Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807021460/sj2305sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807021460/sj2305Isup2.hkl |
CCDC reference: 629748
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).
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.
For related structures of 3,5-dinitrosalicylate complexes, see: Othman et al. (2003), Su & Xu (2005) and Tian et al. (2005).
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.
[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 |
Bruker APEXII area-detector diffractometer | 4797 independent reflections |
Radiation source: fine-focus sealed tube | 4363 reflections with I > 2σ(I) |
Graphite monochromator | 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 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 |
[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)° |
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 |
R[F2 > 2σ(F2)] = 0.026 | 6 restraints |
wR(F2) = 0.063 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | Δρmax = 0.59 e Å−3 |
4797 reflections | Δρmin = −0.67 e Å−3 |
341 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 | 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* |
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) |
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 code: (i) −x+2, −y+2, −z+1. |
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. |
Experimental details
Crystal data | |
Chemical formula | [Cd2(C7H3N2O7)2(C3H4N2)6]·2H2O |
Mr | 1121.54 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 9.6267 (3), 10.5305 (3), 11.9560 (4) |
α, β, γ (°) | 63.967 (2), 73.013 (2), 79.712 (2) |
V (Å3) | 1039.75 (6) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.11 |
Crystal size (mm) | 0.25 × 0.20 × 0.18 |
Data collection | |
Diffractometer | Bruker APEXII area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.768, 0.825 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 17831, 4797, 4363 |
Rint | 0.028 |
(sin θ/λ)max (Å−1) | 0.652 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.026, 0.063, 1.04 |
No. of reflections | 4797 |
No. of parameters | 341 |
No. of restraints | 6 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.59, −0.67 |
Computer programs: APEXII (Bruker, 2004), SAINT (Bruker, 2004), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2004), SHELXTL.
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O4i | 0.817 (16) | 2.156 (16) | 2.970 (3) | 174 (3) |
N6—H6···O3ii | 0.86 | 1.95 | 2.805 (4) | 176.3 |
N4—H4···O1Wiii | 0.86 | 2.09 | 2.932 (3) | 164.8 |
N2—H2···O6iv | 0.86 | 2.51 | 3.132 (3) | 129.7 |
N2—H2···O1Wiv | 0.86 | 2.18 | 2.915 (3) | 142.7 |
O1W—H2W···O1 | 0.839 (16) | 1.987 (16) | 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. |
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.