Acta Cryst. (2011). E67, m1407 [ doi:10.1107/S1600536811037573 ]
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N}cadmiumIn the title complex, [CdI2(C14H13N)2], the Cd atom lies on a twofold rotation axis that relates the I atom and the 4-(2-methylstyryl)pyridine ligand to their counterparts. Therefore the asymmetric unit contains one crystallographically independent half-molecule. The Cd atom adopts a tetrahedral coordination geometry, coordinated by two I atoms and two N atoms from the symmetry-related 4-(2-methylstyryl)pyridine ligands.
To a 10 mL Pyrex glass tube was loaded CdI2 (37 mg, 0.1 mmol), 4-(2-methylstyryl)pyridine (20 mg, 0.1 mmol) and 3 ml of H2O. The tube was sealed and heated in an oven to 160 °C for 3 d, and then cooled to ambient temperature at the rate of 5°C h-1 to form yellow crystals.
All the H atoms were placed in geometrically idealized positions (C–H = 0.95 Å for phenyl/pyridyl/vinyl groups and C–H = 0.98 Å for methyl groups) and constrained to ride on their parent atoms with Uiso(H) = 1.2Ueq(C) for phenyl/pyridyl/vinyl groups and Uiso(H) = 1.5Ueq(C) for methyl groups.
Data collection: CrystalClear (Rigaku, 2001); cell refinement: CrystalClear (Rigaku, 2001); data reduction: CrystalStructure (Rigaku/MSC, 2004); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).
![[Figure 1]](./bq2302fig1thm.gif)
| Fig. 1. Coordination environment of Cd in the compound with nonhydrogen atoms represented by thermal ellipsoids draw at 30% probability level, hydrogen atoms are drawn as spheres of arbitrary radius. [Symmetry code, i: - x, y, - z - 1/2.] |
| [CdI2(C14H13N)2] | F(000) = 1448 |
| Mr = 756.72 | Dx = 1.847 Mg m−3 |
| Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
| Hall symbol: -C 2yc | Cell parameters from 6049 reflections |
| a = 26.739 (5) Å | θ = 3.1–27.5° |
| b = 7.3613 (15) Å | µ = 3.09 mm−1 |
| c = 16.072 (3) Å | T = 223 K |
| β = 120.67 (3)° | Block, yellow |
| V = 2721.0 (12) Å3 | 0.35 × 0.30 × 0.25 mm |
| Z = 4 |
| Rigaku MercuryCCD area-detector diffractometer | 3106 independent reflections |
| Radiation source: fine-focus sealed tube | 2204 reflections with I > 2σ(I) |
| graphite | Rint = 0.051 |
| ω scans | θmax = 27.5°, θmin = 3.3° |
| Absorption correction: multi-scan (REQAB; Jacobson, 1998) | h = −33→31 |
| Tmin = 0.354, Tmax = 0.452 | k = −9→6 |
| 11814 measured reflections | l = −20→20 |
| 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)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.058 | H-atom parameters constrained |
| S = 0.83 | w = 1/[σ2(Fo2) + (0.0229P)2] where P = (Fo2 + 2Fc2)/3 |
| 3106 reflections | (Δ/σ)max = 0.001 |
| 151 parameters | Δρmax = 0.92 e Å−3 |
| 0 restraints | Δρmin = −0.57 e Å−3 |
| [CdI2(C14H13N)2] | V = 2721.0 (12) Å3 |
| Mr = 756.72 | Z = 4 |
| Monoclinic, C2/c | Mo Kα radiation |
| a = 26.739 (5) Å | µ = 3.09 mm−1 |
| b = 7.3613 (15) Å | T = 223 K |
| c = 16.072 (3) Å | 0.35 × 0.30 × 0.25 mm |
| β = 120.67 (3)° |
| Rigaku MercuryCCD area-detector diffractometer | 3106 independent reflections |
| Absorption correction: multi-scan (REQAB; Jacobson, 1998) | 2204 reflections with I > 2σ(I) |
| Tmin = 0.354, Tmax = 0.452 | Rint = 0.051 |
| 11814 measured reflections | θmax = 27.5° |
| R[F2 > 2σ(F2)] = 0.029 | H-atom parameters constrained |
| wR(F2) = 0.058 | Δρmax = 0.92 e Å−3 |
| S = 0.83 | Δρmin = −0.57 e Å−3 |
| 3106 reflections | Absolute structure: ? |
| 151 parameters | Flack parameter: ? |
| 0 restraints | Rogers parameter: ? |
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 | 0.0000 | 1.22721 (5) | 0.7500 | 0.03840 (11) | |
| I1 | 0.053615 (12) | 1.38570 (3) | 0.66568 (2) | 0.05147 (10) | |
| N1 | 0.06294 (12) | 1.0045 (4) | 0.8449 (2) | 0.0370 (7) | |
| C1 | 0.04379 (17) | 0.8800 (5) | 0.8835 (3) | 0.0472 (10) | |
| H1 | 0.0067 | 0.8965 | 0.8753 | 0.057* | |
| C2 | 0.07507 (16) | 0.7311 (5) | 0.9338 (3) | 0.0427 (9) | |
| H2 | 0.0594 | 0.6495 | 0.9595 | 0.051* | |
| C3 | 0.12992 (16) | 0.6994 (4) | 0.9473 (3) | 0.0387 (8) | |
| C4 | 0.14992 (16) | 0.8297 (5) | 0.9084 (3) | 0.0462 (10) | |
| H4 | 0.1870 | 0.8169 | 0.9161 | 0.055* | |
| C5 | 0.11640 (16) | 0.9759 (5) | 0.8594 (3) | 0.0447 (9) | |
| H5 | 0.1315 | 1.0611 | 0.8345 | 0.054* | |
| C6 | 0.16459 (16) | 0.5436 (5) | 0.9986 (3) | 0.0442 (9) | |
| H6 | 0.2028 | 0.5398 | 1.0102 | 0.053* | |
| C7 | 0.14763 (16) | 0.4041 (4) | 1.0314 (3) | 0.0386 (8) | |
| H7 | 0.1096 | 0.4109 | 1.0206 | 0.046* | |
| C8 | 0.18089 (16) | 0.2417 (4) | 1.0822 (2) | 0.0383 (8) | |
| C9 | 0.23779 (17) | 0.2147 (5) | 1.1024 (3) | 0.0468 (9) | |
| H9 | 0.2551 | 0.3034 | 1.0831 | 0.056* | |
| C10 | 0.26921 (18) | 0.0622 (6) | 1.1497 (3) | 0.0553 (11) | |
| H10 | 0.3074 | 0.0467 | 1.1626 | 0.066* | |
| C11 | 0.2436 (2) | −0.0677 (5) | 1.1780 (3) | 0.0577 (11) | |
| H11 | 0.2644 | −0.1731 | 1.2100 | 0.069* | |
| C12 | 0.18815 (18) | −0.0439 (5) | 1.1597 (3) | 0.0491 (10) | |
| H12 | 0.1716 | −0.1337 | 1.1798 | 0.059* | |
| C13 | 0.15574 (16) | 0.1084 (4) | 1.1126 (3) | 0.0386 (8) | |
| C14 | 0.09544 (18) | 0.1297 (5) | 1.0972 (3) | 0.0544 (11) | |
| H14A | 0.0833 | 0.0160 | 1.1121 | 0.082* | |
| H14B | 0.0685 | 0.1622 | 1.0304 | 0.082* | |
| H14C | 0.0957 | 0.2244 | 1.1394 | 0.082* |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Cd1 | 0.0410 (2) | 0.03176 (19) | 0.0471 (3) | 0.000 | 0.0258 (2) | 0.000 |
| I1 | 0.05478 (19) | 0.04516 (15) | 0.0666 (2) | 0.00138 (12) | 0.03979 (17) | 0.01120 (12) |
| N1 | 0.0339 (17) | 0.0353 (16) | 0.0432 (18) | −0.0012 (13) | 0.0207 (16) | 0.0020 (13) |
| C1 | 0.042 (2) | 0.048 (2) | 0.063 (3) | 0.0021 (18) | 0.035 (2) | 0.0091 (19) |
| C2 | 0.044 (2) | 0.040 (2) | 0.053 (3) | −0.0016 (17) | 0.031 (2) | 0.0103 (18) |
| C3 | 0.045 (2) | 0.0332 (18) | 0.041 (2) | −0.0024 (16) | 0.025 (2) | −0.0014 (16) |
| C4 | 0.039 (2) | 0.043 (2) | 0.066 (3) | 0.0038 (17) | 0.033 (2) | 0.0090 (19) |
| C5 | 0.045 (2) | 0.041 (2) | 0.054 (3) | −0.0046 (18) | 0.029 (2) | 0.0058 (18) |
| C6 | 0.034 (2) | 0.052 (2) | 0.046 (2) | 0.0045 (17) | 0.019 (2) | 0.0080 (18) |
| C7 | 0.040 (2) | 0.0359 (19) | 0.040 (2) | −0.0001 (16) | 0.021 (2) | 0.0009 (16) |
| C8 | 0.047 (2) | 0.0330 (18) | 0.037 (2) | 0.0022 (16) | 0.023 (2) | −0.0013 (15) |
| C9 | 0.049 (3) | 0.046 (2) | 0.045 (3) | 0.0011 (19) | 0.023 (2) | 0.0017 (18) |
| C10 | 0.048 (3) | 0.063 (3) | 0.046 (3) | 0.012 (2) | 0.018 (2) | 0.000 (2) |
| C11 | 0.071 (3) | 0.049 (2) | 0.043 (3) | 0.019 (2) | 0.022 (3) | 0.0122 (19) |
| C12 | 0.063 (3) | 0.040 (2) | 0.044 (2) | 0.0043 (19) | 0.028 (2) | 0.0044 (18) |
| C13 | 0.049 (2) | 0.0348 (18) | 0.032 (2) | 0.0034 (17) | 0.021 (2) | −0.0007 (15) |
| C14 | 0.068 (3) | 0.040 (2) | 0.073 (3) | 0.0037 (19) | 0.049 (3) | 0.0068 (19) |
| Cd1—N1i | 2.286 (3) | C7—C8 | 1.464 (5) |
| Cd1—N1 | 2.286 (3) | C7—H7 | 0.9400 |
| Cd1—I1i | 2.6898 (5) | C8—C9 | 1.398 (5) |
| Cd1—I1 | 2.6898 (5) | C8—C13 | 1.410 (4) |
| N1—C5 | 1.342 (4) | C9—C10 | 1.376 (5) |
| N1—C1 | 1.346 (4) | C9—H9 | 0.9400 |
| C1—C2 | 1.366 (5) | C10—C11 | 1.380 (5) |
| C1—H1 | 0.9400 | C10—H10 | 0.9400 |
| C2—C3 | 1.389 (4) | C11—C12 | 1.369 (5) |
| C2—H2 | 0.9400 | C11—H11 | 0.9400 |
| C3—C4 | 1.391 (4) | C12—C13 | 1.383 (5) |
| C3—C6 | 1.441 (5) | C12—H12 | 0.9400 |
| C4—C5 | 1.365 (5) | C13—C14 | 1.510 (5) |
| C4—H4 | 0.9400 | C14—H14A | 0.9700 |
| C5—H5 | 0.9400 | C14—H14B | 0.9700 |
| C6—C7 | 1.335 (4) | C14—H14C | 0.9700 |
| C6—H6 | 0.9400 | ||
| N1i—Cd1—N1 | 88.38 (14) | C6—C7—C8 | 128.0 (3) |
| N1i—Cd1—I1i | 104.30 (6) | C6—C7—H7 | 116.0 |
| N1—Cd1—I1i | 112.03 (6) | C8—C7—H7 | 116.0 |
| N1i—Cd1—I1 | 112.03 (6) | C9—C8—C13 | 118.3 (3) |
| N1—Cd1—I1 | 104.29 (6) | C9—C8—C7 | 121.7 (3) |
| I1i—Cd1—I1 | 128.59 (2) | C13—C8—C7 | 120.0 (3) |
| C5—N1—C1 | 115.8 (3) | C10—C9—C8 | 122.0 (3) |
| C5—N1—Cd1 | 125.8 (2) | C10—C9—H9 | 119.0 |
| C1—N1—Cd1 | 118.2 (2) | C8—C9—H9 | 119.0 |
| N1—C1—C2 | 123.9 (3) | C9—C10—C11 | 118.8 (4) |
| N1—C1—H1 | 118.1 | C9—C10—H10 | 120.6 |
| C2—C1—H1 | 118.1 | C11—C10—H10 | 120.6 |
| C1—C2—C3 | 120.4 (3) | C12—C11—C10 | 120.3 (4) |
| C1—C2—H2 | 119.8 | C12—C11—H11 | 119.8 |
| C3—C2—H2 | 119.8 | C10—C11—H11 | 119.8 |
| C2—C3—C4 | 115.5 (3) | C11—C12—C13 | 122.0 (3) |
| C2—C3—C6 | 122.9 (3) | C11—C12—H12 | 119.0 |
| C4—C3—C6 | 121.6 (3) | C13—C12—H12 | 119.0 |
| C5—C4—C3 | 120.9 (3) | C12—C13—C8 | 118.5 (3) |
| C5—C4—H4 | 119.6 | C12—C13—C14 | 119.5 (3) |
| C3—C4—H4 | 119.6 | C8—C13—C14 | 122.0 (3) |
| N1—C5—C4 | 123.5 (3) | C13—C14—H14A | 109.5 |
| N1—C5—H5 | 118.3 | C13—C14—H14B | 109.5 |
| C4—C5—H5 | 118.3 | H14A—C14—H14B | 109.5 |
| C7—C6—C3 | 126.2 (3) | C13—C14—H14C | 109.5 |
| C7—C6—H6 | 116.9 | H14A—C14—H14C | 109.5 |
| C3—C6—H6 | 116.9 | H14B—C14—H14C | 109.5 |
| Symmetry codes: (i) −x, y, −z+3/2. |
This work was supported by the Research Start-Up Fund for New Staff of Huaibei Normal University.
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In the past decades, the chemistry of cadmium coordination compounds has attracted much attention owing to their interesting synthetic chemistry and potential applications to luminescence. In this paper, we report the crystal structure of the title compound, a new cadmium complex obtained by the reaction of CdI2 and 4-(2-methylstyryl)pyridine.
The title complex crystallizes in the triclinic space group Pī, and the asymmetric unit consists of one crystallographically independent half-molecule. As shown in Fig. 1, each Cd atom is tetrahedrally coordinated by two I atoms and two N atoms from two 4-(2-methylstyryl)pyridine ligands. The mean Cd–I and Cd–N bond lengths are similar with those of the reported complexes (Park et al., 2010; Pickardt et al., 1999; Deng et al., 2009; Deiters et al., 2006; Amoedo-Portela et al., 2003).