| Literature DB >> 22719316 |
Radosław Starosta1, Urszula K Komarnicka, Justyna Nagaj, Kamila Stokowa-Sołtys, Aleksandra Bykowska.
Abstract
In the centrosymmetric dinuclear title complex, [Cu(2)I(2)(C(22)H(16)N(2)O(4))(2)], the Cu(I) atom is coordinated in a distorted tetra-hedral geometry by an N,N'-bidentate dimethyl 2,2'-biquinoline-4,4'-dicarboxyl-ate ligand and two symmetry-related I atoms, which act as bridges to a symmetry-related Cu(I) atom. The distance between the Cu(I) atoms within the dinuclear unit is 2.6723 (11) Å.Entities:
Year: 2012 PMID: 22719316 PMCID: PMC3379095 DOI: 10.1107/S1600536812020843
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| [Cu2I2(C22H16N2O4)2] | |
| Triclinic, | |
| Hall symbol: -P 1 | Mo |
| Cell parameters from 11359 reflections | |
| θ = 2.9–36.8° | |
| µ = 2.76 mm−1 | |
| α = 96.59 (3)° | |
| β = 102.49 (3)° | Plate, orange |
| γ = 103.51 (3)° | 0.15 × 0.10 × 0.10 mm |
| Kuma KM-4-CCD κ-geometry diffractometer | 5471 independent reflections |
| Radiation source: fine-focus sealed tube | 4606 reflections with |
| Graphite monochromator | |
| ω scans | θmax = 30.0°, θmin = 2.9° |
| Absorption correction: analytical [ | |
| 15308 measured reflections |
| Refinement on | Primary atom site location: structure-invariant direct methods |
| Least-squares matrix: full | Secondary atom site location: difference Fourier map |
| Hydrogen site location: inferred from neighbouring sites | |
| H-atom parameters constrained | |
| 5471 reflections | (Δ/σ)max = 0.001 |
| 273 parameters | Δρmax = 0.89 e Å−3 |
| 0 restraints | Δρmin = −1.16 e Å−3 |
| Experimental. Absorption correction: CrysAlis RED, (Oxford Diffraction, 2006). Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S., 1995) |
| 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 |
| Cu1 | 0.34262 (3) | −0.02511 (3) | 0.49564 (2) | 0.01649 (7) | |
| I1 | 0.495174 (17) | 0.240323 (17) | 0.478225 (12) | 0.01826 (5) | |
| N1A | 0.1380 (2) | −0.1629 (2) | 0.38141 (15) | 0.0142 (3) | |
| C2A | 0.0293 (3) | −0.2436 (3) | 0.42433 (18) | 0.0153 (4) | |
| C3A | −0.0976 (3) | −0.3688 (3) | 0.36264 (18) | 0.0172 (4) | |
| H3A | −0.1715 | −0.4265 | 0.3963 | 0.021* | |
| C4A | −0.1132 (3) | −0.4064 (3) | 0.25341 (18) | 0.0165 (4) | |
| C5A | −0.0028 (3) | −0.3491 (3) | 0.09277 (18) | 0.0191 (4) | |
| H5A | −0.0859 | −0.4295 | 0.0451 | 0.023* | |
| C6A | 0.1133 (3) | −0.2621 (3) | 0.05366 (19) | 0.0204 (5) | |
| H6A | 0.1111 | −0.2840 | −0.0207 | 0.024* | |
| C7A | 0.2367 (3) | −0.1399 (3) | 0.12198 (19) | 0.0200 (5) | |
| H7A | 0.3155 | −0.0795 | 0.0932 | 0.024* | |
| C8A | 0.2426 (3) | −0.1086 (3) | 0.22991 (19) | 0.0178 (4) | |
| H8A | 0.3256 | −0.0265 | 0.2759 | 0.021* | |
| C9A | 0.1252 (3) | −0.1986 (2) | 0.27237 (18) | 0.0150 (4) | |
| C10A | −0.0005 (3) | −0.3205 (3) | 0.20414 (18) | 0.0158 (4) | |
| C11A | −0.2508 (3) | −0.5363 (3) | 0.18690 (19) | 0.0190 (4) | |
| O11A | −0.3182 (2) | −0.5417 (2) | 0.09388 (14) | 0.0281 (4) | |
| O12A | −0.28999 (19) | −0.64555 (19) | 0.24393 (14) | 0.0212 (3) | |
| C12A | −0.4228 (3) | −0.7757 (3) | 0.1849 (2) | 0.0245 (5) | |
| H12D | −0.5155 | −0.7399 | 0.1519 | 0.037* | |
| H12E | −0.4536 | −0.8435 | 0.2349 | 0.037* | |
| H12F | −0.3887 | −0.8313 | 0.1283 | 0.037* | |
| N1B | 0.1763 (2) | −0.0732 (2) | 0.58953 (15) | 0.0144 (3) | |
| C2B | 0.0491 (2) | −0.1915 (3) | 0.54192 (17) | 0.0140 (4) | |
| C3B | −0.0588 (3) | −0.2629 (3) | 0.59879 (18) | 0.0154 (4) | |
| H3B | −0.1447 | −0.3501 | 0.5632 | 0.019* | |
| C4B | −0.0395 (3) | −0.2061 (3) | 0.70607 (18) | 0.0155 (4) | |
| C5B | 0.1212 (3) | −0.0045 (3) | 0.86815 (18) | 0.0169 (4) | |
| H5B | 0.0512 | −0.0429 | 0.9113 | 0.020* | |
| C6B | 0.2517 (3) | 0.1184 (3) | 0.91204 (18) | 0.0193 (4) | |
| H6B | 0.2709 | 0.1642 | 0.9854 | 0.023* | |
| C7B | 0.3583 (3) | 0.1782 (3) | 0.85011 (19) | 0.0188 (4) | |
| H7B | 0.4489 | 0.2630 | 0.8821 | 0.023* | |
| C8B | 0.3309 (3) | 0.1139 (3) | 0.74412 (18) | 0.0176 (4) | |
| H8B | 0.4023 | 0.1548 | 0.7025 | 0.021* | |
| C9B | 0.1967 (3) | −0.0135 (3) | 0.69604 (18) | 0.0153 (4) | |
| C10B | 0.0894 (3) | −0.0752 (2) | 0.75828 (17) | 0.0145 (4) | |
| C11B | −0.1583 (3) | −0.2831 (3) | 0.76375 (18) | 0.0163 (4) | |
| O11B | −0.1970 (2) | −0.2197 (2) | 0.83756 (14) | 0.0220 (4) | |
| O12B | −0.2166 (2) | −0.43175 (19) | 0.72286 (14) | 0.0210 (3) | |
| C12B | −0.3430 (3) | −0.5141 (3) | 0.7667 (2) | 0.0241 (5) | |
| H12A | −0.3126 | −0.4851 | 0.8456 | 0.036* | |
| H12B | −0.3575 | −0.6240 | 0.7470 | 0.036* | |
| H12C | −0.4443 | −0.4890 | 0.7371 | 0.036* |
| Cu1 | 0.01350 (13) | 0.01802 (14) | 0.01445 (13) | −0.00091 (10) | 0.00308 (10) | 0.00031 (10) |
| I1 | 0.01682 (7) | 0.01604 (7) | 0.01965 (8) | 0.00169 (5) | 0.00320 (5) | 0.00222 (5) |
| N1A | 0.0140 (8) | 0.0151 (9) | 0.0116 (8) | 0.0030 (7) | 0.0011 (7) | 0.0007 (7) |
| C2A | 0.0139 (9) | 0.0167 (10) | 0.0136 (10) | 0.0032 (8) | 0.0028 (8) | −0.0001 (8) |
| C3A | 0.0139 (10) | 0.0188 (11) | 0.0161 (10) | 0.0003 (8) | 0.0029 (8) | 0.0020 (8) |
| C4A | 0.0170 (10) | 0.0145 (10) | 0.0150 (10) | 0.0019 (8) | 0.0020 (8) | −0.0011 (8) |
| C5A | 0.0216 (11) | 0.0190 (11) | 0.0140 (10) | 0.0038 (9) | 0.0028 (8) | −0.0011 (8) |
| C6A | 0.0274 (12) | 0.0200 (11) | 0.0122 (10) | 0.0059 (9) | 0.0039 (9) | −0.0006 (8) |
| C7A | 0.0227 (11) | 0.0205 (11) | 0.0170 (10) | 0.0040 (9) | 0.0063 (9) | 0.0051 (9) |
| C8A | 0.0173 (10) | 0.0180 (11) | 0.0160 (10) | 0.0026 (8) | 0.0023 (8) | 0.0027 (8) |
| C9A | 0.0145 (9) | 0.0146 (10) | 0.0142 (10) | 0.0028 (8) | 0.0018 (8) | 0.0016 (8) |
| C10A | 0.0150 (10) | 0.0160 (10) | 0.0140 (10) | 0.0031 (8) | 0.0009 (8) | −0.0001 (8) |
| C11A | 0.0157 (10) | 0.0198 (11) | 0.0186 (11) | 0.0011 (8) | 0.0053 (8) | −0.0024 (9) |
| O11A | 0.0260 (9) | 0.0315 (10) | 0.0161 (8) | −0.0037 (8) | −0.0016 (7) | −0.0013 (7) |
| O12A | 0.0164 (8) | 0.0178 (8) | 0.0224 (8) | −0.0030 (6) | 0.0000 (6) | 0.0000 (7) |
| C12A | 0.0162 (11) | 0.0184 (11) | 0.0312 (13) | −0.0030 (9) | 0.0012 (10) | −0.0017 (10) |
| N1B | 0.0129 (8) | 0.0160 (9) | 0.0123 (8) | 0.0013 (7) | 0.0024 (7) | 0.0008 (7) |
| C2B | 0.0121 (9) | 0.0148 (10) | 0.0124 (9) | 0.0012 (7) | 0.0013 (7) | 0.0002 (8) |
| C3B | 0.0118 (9) | 0.0170 (10) | 0.0151 (10) | 0.0016 (8) | 0.0012 (8) | 0.0016 (8) |
| C4B | 0.0129 (9) | 0.0173 (10) | 0.0158 (10) | 0.0034 (8) | 0.0039 (8) | 0.0021 (8) |
| C5B | 0.0176 (10) | 0.0192 (11) | 0.0138 (10) | 0.0056 (8) | 0.0036 (8) | 0.0022 (8) |
| C6B | 0.0220 (11) | 0.0211 (11) | 0.0124 (10) | 0.0053 (9) | 0.0024 (8) | −0.0020 (8) |
| C7B | 0.0175 (10) | 0.0162 (10) | 0.0180 (10) | 0.0004 (8) | 0.0018 (8) | −0.0021 (8) |
| C8B | 0.0167 (10) | 0.0181 (11) | 0.0157 (10) | 0.0007 (8) | 0.0047 (8) | 0.0005 (8) |
| C9B | 0.0141 (9) | 0.0168 (10) | 0.0142 (10) | 0.0042 (8) | 0.0023 (8) | 0.0011 (8) |
| C10B | 0.0142 (9) | 0.0157 (10) | 0.0135 (10) | 0.0042 (8) | 0.0030 (8) | 0.0021 (8) |
| C11B | 0.0145 (9) | 0.0182 (10) | 0.0149 (10) | 0.0035 (8) | 0.0017 (8) | 0.0036 (8) |
| O11B | 0.0212 (8) | 0.0233 (9) | 0.0191 (8) | 0.0007 (7) | 0.0085 (7) | −0.0016 (7) |
| O12B | 0.0214 (8) | 0.0167 (8) | 0.0250 (9) | 0.0013 (6) | 0.0110 (7) | 0.0025 (7) |
| C12B | 0.0244 (12) | 0.0179 (11) | 0.0299 (13) | 0.0001 (9) | 0.0132 (10) | 0.0042 (10) |
| Cu1—N1A | 2.088 (2) | C12A—H12D | 0.9800 |
| Cu1—N1B | 2.092 (2) | C12A—H12E | 0.9800 |
| Cu1—I1 | 2.5473 (10) | C12A—H12F | 0.9800 |
| Cu1—I1i | 2.6996 (9) | N1B—C2B | 1.336 (3) |
| Cu1—Cu1i | 2.6723 (11) | N1B—C9B | 1.373 (3) |
| I1—Cu1i | 2.6997 (9) | C2B—C3B | 1.408 (3) |
| N1A—C2A | 1.325 (3) | C3B—C4B | 1.377 (3) |
| N1A—C9A | 1.377 (3) | C3B—H3B | 0.9500 |
| C2A—C3A | 1.414 (3) | C4B—C10B | 1.422 (3) |
| C2A—C2B | 1.493 (3) | C4B—C11B | 1.500 (3) |
| C3A—C4A | 1.377 (3) | C5B—C6B | 1.368 (3) |
| C3A—H3A | 0.9500 | C5B—C10B | 1.425 (3) |
| C4A—C10A | 1.423 (3) | C5B—H5B | 0.9500 |
| C4A—C11A | 1.502 (3) | C6B—C7B | 1.413 (3) |
| C5A—C6A | 1.366 (3) | C6B—H6B | 0.9500 |
| C5A—C10A | 1.421 (3) | C7B—C8B | 1.368 (3) |
| C5A—H5A | 0.9500 | C7B—H7B | 0.9500 |
| C6A—C7A | 1.412 (3) | C8B—C9B | 1.419 (3) |
| C6A—H6A | 0.9500 | C8B—H8B | 0.9500 |
| C7A—C8A | 1.372 (3) | C9B—C10B | 1.426 (3) |
| C7A—H7A | 0.9500 | C11B—O11B | 1.208 (3) |
| C8A—C9A | 1.412 (3) | C11B—O12B | 1.336 (3) |
| C8A—H8A | 0.9500 | O12B—C12B | 1.448 (3) |
| C9A—C10A | 1.420 (3) | C12B—H12A | 0.9800 |
| C11A—O11A | 1.205 (3) | C12B—H12B | 0.9800 |
| C11A—O12A | 1.332 (3) | C12B—H12C | 0.9800 |
| O12A—C12A | 1.455 (3) | ||
| N1A—Cu1—N1B | 78.10 (8) | O12A—C12A—H12F | 109.5 |
| N1A—Cu1—I1 | 124.55 (6) | H12D—C12A—H12F | 109.5 |
| N1B—Cu1—I1 | 125.61 (6) | H12E—C12A—H12F | 109.5 |
| N1A—Cu1—I1i | 96.95 (6) | C2B—N1B—C9B | 118.65 (19) |
| N1B—Cu1—I1i | 103.46 (6) | C2B—N1B—Cu1 | 113.28 (14) |
| I1—Cu1—I1i | 118.85 (3) | C9B—N1B—Cu1 | 127.25 (15) |
| Cu1—I1—Cu1i | 61.15 (3) | N1B—C2B—C3B | 122.3 (2) |
| C2A—N1A—C9A | 119.28 (19) | N1B—C2B—C2A | 115.52 (19) |
| C2A—N1A—Cu1 | 113.75 (15) | C3B—C2B—C2A | 122.14 (19) |
| C9A—N1A—Cu1 | 125.41 (15) | C4B—C3B—C2B | 119.9 (2) |
| N1A—C2A—C3A | 122.3 (2) | C4B—C3B—H3B | 120.1 |
| N1A—C2A—C2B | 115.21 (19) | C2B—C3B—H3B | 120.1 |
| C3A—C2A—C2B | 122.5 (2) | C3B—C4B—C10B | 119.5 (2) |
| C4A—C3A—C2A | 119.4 (2) | C3B—C4B—C11B | 118.5 (2) |
| C4A—C3A—H3A | 120.3 | C10B—C4B—C11B | 121.9 (2) |
| C2A—C3A—H3A | 120.3 | C6B—C5B—C10B | 120.6 (2) |
| C3A—C4A—C10A | 119.8 (2) | C6B—C5B—H5B | 119.7 |
| C3A—C4A—C11A | 119.7 (2) | C10B—C5B—H5B | 119.7 |
| C10A—C4A—C11A | 120.5 (2) | C5B—C6B—C7B | 121.1 (2) |
| C6A—C5A—C10A | 120.6 (2) | C5B—C6B—H6B | 119.4 |
| C6A—C5A—H5A | 119.7 | C7B—C6B—H6B | 119.4 |
| C10A—C5A—H5A | 119.7 | C8B—C7B—C6B | 119.9 (2) |
| C5A—C6A—C7A | 121.1 (2) | C8B—C7B—H7B | 120.0 |
| C5A—C6A—H6A | 119.5 | C6B—C7B—H7B | 120.0 |
| C7A—C6A—H6A | 119.5 | C7B—C8B—C9B | 120.4 (2) |
| C8A—C7A—C6A | 120.0 (2) | C7B—C8B—H8B | 119.8 |
| C8A—C7A—H7A | 120.0 | C9B—C8B—H8B | 119.8 |
| C6A—C7A—H7A | 120.0 | N1B—C9B—C8B | 117.5 (2) |
| C7A—C8A—C9A | 119.8 (2) | N1B—C9B—C10B | 122.5 (2) |
| C7A—C8A—H8A | 120.1 | C8B—C9B—C10B | 120.0 (2) |
| C9A—C8A—H8A | 120.1 | C4B—C10B—C5B | 125.0 (2) |
| N1A—C9A—C8A | 117.3 (2) | C4B—C10B—C9B | 117.0 (2) |
| N1A—C9A—C10A | 122.1 (2) | C5B—C10B—C9B | 118.0 (2) |
| C8A—C9A—C10A | 120.6 (2) | O11B—C11B—O12B | 124.0 (2) |
| C9A—C10A—C5A | 117.9 (2) | O11B—C11B—C4B | 124.8 (2) |
| C9A—C10A—C4A | 117.1 (2) | O12B—C11B—C4B | 111.19 (19) |
| C5A—C10A—C4A | 125.0 (2) | C11B—O12B—C12B | 115.55 (18) |
| O11A—C11A—O12A | 123.9 (2) | O12B—C12B—H12A | 109.5 |
| O11A—C11A—C4A | 124.7 (2) | O12B—C12B—H12B | 109.5 |
| O12A—C11A—C4A | 111.4 (2) | H12A—C12B—H12B | 109.5 |
| C11A—O12A—C12A | 114.73 (19) | O12B—C12B—H12C | 109.5 |
| O12A—C12A—H12D | 109.5 | H12A—C12B—H12C | 109.5 |
| O12A—C12A—H12E | 109.5 | H12B—C12B—H12C | 109.5 |
| H12D—C12A—H12E | 109.5 | ||
| N1A—Cu1—I1—Cu1i | −123.16 (7) | I1—Cu1—N1B—C2B | 140.88 (14) |
| N1B—Cu1—I1—Cu1i | 136.17 (7) | I1i—Cu1—N1B—C2B | −77.71 (15) |
| I1i—Cu1—I1—Cu1i | 0.0 | N1A—Cu1—N1B—C9B | −173.9 (2) |
| N1B—Cu1—N1A—C2A | −17.89 (15) | I1—Cu1—N1B—C9B | −49.7 (2) |
| I1—Cu1—N1A—C2A | −143.16 (14) | I1i—Cu1—N1B—C9B | 91.69 (18) |
| I1i—Cu1—N1A—C2A | 84.46 (15) | C9B—N1B—C2B—C3B | −4.1 (3) |
| N1B—Cu1—N1A—C9A | 176.59 (19) | Cu1—N1B—C2B—C3B | 166.34 (17) |
| I1—Cu1—N1A—C9A | 51.33 (19) | C9B—N1B—C2B—C2A | 176.24 (19) |
| I1i—Cu1—N1A—C9A | −81.05 (18) | Cu1—N1B—C2B—C2A | −13.4 (2) |
| C9A—N1A—C2A—C3A | 1.9 (3) | N1A—C2A—C2B—N1B | −1.9 (3) |
| Cu1—N1A—C2A—C3A | −164.62 (17) | C3A—C2A—C2B—N1B | 179.0 (2) |
| C9A—N1A—C2A—C2B | −177.27 (19) | N1A—C2A—C2B—C3B | 178.4 (2) |
| Cu1—N1A—C2A—C2B | 16.2 (2) | C3A—C2A—C2B—C3B | −0.7 (3) |
| N1A—C2A—C3A—C4A | −2.1 (3) | N1B—C2B—C3B—C4B | 3.3 (3) |
| C2B—C2A—C3A—C4A | 177.0 (2) | C2A—C2B—C3B—C4B | −177.0 (2) |
| C2A—C3A—C4A—C10A | 0.9 (3) | C2B—C3B—C4B—C10B | 0.2 (3) |
| C2A—C3A—C4A—C11A | −178.1 (2) | C2B—C3B—C4B—C11B | 178.9 (2) |
| C10A—C5A—C6A—C7A | −1.2 (4) | C10B—C5B—C6B—C7B | −0.1 (4) |
| C5A—C6A—C7A—C8A | 1.0 (4) | C5B—C6B—C7B—C8B | 0.6 (4) |
| C6A—C7A—C8A—C9A | 0.0 (3) | C6B—C7B—C8B—C9B | −0.5 (4) |
| C2A—N1A—C9A—C8A | 179.3 (2) | C2B—N1B—C9B—C8B | −178.8 (2) |
| Cu1—N1A—C9A—C8A | −15.9 (3) | Cu1—N1B—C9B—C8B | 12.3 (3) |
| C2A—N1A—C9A—C10A | −0.5 (3) | C2B—N1B—C9B—C10B | 1.5 (3) |
| Cu1—N1A—C9A—C10A | 164.31 (16) | Cu1—N1B—C9B—C10B | −167.44 (16) |
| C7A—C8A—C9A—N1A | 179.4 (2) | C7B—C8B—C9B—N1B | −179.7 (2) |
| C7A—C8A—C9A—C10A | −0.8 (3) | C7B—C8B—C9B—C10B | 0.0 (3) |
| N1A—C9A—C10A—C5A | −179.6 (2) | C3B—C4B—C10B—C5B | 179.2 (2) |
| C8A—C9A—C10A—C5A | 0.6 (3) | C11B—C4B—C10B—C5B | 0.6 (3) |
| N1A—C9A—C10A—C4A | −0.6 (3) | C3B—C4B—C10B—C9B | −2.6 (3) |
| C8A—C9A—C10A—C4A | 179.5 (2) | C11B—C4B—C10B—C9B | 178.8 (2) |
| C6A—C5A—C10A—C9A | 0.4 (3) | C6B—C5B—C10B—C4B | 177.8 (2) |
| C6A—C5A—C10A—C4A | −178.5 (2) | C6B—C5B—C10B—C9B | −0.4 (3) |
| C3A—C4A—C10A—C9A | 0.4 (3) | N1B—C9B—C10B—C4B | 1.8 (3) |
| C11A—C4A—C10A—C9A | 179.4 (2) | C8B—C9B—C10B—C4B | −177.9 (2) |
| C3A—C4A—C10A—C5A | 179.3 (2) | N1B—C9B—C10B—C5B | −179.8 (2) |
| C11A—C4A—C10A—C5A | −1.7 (3) | C8B—C9B—C10B—C5B | 0.4 (3) |
| C3A—C4A—C11A—O11A | 146.9 (3) | C3B—C4B—C11B—O11B | −149.8 (2) |
| C10A—C4A—C11A—O11A | −32.1 (4) | C10B—C4B—C11B—O11B | 28.8 (3) |
| C3A—C4A—C11A—O12A | −32.9 (3) | C3B—C4B—C11B—O12B | 30.2 (3) |
| C10A—C4A—C11A—O12A | 148.1 (2) | C10B—C4B—C11B—O12B | −151.2 (2) |
| O11A—C11A—O12A—C12A | 0.2 (3) | O11B—C11B—O12B—C12B | 5.1 (3) |
| C4A—C11A—O12A—C12A | 179.96 (18) | C4B—C11B—O12B—C12B | −174.87 (19) |
| N1A—Cu1—N1B—C2B | 16.69 (15) |
Selected bond lengths (Å)
| Cu1—N1 | 2.088 (2) |
| Cu1—N1 | 2.092 (2) |
| Cu1—I1 | 2.5473 (10) |
| Cu1—I1i | 2.6996 (9) |
Symmetry code: (i) .