metal-organic compounds
In the title compound, [Cd(C7H7N2O4)2]n, C7H7N2O4− zwitterions link Cd2+ cations into a network of [Cd(C7H7N2O4)2]n sheets. The carboxylate arms of the ligand chelate to the metal, which shows square-antiprismatic coordination. The Cd2+ ion occupies a special position 2 site symmetry. The crystals were found to be twinned.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806041407/ci2185sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806041407/ci2185Isup2.hkl |
CCDC reference: 627457
Computing details top
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: SHELXL97.
Crystal data top
[Cd(C7H7N2O4)2] | Dx = 2.001 Mg m−3 |
Mr = 478.69 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I41/a | Cell parameters from 11950 reflections |
Hall symbol: -I 4ad | θ = 3.4–27.5° |
a = 14.9585 (4) Å | µ = 1.43 mm−1 |
c = 14.2034 (4) Å | T = 295 K |
V = 3178.11 (11) Å3 | Prism, colourless |
Z = 8 | 0.30 × 0.24 × 0.18 mm |
F(000) = 1904 |
Data collection top
Rigaku R-AXIS RAPID IP diffractometer | 1814 independent reflections |
Radiation source: fine-focus sealed tube | 1602 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
ω scans | θmax = 27.5°, θmin = 3.4° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −19→19 |
Tmin = 0.570, Tmax = 0.783 | k = −19→19 |
15612 measured reflections | l = −18→18 |
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)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.053 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0317P)2 + 0.193P] where P = (Fo2 + 2Fc2)/3 |
1814 reflections | (Δ/σ)max = 0.001 |
124 parameters | Δρmax = 0.29 e Å−3 |
0 restraints | Δρmin = −0.37 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Cd1 | 1.0000 | 0.2500 | 0.36280 (2) | 0.02957 (8) | |
O1 | 1.0087 (2) | 0.1377 (1) | 0.4771 (1) | 0.0519 (5) | |
O2 | 0.8711 (1) | 0.1905 (1) | 0.4717 (1) | 0.0466 (5) | |
O3 | 0.6122 (1) | −0.2714 (1) | 0.5030 (2) | 0.0469 (5) | |
O4 | 0.5778 (1) | −0.1304 (1) | 0.4732 (1) | 0.0387 (5) | |
N1 | 0.8191 (1) | 0.0356 (1) | 0.5805 (2) | 0.0285 (5) | |
N2 | 0.7224 (1) | −0.0716 (2) | 0.5825 (2) | 0.0305 (6) | |
C1 | 0.9288 (2) | 0.1403 (2) | 0.5039 (2) | 0.0333 (6) | |
C2 | 0.9068 (2) | 0.0793 (2) | 0.5865 (2) | 0.0396 (7) | |
C3 | 0.7359 (2) | 0.0748 (2) | 0.5837 (2) | 0.0388 (7) | |
C4 | 0.6758 (2) | 0.0078 (2) | 0.5855 (2) | 0.0382 (7) | |
C5 | 0.8086 (2) | −0.0525 (2) | 0.5788 (2) | 0.0293 (5) | |
C6 | 0.6871 (2) | −0.1626 (2) | 0.5915 (2) | 0.0377 (7) | |
C7 | 0.6208 (2) | −0.1889 (2) | 0.5160 (2) | 0.0326 (6) | |
H2a | 0.9525 | 0.0336 | 0.5909 | 0.048* | |
H2b | 0.9090 | 0.1142 | 0.6441 | 0.048* | |
H3 | 0.7236 | 0.1357 | 0.5845 | 0.047* | |
H4 | 0.6140 | 0.0141 | 0.5882 | 0.046* | |
H5 | 0.8547 | −0.0941 | 0.5755 | 0.035* | |
H6a | 0.6584 | −0.1683 | 0.6524 | 0.045* | |
H6b | 0.7368 | −0.2043 | 0.5900 | 0.045* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0293 (1) | 0.0242 (1) | 0.0352 (1) | 0.0030 (1) | 0.000 | 0.000 |
O1 | 0.046 (1) | 0.047 (1) | 0.063 (1) | −0.003 (1) | 0.023 (1) | 0.010 (1) |
O2 | 0.044 (1) | 0.042 (1) | 0.054 (1) | −0.009 (1) | −0.006 (1) | 0.016 (1) |
O3 | 0.046 (1) | 0.033 (1) | 0.062 (1) | −0.003 (1) | −0.011 (1) | −0.011 (1) |
O4 | 0.038 (1) | 0.041 (1) | 0.037 (1) | −0.005 (1) | −0.007 (1) | 0.003 (1) |
N1 | 0.026 (1) | 0.031 (1) | 0.028 (1) | −0.004 (1) | −0.001 (1) | 0.005 (1) |
N2 | 0.031 (1) | 0.031 (1) | 0.030 (1) | −0.006 (1) | −0.002 (1) | 0.000 (1) |
C1 | 0.039 (1) | 0.031 (1) | 0.030 (1) | −0.014 (1) | 0.003 (1) | −0.004 (1) |
C2 | 0.031 (2) | 0.049 (2) | 0.039 (1) | −0.010 (1) | −0.004 (1) | 0.011 (1) |
C3 | 0.034 (2) | 0.031 (2) | 0.051 (2) | 0.005 (2) | 0.009 (2) | −0.007 (1) |
C4 | 0.027 (1) | 0.041 (2) | 0.047 (2) | −0.003 (2) | 0.008 (1) | −0.009 (2) |
C5 | 0.026 (2) | 0.035 (2) | 0.028 (1) | 0.001 (1) | −0.002 (1) | 0.005 (1) |
C6 | 0.040 (2) | 0.032 (2) | 0.041 (1) | −0.011 (1) | −0.009 (1) | 0.007 (1) |
C7 | 0.026 (1) | 0.037 (1) | 0.035 (2) | −0.006 (1) | 0.006 (1) | −0.003 (1) |
Geometric parameters (Å, º) top
Cd1—O1 | 2.339 (2) | N1—C2 | 1.469 (3) |
Cd1—O1i | 2.339 (2) | N2—C5 | 1.322 (4) |
Cd1—O2 | 2.627 (2) | N2—C4 | 1.379 (4) |
Cd1—O2i | 2.627 (2) | N2—C6 | 1.466 (3) |
Cd1—O3ii | 2.372 (2) | C1—C2 | 1.522 (4) |
Cd1—O3iii | 2.372 (2) | C3—C4 | 1.346 (3) |
Cd1—O4ii | 2.460 (2) | C6—C7 | 1.512 (4) |
Cd1—O4iii | 2.460 (2) | C2—H2a | 0.97 |
O1—C1 | 1.255 (3) | C2—H2b | 0.97 |
O2—C1 | 1.232 (3) | C3—H3 | 0.93 |
O3—C7 | 1.254 (4) | C4—H4 | 0.93 |
O4—C7 | 1.245 (3) | C5—H5 | 0.93 |
N1—C5 | 1.327 (4) | C6—H6a | 0.97 |
N1—C3 | 1.375 (4) | C6—H6b | 0.97 |
O1—Cd1—O1i | 92.1 (1) | C5—N1—C2 | 123.3 (2) |
O1—Cd1—O2 | 52.3 (1) | C3—N1—C2 | 128.0 (2) |
O1—Cd1—O2i | 78.1 (1) | C5—N2—C4 | 107.9 (3) |
O1—Cd1—O3ii | 88.9 (1) | C5—N2—C6 | 123.8 (2) |
O1—Cd1—O3iii | 169.1 (1) | C4—N2—C6 | 128.0 (2) |
O1—Cd1—O4ii | 88.0 (1) | O2—C1—O1 | 124.9 (3) |
O1—Cd1—O4iii | 136.5 (1) | O2—C1—C2 | 120.0 (3) |
O1i—Cd1—O2 | 78.1 (1) | O1—C1—C2 | 114.9 (3) |
O1i—Cd1—O2i | 52.3 (1) | N1—C2—C1 | 114.5 (2) |
O1i—Cd1—O3ii | 169.1 (1) | C4—C3—N1 | 106.7 (3) |
O1i—Cd1—O3iii | 88.9 (1) | C3—C4—N2 | 107.7 (3) |
O1i—Cd1—O4ii | 136.5 (1) | N2—C5—N1 | 109.2 (2) |
O1i—Cd1—O4iii | 88.0 (1) | N2—C6—C7 | 114.6 (2) |
O2—Cd1—O2i | 107.9 (1) | O4—C7—O3 | 124.5 (3) |
O2—Cd1—O3ii | 94.0 (1) | O4—C7—C6 | 120.1 (2) |
O2—Cd1—O3iii | 138.3 (1) | O3—C7—C6 | 115.3 (3) |
O2—Cd1—O4ii | 131.8 (1) | N1—C2—H2a | 108.6 |
O2—Cd1—O4iii | 85.3 (1) | C1—C2—H2a | 108.6 |
O2i—Cd1—O3ii | 138.3 (1) | N1—C2—H2b | 108.6 |
O2i—Cd1—O3iii | 94.0 (1) | C1—C2—H2b | 108.6 |
O2i—Cd1—O4ii | 85.3 (1) | H2a—C2—H2b | 107.6 |
O2i—Cd1—O4iii | 131.8 (1) | C4—C3—H3 | 126.7 |
O3ii—Cd1—O3iii | 92.2 (1) | N1—C3—H3 | 126.7 |
O3ii—Cd1—O4ii | 54.5 (1) | C3—C4—H4 | 126.2 |
O3ii—Cd1—O4iii | 83.8 (1) | N2—C4—H4 | 126.2 |
O3iii—Cd1—O4ii | 83.8 (1) | N2—C5—H5 | 125.4 |
O3iii—Cd1—O4iii | 54.5 (1) | N1—C5—H5 | 125.4 |
O4ii—Cd1—O4iii | 120.4 (1) | N2—C6—H6a | 108.6 |
C1—O1—Cd1 | 97.8 (2) | C7—C6—H6a | 108.6 |
C1—O2—Cd1 | 84.9 (2) | N2—C6—H6b | 108.6 |
C7—O3—Cd1iv | 92.4 (2) | C7—C6—H6b | 108.6 |
C7—O4—Cd1iv | 88.6 (2) | H6a—C6—H6b | 107.6 |
C5—N1—C3 | 108.5 (2) | ||
O1i—Cd1—O1—C1 | 72.9 (2) | O2—C1—C2—N1 | 42.2 (4) |
O3ii—Cd1—O1—C1 | −96.2 (2) | O1—C1—C2—N1 | −141.3 (3) |
O3iii—Cd1—O1—C1 | 168.1 (3) | C5—N1—C3—C4 | 1.0 (4) |
O4ii—Cd1—O1—C1 | −150.7 (2) | C2—N1—C3—C4 | −173.7 (3) |
O4iii—Cd1—O1—C1 | −16.4 (2) | N1—C3—C4—N2 | −0.6 (4) |
O2i—Cd1—O1—C1 | 123.7 (2) | C5—N2—C4—C3 | −0.1 (4) |
O2—Cd1—O1—C1 | −0.3 (2) | C6—N2—C4—C3 | 173.9 (3) |
O1i—Cd1—O2—C1 | −101.8 (2) | C4—N2—C5—N1 | 0.8 (3) |
O1—Cd1—O2—C1 | 0.3 (2) | C6—N2—C5—N1 | −173.6 (3) |
O3ii—Cd1—O2—C1 | 85.8 (2) | C3—N1—C5—N2 | −1.1 (3) |
O3iii—Cd1—O2—C1 | −176.4 (1) | C2—N1—C5—N2 | 173.9 (2) |
O4ii—Cd1—O2—C1 | 41.8 (2) | C5—N2—C6—C7 | −125.3 (3) |
O4iii—Cd1—O2—C1 | 169.3 (2) | C4—N2—C6—C7 | 61.5 (4) |
O2i—Cd1—O2—C1 | −58.2 (2) | Cd1iv—O4—C7—O3 | 0.4 (3) |
Cd1—O2—C1—O1 | −0.6 (3) | Cd1iv—O4—C7—C6 | −177.7 (2) |
Cd1—O2—C1—C2 | 175.5 (2) | Cd1iv—O3—C7—O4 | −0.4 (3) |
Cd1—O1—C1—O2 | 0.6 (3) | Cd1iv—O3—C7—C6 | 177.8 (2) |
Cd1—O1—C1—C2 | −175.7 (2) | N2—C6—C7—O4 | −24.0 (4) |
C5—N1—C2—C1 | 119.8 (3) | N2—C6—C7—O3 | 157.6 (3) |
C3—N1—C2—C1 | −66.1 (4) |
Symmetry codes: (i) −x+2, −y+1/2, z; (ii) y+5/4, −x+3/4, −z+3/4; (iii) −y+3/4, x−1/4, −z+3/4; (iv) y+1/4, −x+3/4, −z+3/4. |