd1 | 111.7 (6) | O7—N8—C4 | 118.77 (19) |
| N6—C14—N5 | 112.6 (3) | O6—N8—C4 | 117.5 (2) |
| N6—C14—H14 | 123.7 | C3—O1—Cd1 | 129.08 (12) |
| N5—C14—H14 | 123.7 | C1—O2—Cd1i | 107.47 (12) |
| C14—N6—C15 | 106.4 (4) | C1—O2—Cd1 | 138.66 (13) |
| C14—N6—H6 | 126.8 | Cd1i—O2—Cd1 | 111.18 (6) |
| C15—N6—H6 | 126.8 | H2W—O1W—H1W | 113 (2) |
| C16—C15—N6 | 106.2 (4) | | |
| Symmetry codes: (i) −x+2, −y+2, −z+1. |
Hydrogen-bond geometry (Å, °) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| O1W—H1W···O4ii | 0.82 (2) | 2.16 (2) | 2.970 (3) | 174 (3) |
| N6—H6···O3iii | 0.86 | 1.95 | 2.805 (4) | 176 |
| N4—H4···O1Wiv | 0.86 | 2.09 | 2.932 (3) | 165 |
| N2—H2···O6v | 0.86 | 2.51 | 3.132 (3) | 130 |
| N2—H2···O1Wv | 0.86 | 2.18 | 2.915 (3) | 143 |
| O1W—H2W···O1 | 0.84 (2) | 1.99 (2) | 2.825 (2) | 179 (3) |
| Symmetry codes: (ii) x, y−1, z; (iii) x−1, y, z; (iv) −x+1, −y+1, −z+2; (v) −x+2, −y+1, −z+2. |
Table 1
Hydrogen-bond geometry (Å, °) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| O1W—H1W···O4i | 0.82 (2) | 2.16 (2) | 2.970 (3) | 174 (3) |
| N6—H6···O3ii | 0.86 | 1.95 | 2.805 (4) | 176 |
| N4—H4···O1Wiii | 0.86 | 2.09 | 2.932 (3) | 165 |
| N2—H2···O6iv | 0.86 | 2.51 | 3.132 (3) | 130 |
| N2—H2···O1Wiv | 0.86 | 2.18 | 2.915 (3) | 143 |
| O1W—H2W···O1 | 0.84 (2) | 1.99 (2) | 2.825 (2) | 179 (3) |
| Symmetry codes: (i) x, y−1, z; (ii) x−1, y, z; (iii) −x+1, −y+1, −z+2; (iv) −x+2, −y+1, −z+2. |
The authors acknowledge South China Normal University for supporting this work.
Bruker (2004). APEXII (Version 6.12) and SMART (Version 6.12). Bruker AXS Inc, Madison, Wisconsin, USA.
Othman, A. B., Effendy, initials?, Skelton, B. W. & White, A. H. (2003). Aust. J. Chem. 56, 719–721.
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (1997). SHELXL97 and SHELXS97. University of Göttingen, Germany.
Su, J.-R. & Xu, D.-J. (2005). Acta Cryst. E61, m1503–m1505.
Tian, L.-J., Yu, H.-X., Sun, Y.-X. & Zhang, B. (2005). Acta Cryst. E61, m2029–m2030.
![[Figure 1]](./sj2305fig1thm.gif)
Whereas a large number of metal derivatives of benzoic acid have been reported, there are few examples of metal derivatives of 3,5-dinitrosalicylic acid, and examples of crystal structure reports are limited to the silver (Othman et al., 2003), copper (Su & Xu, 2005) and tin (Tian et al., 2005) derivatives only. We report here a dinuclear cadmium(II) complex formed by the reaction of cadmium nitrate, 3,5-dinitrosalicylic acid and imidazole in an aqueous solution.
As illustrated in Fig. 1, in the asymmetric unit of (I) each CdII centre is coordinated by three O atoms from two 3,5-dinitrosalicylate ligands, three N atoms from three imidazole ligands, and displaying a distorted octahedral geometry. The complex lies about an inversion centre to form a dinuclear complex with a Cd···Cd separation of 3.906 (4) Å. Individual molecules are further extended into a supramolecular network through intermolecular hydrogen bonds (Table 1) involving both the complex and the water solvate.