| Literature DB >> 21200612 |
Luís Cunha-Silva, Fa-Nian Shi, Jacek Klinowski, Tito Trindade, João Rocha, Filipe A Almeida Paz.
Abstract
The title compound, [Zn(2)V(2)(C(5)H(6)NO(7)P)(2)O(2)(H(2)O)(10)]·2H(2)O, contains a [V(2)O(2)(pmida)(2)](4-) dimeric anionic unit [where H(4)pmida is N-(phosphono-meth-yl)imino-diacetic acid] lying on a centre of symmetry which is exo-coordinated via the two deprotonated phospho-nate groups to two Zn(2+) cations, with the coordination environment of Zn completed by five water mol-ecules. The crystal packing is mediated by an extensive network of strong and highly directional O-H⋯O hydrogen bonds involving the water mol-ecules (coordinated and uncoordinated) and the functional groups of pmida(4-), leading to a three-dimensional supra-molecular network.Entities:
Year: 2007 PMID: 21200612 PMCID: PMC2914926 DOI: 10.1107/S1600536807062253
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| [Zn2V2(C5H6NO7P)2O2(H2O)10]·2H2O | |
| Monoclinic, | Mo |
| Hall symbol: -P 2ybc | Cell parameters from 9009 reflections |
| θ = 2.6–37.6º | |
| µ = 2.40 mm−1 | |
| β = 111.147 (2)º | Prism, blue |
| 0.22 × 0.14 × 0.10 mm | |
| Bruker X8 APEXII Kappa CCD diffractometer | 4040 independent reflections |
| Radiation source: fine-focus sealed tube | 3765 reflections with |
| Monochromator: graphite | |
| θmax = 29.1º | |
| Thin–slice ω and φ scans | θmin = 3.6º |
| Absorption correction: multi-scan(SADABS; Sheldrick, 1998) | |
| 95509 measured reflections |
| Refinement on | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| H atoms treated by a mixture of independent and constrained refinement | |
| | |
| (Δ/σ)max = 0.002 | |
| 4040 reflections | Δρmax = 1.06 e Å−3 |
| 238 parameters | Δρmin = −0.87 e Å−3 |
| 15 restraints | Extinction correction: none |
| Primary atom site location: structure-invariant direct methods |
| Experimental. See dedicated section in the main paper |
| 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 |
| Zn1 | 0.47946 (2) | 0.566124 (16) | 0.26276 (2) | 0.02202 (7) | |
| V1 | 1.01192 (3) | 0.52639 (2) | 0.74230 (3) | 0.01679 (8) | |
| P1 | 0.81721 (5) | 0.55866 (3) | 0.44467 (5) | 0.01775 (10) | |
| N1 | 0.98913 (17) | 0.66771 (11) | 0.63798 (15) | 0.0188 (3) | |
| O5 | 0.85567 (14) | 0.49988 (10) | 0.57024 (13) | 0.0223 (3) | |
| O7 | 0.66854 (14) | 0.59666 (10) | 0.40459 (14) | 0.0242 (3) | |
| O4 | 1.16206 (16) | 0.60558 (10) | 0.87361 (13) | 0.0252 (3) | |
| C5 | 0.9481 (2) | 0.65025 (13) | 0.49415 (17) | 0.0199 (3) | |
| H5A | 1.0323 | 0.6340 | 0.4747 | 0.024* | |
| H5B | 0.9072 | 0.7041 | 0.4446 | 0.024* | |
| O6 | 0.83989 (15) | 0.50552 (10) | 0.33263 (14) | 0.0249 (3) | |
| O2 | 0.86146 (16) | 0.59104 (10) | 0.79428 (16) | 0.0275 (3) | |
| C4 | 1.1990 (2) | 0.68247 (13) | 0.84317 (19) | 0.0229 (4) | |
| C1 | 0.8075 (2) | 0.66657 (14) | 0.7474 (2) | 0.0239 (4) | |
| O8 | 1.0159 (2) | 0.43890 (11) | 0.83081 (18) | 0.0348 (4) | |
| C3 | 1.1313 (2) | 0.71027 (15) | 0.69835 (19) | 0.0263 (4) | |
| H3A | 1.1213 | 0.7751 | 0.6922 | 0.032* | |
| H3B | 1.1924 | 0.6920 | 0.6509 | 0.032* | |
| C2 | 0.8762 (2) | 0.71885 (14) | 0.6657 (2) | 0.0266 (4) | |
| H2A | 0.8027 | 0.7359 | 0.5824 | 0.032* | |
| H2B | 0.9176 | 0.7736 | 0.7125 | 0.032* | |
| O3 | 1.28796 (19) | 0.73187 (12) | 0.92367 (16) | 0.0371 (4) | |
| O1 | 0.70218 (18) | 0.69941 (11) | 0.76509 (19) | 0.0360 (4) | |
| O1W | 0.5041 (2) | 0.43314 (11) | 0.32805 (19) | 0.0392 (4) | |
| H1W | 0.440 (3) | 0.390 (2) | 0.288 (3) | 0.059* | |
| H2W | 0.528 (4) | 0.419 (2) | 0.414 (2) | 0.059* | |
| O2W | 0.36824 (16) | 0.59655 (11) | 0.39610 (15) | 0.0266 (3) | |
| H3W | 0.348 (3) | 0.6535 (14) | 0.402 (3) | 0.040* | |
| H4W | 0.298 (3) | 0.5638 (17) | 0.401 (3) | 0.040* | |
| O3W | 0.28954 (18) | 0.52927 (14) | 0.11685 (17) | 0.0409 (4) | |
| H5W | 0.238 (4) | 0.560 (2) | 0.045 (3) | 0.061* | |
| H6W | 0.234 (4) | 0.491 (2) | 0.136 (3) | 0.061* | |
| O4W | 0.45023 (17) | 0.69926 (11) | 0.19464 (16) | 0.0304 (3) | |
| H7W | 0.397 (3) | 0.706 (2) | 0.113 (2) | 0.046* | |
| H8W | 0.531 (3) | 0.727 (2) | 0.205 (3) | 0.046* | |
| O5W | 0.58091 (19) | 0.53840 (17) | 0.12317 (18) | 0.0446 (5) | |
| H9W | 0.666 (3) | 0.513 (2) | 0.170 (3) | 0.067* | |
| H10W | 0.598 (4) | 0.574 (2) | 0.068 (3) | 0.067* | |
| O6W | 0.5884 (6) | 0.6734 (4) | −0.0345 (5) | 0.1474 (18) |
| Zn1 | 0.01727 (12) | 0.02490 (13) | 0.01985 (12) | −0.00060 (8) | 0.00183 (8) | 0.00210 (8) |
| V1 | 0.01574 (14) | 0.01789 (15) | 0.01586 (14) | 0.00001 (10) | 0.00464 (11) | 0.00076 (10) |
| P1 | 0.01270 (19) | 0.0220 (2) | 0.0165 (2) | −0.00024 (16) | 0.00279 (16) | −0.00184 (16) |
| N1 | 0.0182 (7) | 0.0201 (7) | 0.0165 (7) | −0.0029 (6) | 0.0045 (5) | −0.0002 (5) |
| O5 | 0.0185 (6) | 0.0238 (6) | 0.0206 (6) | −0.0037 (5) | 0.0023 (5) | 0.0009 (5) |
| O7 | 0.0142 (6) | 0.0304 (7) | 0.0239 (6) | 0.0025 (5) | 0.0018 (5) | −0.0048 (6) |
| O4 | 0.0279 (7) | 0.0252 (7) | 0.0171 (6) | −0.0049 (6) | 0.0017 (5) | 0.0016 (5) |
| C5 | 0.0195 (8) | 0.0232 (8) | 0.0152 (7) | −0.0024 (7) | 0.0041 (6) | 0.0014 (6) |
| O6 | 0.0177 (6) | 0.0331 (7) | 0.0233 (6) | −0.0002 (5) | 0.0067 (5) | −0.0079 (6) |
| O2 | 0.0287 (7) | 0.0247 (7) | 0.0357 (8) | 0.0029 (6) | 0.0196 (6) | 0.0039 (6) |
| C4 | 0.0210 (8) | 0.0251 (9) | 0.0190 (8) | −0.0035 (7) | 0.0026 (7) | 0.0003 (7) |
| C1 | 0.0227 (9) | 0.0225 (9) | 0.0270 (9) | −0.0022 (7) | 0.0094 (7) | −0.0053 (7) |
| O8 | 0.0410 (9) | 0.0272 (8) | 0.0383 (9) | 0.0017 (7) | 0.0169 (7) | 0.0086 (7) |
| C3 | 0.0248 (9) | 0.0288 (10) | 0.0202 (8) | −0.0110 (8) | 0.0021 (7) | 0.0036 (7) |
| C2 | 0.0337 (10) | 0.0189 (8) | 0.0299 (10) | 0.0036 (8) | 0.0148 (8) | 0.0009 (7) |
| O3 | 0.0405 (9) | 0.0334 (8) | 0.0242 (7) | −0.0151 (7) | −0.0043 (7) | 0.0007 (6) |
| O1 | 0.0305 (8) | 0.0297 (8) | 0.0538 (10) | 0.0047 (6) | 0.0226 (8) | −0.0033 (7) |
| O1W | 0.0428 (10) | 0.0270 (8) | 0.0340 (9) | −0.0057 (7) | −0.0029 (7) | 0.0044 (7) |
| O2W | 0.0235 (7) | 0.0261 (7) | 0.0316 (7) | −0.0003 (6) | 0.0117 (6) | 0.0027 (6) |
| O3W | 0.0269 (8) | 0.0578 (12) | 0.0266 (8) | −0.0179 (8) | −0.0040 (6) | 0.0167 (8) |
| O4W | 0.0274 (7) | 0.0287 (8) | 0.0303 (8) | −0.0041 (6) | 0.0046 (6) | 0.0066 (6) |
| O5W | 0.0281 (8) | 0.0761 (14) | 0.0268 (8) | 0.0078 (9) | 0.0064 (7) | −0.0058 (9) |
| O6W | 0.163 (4) | 0.159 (5) | 0.143 (4) | −0.009 (4) | 0.083 (4) | 0.009 (3) |
| Zn1—O7 | 2.0133 (14) | C5—H5B | 0.9700 |
| Zn1—O3W | 2.0609 (16) | O6—V1i | 1.9890 (14) |
| Zn1—O1W | 2.0860 (17) | O2—C1 | 1.271 (3) |
| Zn1—O4W | 2.0974 (16) | C4—O3 | 1.238 (2) |
| Zn1—O5W | 2.1440 (18) | C4—C3 | 1.524 (3) |
| Zn1—O2W | 2.1660 (15) | C1—O1 | 1.239 (3) |
| V1—O8 | 1.6086 (16) | C1—C2 | 1.517 (3) |
| V1—O6i | 1.9890 (14) | C3—H3A | 0.9700 |
| V1—O5 | 1.9932 (14) | C3—H3B | 0.9700 |
| V1—O2 | 2.0312 (15) | C2—H2A | 0.9700 |
| V1—O4 | 2.0321 (14) | C2—H2B | 0.9700 |
| V1—N1 | 2.3590 (16) | O1W—H1W | 0.90 (2) |
| P1—O7 | 1.5030 (14) | O1W—H2W | 0.90 (2) |
| P1—O6 | 1.5324 (15) | O2W—H3W | 0.88 (2) |
| P1—O5 | 1.5443 (14) | O2W—H4W | 0.87 (2) |
| P1—C5 | 1.8323 (19) | O3W—H5W | 0.89 (2) |
| N1—C3 | 1.478 (2) | O3W—H6W | 0.88 (2) |
| N1—C2 | 1.481 (3) | O4W—H7W | 0.86 (2) |
| N1—C5 | 1.484 (2) | O4W—H8W | 0.88 (2) |
| O4—C4 | 1.282 (2) | O5W—H9W | 0.90 (2) |
| C5—H5A | 0.9700 | O5W—H10W | 0.86 (2) |
| O7—Zn1—O3W | 177.43 (8) | P1—O7—Zn1 | 134.17 (9) |
| O7—Zn1—O1W | 89.53 (7) | C4—O4—V1 | 123.17 (12) |
| O3W—Zn1—O1W | 88.34 (7) | N1—C5—P1 | 109.58 (12) |
| O7—Zn1—O4W | 91.64 (6) | N1—C5—H5A | 109.8 |
| O3W—Zn1—O4W | 90.49 (7) | P1—C5—H5A | 109.8 |
| O1W—Zn1—O4W | 178.81 (7) | N1—C5—H5B | 109.8 |
| O7—Zn1—O5W | 91.53 (6) | P1—C5—H5B | 109.8 |
| O3W—Zn1—O5W | 87.09 (8) | H5A—C5—H5B | 108.2 |
| O1W—Zn1—O5W | 91.61 (9) | P1—O6—V1i | 142.36 (9) |
| O4W—Zn1—O5W | 88.58 (8) | C1—O2—V1 | 123.99 (13) |
| O7—Zn1—O2W | 90.73 (6) | O3—C4—O4 | 123.37 (18) |
| O3W—Zn1—O2W | 90.71 (7) | O3—C4—C3 | 120.23 (18) |
| O1W—Zn1—O2W | 89.93 (7) | O4—C4—C3 | 116.37 (16) |
| O4W—Zn1—O2W | 89.83 (6) | O1—C1—O2 | 123.4 (2) |
| O5W—Zn1—O2W | 177.27 (7) | O1—C1—C2 | 118.61 (19) |
| O8—V1—O6i | 100.84 (8) | O2—C1—C2 | 118.02 (17) |
| O8—V1—O5 | 103.84 (8) | N1—C3—C4 | 109.82 (15) |
| O6i—V1—O5 | 91.21 (6) | N1—C3—H3A | 109.7 |
| O8—V1—O2 | 94.57 (8) | C4—C3—H3A | 109.7 |
| O6i—V1—O2 | 164.50 (7) | N1—C3—H3B | 109.7 |
| O5—V1—O2 | 86.67 (6) | C4—C3—H3B | 109.7 |
| O8—V1—O4 | 101.49 (8) | H3A—C3—H3B | 108.2 |
| O6i—V1—O4 | 87.20 (6) | N1—C2—C1 | 113.27 (16) |
| O5—V1—O4 | 154.45 (6) | N1—C2—H2A | 108.9 |
| O2—V1—O4 | 88.12 (6) | C1—C2—H2A | 108.9 |
| O8—V1—N1 | 169.79 (8) | N1—C2—H2B | 108.9 |
| O6i—V1—N1 | 88.57 (6) | C1—C2—H2B | 108.9 |
| O5—V1—N1 | 79.69 (6) | H2A—C2—H2B | 107.7 |
| O2—V1—N1 | 75.95 (6) | Zn1—O1W—H1W | 122 (2) |
| O4—V1—N1 | 74.78 (6) | Zn1—O1W—H2W | 121 (2) |
| O7—P1—O6 | 112.33 (8) | H1W—O1W—H2W | 103 (3) |
| O7—P1—O5 | 111.96 (8) | Zn1—O2W—H3W | 115.9 (19) |
| O6—P1—O5 | 110.11 (9) | Zn1—O2W—H4W | 123 (2) |
| O7—P1—C5 | 109.55 (9) | H3W—O2W—H4W | 109 (2) |
| O6—P1—C5 | 108.69 (8) | Zn1—O3W—H5W | 128 (2) |
| O5—P1—C5 | 103.82 (8) | Zn1—O3W—H6W | 119 (2) |
| C3—N1—C2 | 111.98 (16) | H5W—O3W—H6W | 109 (3) |
| C3—N1—C5 | 113.40 (15) | Zn1—O4W—H7W | 115 (2) |
| C2—N1—C5 | 111.14 (15) | Zn1—O4W—H8W | 113 (2) |
| C3—N1—V1 | 105.00 (11) | H7W—O4W—H8W | 106 (3) |
| C2—N1—V1 | 108.06 (11) | Zn1—O5W—H9W | 106 (2) |
| C5—N1—V1 | 106.80 (11) | Zn1—O5W—H10W | 130 (3) |
| P1—O5—V1 | 124.99 (8) | H9W—O5W—H10W | 105 (3) |
| O8—V1—N1—C3 | 95.2 (5) | O5—V1—O4—C4 | −10.3 (3) |
| O6i—V1—N1—C3 | −62.07 (12) | O2—V1—O4—C4 | −88.53 (16) |
| O5—V1—N1—C3 | −153.56 (13) | N1—V1—O4—C4 | −12.59 (15) |
| O2—V1—N1—C3 | 117.32 (13) | C3—N1—C5—P1 | 155.80 (14) |
| O4—V1—N1—C3 | 25.42 (12) | C2—N1—C5—P1 | −77.01 (17) |
| O8—V1—N1—C2 | −24.5 (5) | V1—N1—C5—P1 | 40.64 (13) |
| O6i—V1—N1—C2 | 178.27 (13) | O7—P1—C5—N1 | 89.70 (14) |
| O5—V1—N1—C2 | 86.78 (13) | O6—P1—C5—N1 | −147.23 (12) |
| O2—V1—N1—C2 | −2.35 (12) | O5—P1—C5—N1 | −30.04 (15) |
| O4—V1—N1—C2 | −94.24 (13) | O7—P1—O6—V1i | 147.90 (15) |
| O8—V1—N1—C5 | −144.1 (4) | O5—P1—O6—V1i | −86.60 (17) |
| O6i—V1—N1—C5 | 58.62 (11) | C5—P1—O6—V1i | 26.51 (19) |
| O5—V1—N1—C5 | −32.88 (11) | O8—V1—O2—C1 | −176.55 (17) |
| O2—V1—N1—C5 | −122.00 (12) | O6i—V1—O2—C1 | 9.6 (4) |
| O4—V1—N1—C5 | 146.11 (12) | O5—V1—O2—C1 | −72.91 (17) |
| O7—P1—O5—V1 | −116.85 (10) | O4—V1—O2—C1 | 82.07 (17) |
| O6—P1—O5—V1 | 117.44 (10) | N1—V1—O2—C1 | 7.29 (16) |
| C5—P1—O5—V1 | 1.24 (12) | V1—O4—C4—O3 | 178.20 (17) |
| O8—V1—O5—P1 | −173.68 (11) | V1—O4—C4—C3 | −4.0 (3) |
| O6i—V1—O5—P1 | −72.20 (11) | V1—O2—C1—O1 | 169.44 (16) |
| O2—V1—O5—P1 | 92.43 (11) | V1—O2—C1—C2 | −10.6 (3) |
| O4—V1—O5—P1 | 13.8 (2) | C2—N1—C3—C4 | 83.0 (2) |
| N1—V1—O5—P1 | 16.12 (10) | C5—N1—C3—C4 | −150.29 (17) |
| O6—P1—O7—Zn1 | 21.40 (16) | V1—N1—C3—C4 | −34.07 (19) |
| O5—P1—O7—Zn1 | −103.09 (13) | O3—C4—C3—N1 | −153.7 (2) |
| C5—P1—O7—Zn1 | 142.29 (12) | O4—C4—C3—N1 | 28.5 (3) |
| O1W—Zn1—O7—P1 | 52.88 (14) | C3—N1—C2—C1 | −116.61 (19) |
| O4W—Zn1—O7—P1 | −127.34 (14) | C5—N1—C2—C1 | 115.43 (18) |
| O5W—Zn1—O7—P1 | −38.72 (15) | V1—N1—C2—C1 | −1.4 (2) |
| O2W—Zn1—O7—P1 | 142.81 (13) | O1—C1—C2—N1 | −172.84 (19) |
| O8—V1—O4—C4 | 177.18 (16) | O2—C1—C2—N1 | 7.2 (3) |
| O6i—V1—O4—C4 | 76.69 (16) |
| H··· | ||||
| O1W—H1W···O1ii | 0.90 (2) | 1.88 (2) | 2.770 (2) | 169 (3) |
| O1W—H2W···O2Wii | 0.90 (2) | 1.95 (2) | 2.828 (2) | 164 (3) |
| O2W—H3W···O3iii | 0.88 (2) | 1.85 (2) | 2.725 (2) | 172 (3) |
| O2W—H4W···O5ii | 0.87 (2) | 1.93 (2) | 2.795 (2) | 173 (3) |
| O3W—H6W···O2ii | 0.88 (2) | 1.87 (2) | 2.733 (2) | 171 (3) |
| O3W—H5W···O4iv | 0.89 (2) | 1.86 (2) | 2.726 (2) | 164 (4) |
| O4W—H7W···O3iv | 0.86 (2) | 1.98 (2) | 2.837 (2) | 174 (3) |
| O4W—H8W···O1v | 0.88 (2) | 1.94 (2) | 2.799 (2) | 167 (3) |
| O5W—H9W···O6 | 0.90 (2) | 1.98 (3) | 2.805 (2) | 150 (4) |
| O5W—H10W···O6W | 0.86 (2) | 1.84 (3) | 2.656 (6) | 159 (4) |
Selected bond lengths (Å)
| Zn1—O7 | 2.0133 (14) |
| Zn1—O3 | 2.0609 (16) |
| Zn1—O1 | 2.0860 (17) |
| Zn1—O4 | 2.0974 (16) |
| Zn1—O5 | 2.1440 (18) |
| Zn1—O2 | 2.1660 (15) |
| V1—O8 | 1.6086 (16) |
| V1—O6i | 1.9890 (14) |
| V1—O5 | 1.9932 (14) |
| V1—O2 | 2.0312 (15) |
| V1—O4 | 2.0321 (14) |
| V1—N1 | 2.3590 (16) |
Symmetry code: (i) .
Hydrogen-bond geometry (Å, °)
| H⋯ | ||||
|---|---|---|---|---|
| O1 | 0.90 (2) | 1.88 (2) | 2.770 (2) | 169 (3) |
| O1 | 0.90 (2) | 1.95 (2) | 2.828 (2) | 164 (3) |
| O2 | 0.88 (2) | 1.85 (2) | 2.725 (2) | 172 (3) |
| O2 | 0.87 (2) | 1.93 (2) | 2.795 (2) | 173 (3) |
| O3 | 0.88 (2) | 1.87 (2) | 2.733 (2) | 171 (3) |
| O3 | 0.89 (2) | 1.86 (2) | 2.726 (2) | 164 (4) |
| O4 | 0.86 (2) | 1.98 (2) | 2.837 (2) | 174 (3) |
| O4 | 0.88 (2) | 1.94 (2) | 2.799 (2) | 167 (3) |
| O5 | 0.90 (2) | 1.98 (3) | 2.805 (2) | 150 (4) |
| O5 | 0.86 (2) | 1.84 (3) | 2.656 (6) | 159 (4) |
Symmetry codes: (ii) ; (iii) ; (iv) ; (v) .