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The title complex, [Zn(C9H7O2)2(H2O)2], shows a distorted octahedral coordination and has a crystallographic twofold rotation axis. Intermolecular O-H
O hydrogen bonding forms a two-dimensional network in the ab plane.
O hydrogen bonding forms a two-dimensional network in the ab plane.Supporting information
 | Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100003358/qa0239sup1.cif |
 | Structure factor file (CIF format) https://doi.org/10.1107/S0108270100003358/qa0239Isup2.hkl |
CCDC reference: 144687
S2. Experimental top
Crystals of (I) were grown from an aqueous solution. The crystal specimen was sealed in a capillary to avoid efflorescence.
S3. Refinement top
All H atoms were located from difference syntheses and refined isotropically. The O—H bond distances are 0.75 (5) and 0.84 (7) Å, and the C—H distances are in the range 0.86 (5)–0.98 (5) Å. The Flack parameter value of 0.13 (2) suggests the correct polar direction.
Computing details top
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: TEXSAN.
(I) top
Crystal data top
| [Zn(C9H7O2)2(H2O)2] | Dx = 1.531 Mg m−3 |
| Mr = 395.72 | Mo Kα radiation, λ = 0.71073 Å |
| Monoclinic, C2 | Cell parameters from 25 reflections |
| a = 11.728 (4) Å | θ = 14.5–15.0° |
| b = 5.105 (3) Å | µ = 1.46 mm−1 |
| c = 14.547 (2) Å | T = 299 K |
| β = 99.83 (2)° | Needle, colourless |
| V = 858.2 (5) Å3 | 0.7 × 0.15 × 0.1 mm |
| Z = 2 |
Data collection top
| Rigaku AFC-7R diffractometer | Rint = 0.019 |
| θ–2θ scans | θmax = 30°, θmin = 2.5° |
| Absorption correction: integration (Coppens et al., 1965) | h = 0→17 |
| Tmin = 0.802, Tmax = 0.872 | k = −7→0 |
| 1448 measured reflections | l = −20→20 |
| 1383 independent reflections | 3 standard reflections every 150 reflections |
| 1084 reflections with I > 2σ(I) | intensity decay: none |
Refinement top
| Refinement on F2 | w = 1/[σ2(Fo2) + (0.0404P)2 + 0.4323P] where P = (Fo2 + 2Fc2)/3 |
| R[F2 > 2σ(F2)] = 0.034 | (Δ/σ)max = 0.001 |
| wR(F2) = 0.088 | Δρmax = 0.46 e Å−3 |
| S = 1.05 | Δρmin = −0.42 e Å−3 |
| 1383 reflections | Absolute structure: Flack (1983), no Friedel pairs |
| 150 parameters | Absolute structure parameter: 0.13 (2) |
| All H-atom parameters refined |
Crystal data top
| [Zn(C9H7O2)2(H2O)2] | V = 858.2 (5) Å3 |
| Mr = 395.72 | Z = 2 |
| Monoclinic, C2 | Mo Kα radiation |
| a = 11.728 (4) Å | µ = 1.46 mm−1 |
| b = 5.105 (3) Å | T = 299 K |
| c = 14.547 (2) Å | 0.7 × 0.15 × 0.1 mm |
| β = 99.83 (2)° |
Data collection top
| Rigaku AFC-7R diffractometer | 1084 reflections with I > 2σ(I) |
| Absorption correction: integration (Coppens et al., 1965) | Rint = 0.019 |
| Tmin = 0.802, Tmax = 0.872 | 3 standard reflections every 150 reflections |
| 1448 measured reflections | intensity decay: none |
| 1383 independent reflections |
Refinement top
| R[F2 > 2σ(F2)] = 0.034 | All H-atom parameters refined |
| wR(F2) = 0.088 | Δρmax = 0.46 e Å−3 |
| S = 1.05 | Δρmin = −0.42 e Å−3 |
| 1383 reflections | Absolute structure: Flack (1983), no Friedel pairs |
| 150 parameters | Absolute structure parameter: 0.13 (2) |
Special details top
Refinement. Refinement was based on F2 against all reflections. The weighted R-factor (wR) and goodness of fit (S) were based on F2, and conventional R-factor (R) was calculated on F, with F set to zero for negative F2. The threshold expression of I > 2σ(I) was used only for calculating R-factor(gt). |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
| x | y | z | Uiso*/Ueq | ||
| Zn1 | 0.50000 | 0.81005 (1) | 1.00000 | 0.0376 (2) | |
| O2 | 0.4671 (2) | 0.5277 (6) | 0.8921 (2) | 0.0393 (6) | |
| O3 | 0.3110 (3) | 0.6379 (7) | 0.9457 (2) | 0.0459 (7) | |
| O4 | 0.5827 (3) | 1.0731 (7) | 0.9379 (3) | 0.0468 (8) | |
| C5 | 0.3591 (4) | 0.5011 (8) | 0.8926 (3) | 0.0373 (9) | |
| C6 | 0.2903 (3) | 0.3045 (18) | 0.8313 (3) | 0.0426 (8) | |
| C7 | 0.3331 (4) | 0.1466 (9) | 0.7754 (3) | 0.0389 (9) | |
| C8 | 0.2695 (4) | −0.0443 (9) | 0.7112 (3) | 0.0381 (9) | |
| C9 | 0.3281 (4) | −0.204 (2) | 0.6583 (3) | 0.0458 (9) | |
| C10 | 0.2708 (5) | −0.3814 (11) | 0.5953 (3) | 0.053 (1) | |
| C11 | 0.1534 (5) | −0.4024 (11) | 0.5840 (3) | 0.057 (1) | |
| C12 | 0.0923 (5) | −0.2491 (13) | 0.6359 (4) | 0.062 (2) | |
| C13 | 0.1496 (4) | −0.0705 (11) | 0.6995 (3) | 0.053 (1) | |
| H4A | 0.647 (5) | 1.089 (12) | 0.943 (3) | 0.0542 (2)* | |
| H4B | 0.541 (6) | 1.198 (15) | 0.914 (4) | 0.0897 (3)* | |
| H6 | 0.209 (5) | 0.32 (2) | 0.830 (3) | 0.0857 (2)* | |
| H7 | 0.406 (4) | 0.146 (12) | 0.775 (3) | 0.0539 (2)* | |
| H9 | 0.408 (3) | −0.210 (17) | 0.668 (2) | 0.0413 (1)* | |
| H10 | 0.313 (5) | −0.479 (14) | 0.562 (3) | 0.0717 (2)* | |
| H11 | 0.120 (4) | −0.538 (12) | 0.540 (3) | 0.0592 (2)* | |
| H12 | 0.013 (5) | −0.242 (15) | 0.623 (3) | 0.0687 (2)* | |
| H13 | 0.098 (5) | 0.015 (13) | 0.732 (4) | 0.0643 (2)* |
Atomic displacement parameters (Å2) top
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Zn1 | 0.0521 (4) | 0.0207 (2) | 0.0366 (3) | 0.0000 | −0.0017 (2) | 0.0000 |
| O2 | 0.036 (2) | 0.034 (2) | 0.045 (1) | −0.005 (1) | 0.000 (1) | 0.005 (1) |
| O3 | 0.045 (2) | 0.039 (2) | 0.050 (2) | 0.004 (1) | −0.001 (1) | −0.012 (1) |
| O4 | 0.039 (2) | 0.033 (2) | 0.068 (2) | 0.005 (1) | 0.005 (2) | 0.007 (2) |
| C5 | 0.041 (2) | 0.026 (2) | 0.040 (2) | −0.001 (2) | −0.008 (2) | 0.001 (2) |
| C6 | 0.037 (2) | 0.038 (2) | 0.050 (2) | −0.008 (3) | −0.002 (1) | −0.016 (4) |
| C7 | 0.038 (2) | 0.037 (2) | 0.040 (2) | −0.004 (2) | 0.004 (2) | −0.002 (2) |
| C8 | 0.046 (2) | 0.033 (2) | 0.034 (2) | −0.001 (2) | 0.002 (2) | 0.002 (2) |
| C9 | 0.050 (2) | 0.044 (2) | 0.042 (2) | 0.007 (4) | 0.004 (2) | −0.004 (4) |
| C10 | 0.076 (3) | 0.046 (3) | 0.035 (2) | 0.004 (3) | 0.008 (2) | −0.011 (2) |
| C11 | 0.075 (3) | 0.053 (3) | 0.037 (2) | −0.014 (3) | −0.005 (2) | −0.012 (2) |
| C12 | 0.055 (3) | 0.070 (5) | 0.058 (3) | −0.020 (3) | 0.003 (2) | −0.019 (3) |
| C13 | 0.049 (3) | 0.060 (3) | 0.049 (2) | −0.007 (2) | 0.009 (2) | −0.015 (2) |
Geometric parameters (Å, º) top
| Zn1—O2 | 2.118 (3) | C8—C9 | 1.381 (8) |
| Zn1—O3 | 2.390 (3) | C8—C13 | 1.394 (7) |
| Zn1—O4 | 1.965 (4) | C9—C10 | 1.380 (9) |
| O2—C5 | 1.275 (5) | C9—H9 | 0.92 (4) |
| O3—C5 | 1.246 (5) | C10—C11 | 1.363 (8) |
| O4—H4A | 0.75 (5) | C10—H10 | 0.90 (6) |
| O4—H4B | 0.84 (7) | C11—C12 | 1.371 (8) |
| C5—C6 | 1.487 (8) | C11—H11 | 0.98 (5) |
| C6—C7 | 1.305 (8) | C12—C13 | 1.388 (8) |
| C6—H6 | 0.95 (6) | C12—H12 | 0.92 (5) |
| C7—C8 | 1.463 (6) | C13—H13 | 0.94 (6) |
| C7—H7 | 0.86 (5) | ||
| O2—Zn1—O2i | 94.2 (2) | C6—C7—H7 | 120 (3) |
| O2—Zn1—O3 | 57.6 (1) | C8—C7—H7 | 113 (3) |
| O2—Zn1—O3i | 92.0 (1) | C7—C8—C9 | 120.0 (4) |
| O2—Zn1—O4 | 99.6 (1) | C7—C8—C13 | 122.4 (4) |
| O2—Zn1—O4i | 139.9 (1) | C9—C8—C13 | 117.6 (4) |
| O3—Zn1—O3i | 136.8 (2) | C8—C9—C10 | 121.7 (4) |
| O3—Zn1—O4 | 127.0 (1) | C8—C9—H9 | 121 (3) |
| O3—Zn1—O4i | 84.3 (1) | C10—C9—H9 | 116 (4) |
| O4—Zn1—O4i | 93.8 (2) | C9—C10—C11 | 120.0 (5) |
| Zn1—O2—C5 | 97.1 (2) | C9—C10—H10 | 117 (3) |
| Zn1—O3—C5 | 85.3 (2) | C11—C10—H10 | 122 (3) |
| Zn1—O4—H4A | 125 (4) | C10—C11—C12 | 120.0 (5) |
| Zn1—O4—H4B | 114 (4) | C10—C11—H11 | 114 (3) |
| H4A—O4—H4B | 118 (6) | C12—C11—H11 | 125 (3) |
| O2—C5—O3 | 120.0 (4) | C11—C12—C13 | 120.2 (5) |
| O2—C5—C6 | 120.4 (4) | C11—C12—H12 | 121 (3) |
| O3—C5—C6 | 119.5 (4) | C13—C12—H12 | 117 (4) |
| C5—C6—C7 | 124.3 (4) | C8—C13—C12 | 120.5 (5) |
| C5—C6—H6 | 114 (5) | C8—C13—H13 | 128 (3) |
| C7—C6—H6 | 121 (5) | C12—C13—H13 | 110 (3) |
| C6—C7—C8 | 126.9 (4) |
| Symmetry code: (i) −x+1, y, −z+2. |
Hydrogen-bond geometry (Å, º) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| O4—H4A···O3ii | 0.75 (5) | 1.93 (5) | 2.681 (5) | 175 (6) |
| O4—H4B···O2iii | 0.84 (7) | 1.90 (7) | 2.713 (4) | 163 (6) |
| Symmetry codes: (ii) x+1/2, y+1/2, z; (iii) x, y+1, z. |
Experimental details
| Crystal data | |
| Chemical formula | [Zn(C9H7O2)2(H2O)2] |
| Mr | 395.72 |
| Crystal system, space group | Monoclinic, C2 |
| Temperature (K) | 299 |
| a, b, c (Å) | 11.728 (4), 5.105 (3), 14.547 (2) |
| β (°) | 99.83 (2) |
| V (Å3) | 858.2 (5) |
| Z | 2 |
| Radiation type | Mo Kα |
| µ (mm−1) | 1.46 |
| Crystal size (mm) | 0.7 × 0.15 × 0.1 |
| Data collection | |
| Diffractometer | Rigaku AFC-7R diffractometer |
| Absorption correction | Integration (Coppens et al., 1965) |
| Tmin, Tmax | 0.802, 0.872 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 1448, 1383, 1084 |
| Rint | 0.019 |
| (sin θ/λ)max (Å−1) | 0.703 |
| Refinement | |
| R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.088, 1.05 |
| No. of reflections | 1383 |
| No. of parameters | 150 |
| No. of restraints | ? |
| H-atom treatment | All H-atom parameters refined |
| Δρmax, Δρmin (e Å−3) | 0.46, −0.42 |
| Absolute structure | Flack (1983), no Friedel pairs |
| Absolute structure parameter | 0.13 (2) |
Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation, 1999), SIR92 (Altomare et al., 1994), SHELXL97 (Sheldrick, 1997), TEXSAN.
Selected geometric parameters (Å, º) top
| Zn1—O2 | 2.118 (3) | O2—C5 | 1.275 (5) |
| Zn1—O3 | 2.390 (3) | O3—C5 | 1.246 (5) |
| Zn1—O4 | 1.965 (4) | ||
| O2—Zn1—O2i | 94.2 (2) | O3—Zn1—O3i | 136.8 (2) |
| O2—Zn1—O3 | 57.6 (1) | O3—Zn1—O4 | 127.0 (1) |
| O2—Zn1—O3i | 92.0 (1) | O3—Zn1—O4i | 84.3 (1) |
| O2—Zn1—O4 | 99.6 (1) | O4—Zn1—O4i | 93.8 (2) |
| O2—Zn1—O4i | 139.9 (1) |
| Symmetry code: (i) −x+1, y, −z+2. |
Hydrogen-bond geometry (Å, º) top
| D—H···A | D—H | H···A | D···A | D—H···A |
| O4—H4A···O3ii | 0.75 (5) | 1.93 (5) | 2.681 (5) | 175 (6) |
| O4—H4B···O2iii | 0.84 (7) | 1.90 (7) | 2.713 (4) | 163 (6) |
| Symmetry codes: (ii) x+1/2, y+1/2, z; (iii) x, y+1, z. |
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Metal–ligand interaction is one of the possibilities of controlling the relative arrangement of the trans-cinnamate ions in the crystals to yield the desired photodimer (Ito, 1998). The structure of cis-diaquabis(trans-cinnamato-O,O')zinc(II), (I), has been determined and is presented here.