research communications
accessof a copper complex containing the 4-bromo-2-{[(2-hydroxyethyl)imino]methyl}phenol base Schiff ligand
aDépartement de Chimie, Faculté des Sciences et Techniques, Université Cheik Anta Diop, Dakar, Senegal, bDepartment of Chemical Sciences, Life Science and Environmental Sustainability, University of Parma, Parco Area delle Scienze 17/A, 43124 Parma, Italy, and cBiopharmanet-TEC, University of Parma, Parco Area Delle Scienze 27/A, Parma 43124, Italy
*Correspondence e-mail: [email protected]
The coordination (4-bromo-2-{[(2-hydroxyethyl)imino]methyl}phenololato-κ3O,N,O′)(thiocyanato-κN)copper(II)–5-bromo-2-hydroxybenzaldehyde–water (2/1/1), [Cu(C9H9BrNO2)(NCS)]·0.5C7H5BrO2·0.5H2O or [Cu(HL)(SCN)]2·C7H5BrO2·H2O, crystallizes in the monoclinic space group P21/c. The asymmetric unit contains two mononuclear units of the complex, each consisting of one deprotonated ligand, one thiocyanate anion (SCN−) coordinated through its nitrogen atom, one free water molecule, and one free 5-bromosalicylaldehyde molecule, forming a co-crystal. The copper atom is four-coordinate, adopting a slightly distorted square-planar geometry defined by the tridentate ligand and the nitrogen atom of the thiocyanate anion. Bond length values show that the thiocyanate ion has a linear S—C≡N arrangement, typical of a terminal, N-bound isothiocyanate group. The water molecule plays a key role in linking the two complex units through O—H⋯O hydrogen bonds. In the crystal, C—H⋯O and C—H⋯Br hydrogen bonds allow the free 5-bromosalicylaldehyde molecule to form a bridge between two adjacent layers. Additional O—H⋯O, C—H⋯S, O—H⋯S, and C—H⋯N interactions further consolidate the overall structure.
Keywords: crystal structure; co-crystal; coordination polymer complex; copper(II).
CCDC reference: 2588876
1. Chemical context
The use of salicylaldehyde-derived ligands in the synthesis of coordination complexes has become increasingly important and represents a frequent research topic, particularly in copper-catalysed reactions (Juyal et al., 2023
). Indeed, these ligands contain donor sites such as the phenolic oxygen atom and the imine nitrogen atom, enabling the formation of stable complexes with various geometries, notably polynuclear copper(II) complexes.
Numerous applications have been reported, including in catalysis (Shelar et al., 2021
), materials science (Abu-Dief & Mohamed, 2015
), and medicine (More et al., 2019
). The formation of a co-crystal associated with a polynuclear copper complex represents an important aspect of supramolecular chemistry, as such systems are stabilized by networks of non-covalent interactions, including hydrogen bonds (Benito et al., 2025
).
In the field of crystal engineering, co-crystals defined as single-phase crystalline materials comprising two or more neutral molecular species have long been exploited to tune physicochemical attributes while preserving the molecular identity of active components (Taylor & Day, 2018
). We have synthesized a tridentate Schiff base ligand, (E)-4-bromo-2-{[(2-hydroxyethyl)imino]methyl}phenol, derived from salicylaldehyde, which forms a polynuclear complex with copper(II) chloride and potassium thiocyanate.
2. Structural commentary
The title compound (Fig. 1
) crystallizes in the monoclinic system, space group P21/c. The asymmetric unit, [Cu(HL)(SCN)]2(C7H5BrO2)·H2O, contains two monodeprotonated ligand molecules, two independent copper(II) ions, two monodentate thiocyanate anions, one co-crystallized bromo-hydroxybenzaldehyde molecule and one free water molecule.
| Figure 1 The molecular structure of the title compound showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. |
The Schiff base ligand acts in a tridentate fashion through the phenolate oxygen atom, the azomethine nitrogen atom, and the alcoholic oxygen atom, resulting in one five-membered (CuOCCN) and one six-membered (CuOCCCN) chelate ring around each CuII ion.
Each copper atom is four-coordinate, bound by an N2O2 donor set comprising one azomethine (imine) nitrogen and two oxygen atoms (one phenolate, one alcoholic) from the Schiff base ligand, together with one nitrogen atom from its own thiocyanate group, forming an essentially square-planar, moderately distorted coordination plane. The bond lengths within this square plane are Cu1—O1 = 1.911 (2) Å, Cu1—N1 = 1.928 (3) Å, Cu1—N3 = 1.952 (3) Å, and Cu1—O2 = 2.038 (2) Å. For the corresponding values for Cu2, see Table 1
).
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A single, additional axial contact to the nitrogen atom of the thiocyanate group of the neighbouring mononuclear unit is present at each copper centre, but this contact is long and markedly asymmetric between the two independent centres [2.961 (3) Å for Cu1 versus 3.100 (3) Å for Cu2]. The latter value exceeds the sum of the van der Waals radii for Cu⋯N and cannot reasonably be described as a coordination bond. The geometry is therefore described as distorted square-planar (four-coordinate, N2O2), with a weak, asymmetric secondary axial contact of semi-coordinate character, rather than as distorted square-planar.
It is this weak, asymmetric N⋯Cu axial contact, not a Cu—S bond, that links each mononuclear [Cu(HL)(SCN)] unit to its neighbour and propagates the one-dimensional polymeric chain.
The deviations of the angles from the ideal value of 90° [O1—Cu1—N1 = 93.58 (10)°, O2—Cu1—N3 = 89.45 (11)°, N1—Cu1—O2 = 82.51 (10)°, and O1—Cu1—N3 = 94.69 (11)°] confirm the distortion of the coordination geometry.
The Cu1> ion is displaced from the least-squares plane defined by O1, N1, O2 and N3 (r.m.s. deviation 0.117 Å) by 0.006 (12) Å, indicating that the metal centre lies essentially within the equatorial plane. The dihedral angle of 175.63 (17)° between the phenolate ring plane (O1/C1–C6) and the plane of the open-chain fragment (C7/N1/C8/C9/O2) reveals a slight but measurable deviation from planarity, indicative of a twist in the ligand backbone.
The Cu1⋯Cu2 separation between two adjacent units is 3.7765 (5) Å, a distance too long to invoke any meaningful metal–metal interaction. The cis angles span the range 82.51 (10)–94.69 (11)°, in good agreement with values reported for related complexes. The trans angles O1—Cu1—O2 = 166.82 (10)° and N3—Cu1—N1 = 171.73 (12)° deviate significantly from the ideal value of 180°, further confirming that Cu1 resides in a severely distorted square-planar coordination environment. The environment about Cu2 is similar, see Table 1
).
The bond lengths within the two thiocyanate groups are S1—C19 = 1.629 (3) Å, C19—N3 = 1.153 (4) Å, and S2—C20 = 1.643 (4) Å, C20—N4 = 1.106 (4) Å. These values are consistent with the linear S—C≡N arrangement typical of a terminal, N-bound isothiocyanate group.
The sulfur atoms S1 and S2 are not bonded to any copper atom. The bridging mode is therefore not the classical μ-1,3 (S,N) mode frequently found in Cu–SCN polymers, but an asymmetric end-on μ-1,1 (N,N′) bridge, in which each thiocyanate nitrogen atom is strongly bonded to its own copper centre and forms a second, much weaker, semi-coordinate contact with the neighbouring copper centre, as summarized below.
3. Supramolecular features
We note four strong interactions of the O—H—O type (Table 2
). The water molecule connects unit Cu2 via O4—H4⋯O7 to unit Cu1 via O7—H7A··O1. The O2—H2⋯O3 hydrogen bond similarly connects the two units. The O5—H5A⋯O6 interaction corresponds to the classical intramolecular hydrogen bond within the co-crystallized aldehyde fragment, confirming its nature as an isolated unit maintained in the network mainly by the weak C—H⋯·Br, C—H⋯S, C—H⋯N and C—H⋯O contacts and extending the three-dimensional network and further enhances the cohesion of the structure. The packing is shown in Fig. 2
.
|
| Figure 2 Partial packing diagram for the title compound along [001]. |
4. Database survey
A search of the Cambridge Structural Database (CSD version 5.46, updates of November 2024 and February 2025; Groom et al., 2016) yielded 25 hits containing crystal structures of coordination complexes bearing the 4-bromo-2-{[(2-hydroxyethyl)imino]methyl}phenol ligand. The first result corresponds to the structure of the free ligand reported by Thakur et al. 2024
(refcode YAWNOB01). 23 of the remaining hits correspond to coordination complexes of first-row transition metals. Only one second-row transition metal complex is noted, namely a cadmium complex (AWOHIE; Yu et al., 2011
). Half of the hits correspond to mononuclear complexes in which two molecules of the tridentate ligand chelate the metal ion including refcodes BAVGUD, BAVROI (Abbasi et al., 2017
); HEDKUX (Liang et al., 2006
); HEDKUX01 (Chumakov et al., 2007
); HEDKUX02 (Zabierowski et al., 2013
); MIWSEQ (De et al., 2001
), among others. Polynuclear complexes are also reported, including a dinuclear copper complex (FOQKAY; Thakurta et al., 2009a
,b
), a tetranuclear copper complex (LICWAW; Yoshida et al.), and a tetranuclear iron complex (EBUWII; Oshio et al., 2004
).
5. Synthesis and crystallization
The Schiff base ligand HL was prepared by adding 2.5 g (13.5 mmol) of 5-bromosalicylaldehyde and 0.8 g (13.5 mmol) of 2-aminoethanol, along with a few drops of glacial acetic acid, to 20 mL of ethanol in a flask. The mixture was refluxed, then evaporated to dryness using a rotary evaporator, giving a light-brown oil in 80% yield. This oil was dissolved in ethanol (100 mL) to give a 0.108 mol l−1 ligand solution.
For the complex synthesis, 0.17 g (1 mmol) of copper(II) chloride dihydrate and 0.19 g (2 mmol) of potassium thiocyanate were dissolved in 10 mL of methanol and stirred under reflux for 30 minutes, giving a brown solution. Then, 9.2 mL of the ligand solution was added dropwise to the metal solution. After refluxing for 1 h, a green precipitate formed, which was filtered, washed with methanol, and dried, giving 0.14 g of product. Green single crystals suitable for X-ray diffraction were obtained after two weeks.
6. Refinement
Crystal data, data collection and structure details are summarized in Table 3
. H atoms were positioned geometrically and refined as riding with Uiso(H) = 1.2Ueq(C).
|
Supporting information
CCDC reference: 2588876
contains datablock I. DOI: https://doi.org/10.1107/S2056989026009746/ex2102sup1.cif
Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989026009746/ex2102Isup2.hkl
| [Cu(C9H9BrNO2)(NCS)]·0.5C7H5BrO2·0.5H2O | F(000) = 1864 |
| Mr = 948.44 | Dx = 1.873 Mg m−3 |
| Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
| a = 18.4400 (5) Å | Cell parameters from 60122 reflections |
| b = 13.7346 (3) Å | θ = 1.9–26.4° |
| c = 13.6402 (3) Å | µ = 5.00 mm−1 |
| β = 103.136 (1)° | T = 296 K |
| V = 3364.20 (14) Å3 | Prism, green |
| Z = 4 | 0.2 × 0.2 × 0.2 mm |
| Bruker D8 Venture Equipped with PhotonII Detector diffractometer | 5316 reflections with I > 2σ(I) |
| profile data from ω–scans | Rint = 0.070 |
| Absorption correction: multi-scan (SADABS; Krause et al., 2015) | θmax = 26.4°, θmin = 1.9° |
| h = −23→23 | |
| 60122 measured reflections | k = −17→17 |
| 6909 independent reflections | l = −17→15 |
| Refinement on F2 | 0 restraints |
| Least-squares matrix: full | Hydrogen site location: mixed |
| R[F2 > 2σ(F2)] = 0.034 | H-atom parameters constrained |
| wR(F2) = 0.081 | w = 1/[σ2(Fo2) + (0.0255P)2 + 4.7568P] where P = (Fo2 + 2Fc2)/3 |
| S = 1.01 | (Δ/σ)max = 0.001 |
| 6909 reflections | Δρmax = 0.62 e Å−3 |
| 412 parameters | Δρmin = −0.61 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
| x | y | z | Uiso*/Ueq | ||
| Cu2 | 0.35837 (2) | 0.72579 (3) | 0.41858 (3) | 0.03257 (10) | |
| Cu1 | 0.52874 (2) | 0.71541 (3) | 0.30893 (3) | 0.03342 (10) | |
| Br3 | −0.17062 (2) | 0.47243 (3) | 0.42161 (4) | 0.06458 (14) | |
| Br1 | 0.88193 (3) | 0.96575 (4) | 0.53387 (5) | 0.07697 (16) | |
| Br2 | 0.11977 (3) | 0.30742 (4) | 0.22273 (4) | 0.08438 (19) | |
| S1 | 0.29927 (5) | 0.78586 (7) | 0.09224 (7) | 0.0424 (2) | |
| S2 | 0.58322 (6) | 0.80940 (7) | 0.62694 (8) | 0.0485 (2) | |
| O3 | 0.36588 (12) | 0.59043 (15) | 0.38633 (18) | 0.0365 (5) | |
| O4 | 0.35052 (13) | 0.87140 (16) | 0.41724 (18) | 0.0386 (5) | |
| H4 | 0.388208 | 0.901725 | 0.414008 | 0.058* | |
| O1 | 0.56911 (13) | 0.84305 (15) | 0.33838 (18) | 0.0376 (5) | |
| O2 | 0.48631 (13) | 0.57876 (16) | 0.31199 (19) | 0.0399 (6) | |
| H2 | 0.446357 | 0.578002 | 0.328833 | 0.060* | |
| N4 | 0.46559 (16) | 0.73030 (19) | 0.4895 (2) | 0.0353 (6) | |
| N1 | 0.61991 (15) | 0.65156 (18) | 0.3749 (2) | 0.0340 (6) | |
| N2 | 0.25666 (15) | 0.7357 (2) | 0.3433 (2) | 0.0338 (6) | |
| N3 | 0.43073 (16) | 0.7612 (2) | 0.2376 (2) | 0.0397 (7) | |
| O7 | 0.46760 (17) | 0.96055 (19) | 0.3943 (3) | 0.0702 (10) | |
| H7A | 0.502551 | 0.934333 | 0.372361 | 0.105* | |
| H7B | 0.481742 | 1.019032 | 0.407084 | 0.105* | |
| O5 | 0.0839 (2) | 0.7473 (3) | 0.4295 (3) | 0.0837 (11) | |
| H5A | 0.093367 | 0.779032 | 0.481825 | 0.126* | |
| C19 | 0.37653 (18) | 0.7704 (2) | 0.1765 (2) | 0.0305 (7) | |
| C1 | 0.63814 (19) | 0.8652 (2) | 0.3819 (2) | 0.0336 (7) | |
| C6 | 0.69389 (18) | 0.7959 (2) | 0.4217 (2) | 0.0339 (7) | |
| C7 | 0.68112 (18) | 0.6930 (2) | 0.4166 (3) | 0.0354 (7) | |
| H7 | 0.720737 | 0.653006 | 0.446251 | 0.042* | |
| C10 | 0.30904 (19) | 0.5317 (2) | 0.3505 (2) | 0.0345 (7) | |
| C18 | 0.2894 (2) | 0.9050 (2) | 0.3404 (3) | 0.0412 (8) | |
| H18A | 0.302755 | 0.905842 | 0.275613 | 0.049* | |
| H18B | 0.275062 | 0.970303 | 0.355478 | 0.049* | |
| C17 | 0.2264 (2) | 0.8346 (2) | 0.3389 (3) | 0.0424 (8) | |
| H17A | 0.204564 | 0.846199 | 0.396192 | 0.051* | |
| H17B | 0.188028 | 0.843103 | 0.277853 | 0.051* | |
| O6 | 0.0669 (2) | 0.8034 (3) | 0.6092 (3) | 0.0965 (12) | |
| C15 | 0.23619 (19) | 0.5640 (3) | 0.3092 (3) | 0.0376 (8) | |
| C16 | 0.21500 (19) | 0.6653 (3) | 0.3038 (3) | 0.0385 (8) | |
| H16 | 0.166982 | 0.680496 | 0.268639 | 0.046* | |
| C2 | 0.6592 (2) | 0.9643 (2) | 0.3897 (3) | 0.0399 (8) | |
| H2A | 0.623644 | 1.011294 | 0.363949 | 0.048* | |
| C20 | 0.5114 (2) | 0.7642 (2) | 0.5457 (3) | 0.0385 (8) | |
| C5 | 0.7662 (2) | 0.8277 (3) | 0.4681 (3) | 0.0426 (8) | |
| H5 | 0.802604 | 0.782312 | 0.495451 | 0.051* | |
| C9 | 0.5384 (2) | 0.5164 (3) | 0.3777 (3) | 0.0470 (9) | |
| H9A | 0.528637 | 0.448840 | 0.358511 | 0.056* | |
| H9B | 0.533871 | 0.524355 | 0.446689 | 0.056* | |
| C11 | 0.3229 (2) | 0.4310 (3) | 0.3530 (3) | 0.0450 (9) | |
| H11 | 0.370795 | 0.408127 | 0.379841 | 0.054* | |
| C8 | 0.6145 (2) | 0.5446 (2) | 0.3682 (3) | 0.0452 (9) | |
| H8A | 0.651666 | 0.515002 | 0.421687 | 0.054* | |
| H8B | 0.622919 | 0.522553 | 0.304106 | 0.054* | |
| C3 | 0.7297 (2) | 0.9935 (3) | 0.4337 (3) | 0.0446 (9) | |
| H3 | 0.741978 | 1.059317 | 0.437188 | 0.054* | |
| C4 | 0.7831 (2) | 0.9240 (3) | 0.4734 (3) | 0.0461 (9) | |
| C14 | 0.1799 (2) | 0.4965 (3) | 0.2705 (3) | 0.0495 (10) | |
| H14 | 0.131914 | 0.517809 | 0.241540 | 0.059* | |
| C24 | −0.0898 (2) | 0.5597 (3) | 0.4264 (3) | 0.0462 (9) | |
| C13 | 0.1959 (2) | 0.3992 (3) | 0.2754 (3) | 0.0521 (10) | |
| C12 | 0.2665 (2) | 0.3655 (3) | 0.3162 (3) | 0.0518 (10) | |
| H12 | 0.276256 | 0.299005 | 0.319076 | 0.062* | |
| C25 | −0.0669 (2) | 0.6183 (3) | 0.5070 (3) | 0.0488 (9) | |
| H25 | −0.090676 | 0.615755 | 0.560213 | 0.059* | |
| C26 | −0.0078 (2) | 0.6828 (3) | 0.5107 (3) | 0.0511 (10) | |
| C21 | 0.0275 (2) | 0.6859 (3) | 0.4308 (4) | 0.0555 (11) | |
| C23 | −0.0552 (2) | 0.5622 (3) | 0.3469 (3) | 0.0559 (11) | |
| H23 | −0.071640 | 0.521800 | 0.291633 | 0.067* | |
| C22 | 0.0035 (2) | 0.6245 (3) | 0.3492 (4) | 0.0611 (12) | |
| H22 | 0.027240 | 0.625415 | 0.295851 | 0.073* | |
| C27 | 0.0160 (3) | 0.7449 (4) | 0.5975 (4) | 0.0801 (15) | |
| H27 | −0.009566 | 0.739894 | 0.648683 | 0.096* |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Cu2 | 0.0329 (2) | 0.0294 (2) | 0.0334 (2) | −0.00098 (16) | 0.00347 (17) | −0.00299 (17) |
| Cu1 | 0.0343 (2) | 0.0288 (2) | 0.0348 (2) | 0.00313 (16) | 0.00299 (17) | 0.00019 (17) |
| Br3 | 0.0459 (2) | 0.0590 (3) | 0.0845 (3) | −0.0085 (2) | 0.0057 (2) | −0.0066 (2) |
| Br1 | 0.0490 (3) | 0.0770 (3) | 0.0974 (4) | −0.0180 (2) | 0.0010 (2) | −0.0192 (3) |
| Br2 | 0.0856 (4) | 0.0834 (3) | 0.0933 (4) | −0.0563 (3) | 0.0395 (3) | −0.0404 (3) |
| S1 | 0.0369 (5) | 0.0564 (6) | 0.0320 (5) | 0.0095 (4) | 0.0035 (4) | −0.0040 (4) |
| S2 | 0.0446 (5) | 0.0535 (6) | 0.0441 (5) | −0.0064 (4) | 0.0029 (4) | −0.0037 (4) |
| O3 | 0.0330 (12) | 0.0300 (11) | 0.0454 (14) | −0.0018 (9) | 0.0066 (10) | −0.0056 (10) |
| O4 | 0.0419 (14) | 0.0305 (12) | 0.0446 (14) | −0.0008 (10) | 0.0124 (11) | −0.0016 (11) |
| O1 | 0.0366 (13) | 0.0297 (11) | 0.0434 (14) | 0.0029 (10) | 0.0026 (11) | −0.0007 (10) |
| O2 | 0.0391 (14) | 0.0338 (12) | 0.0475 (15) | −0.0012 (11) | 0.0111 (11) | −0.0019 (11) |
| N4 | 0.0459 (17) | 0.0333 (15) | 0.0233 (14) | −0.0138 (13) | 0.0007 (13) | −0.0050 (12) |
| N1 | 0.0369 (16) | 0.0277 (13) | 0.0372 (16) | 0.0042 (11) | 0.0075 (12) | 0.0027 (12) |
| N2 | 0.0313 (15) | 0.0385 (15) | 0.0319 (15) | 0.0023 (12) | 0.0078 (12) | −0.0005 (12) |
| N3 | 0.0369 (16) | 0.0424 (16) | 0.0379 (17) | 0.0038 (13) | 0.0044 (14) | 0.0008 (13) |
| O7 | 0.0595 (19) | 0.0332 (14) | 0.131 (3) | 0.0022 (13) | 0.048 (2) | 0.0022 (17) |
| O5 | 0.063 (2) | 0.084 (3) | 0.112 (3) | −0.0221 (18) | 0.038 (2) | 0.012 (2) |
| C19 | 0.0388 (19) | 0.0279 (15) | 0.0267 (16) | 0.0020 (13) | 0.0114 (15) | −0.0019 (13) |
| C1 | 0.0390 (19) | 0.0350 (17) | 0.0289 (17) | 0.0013 (14) | 0.0123 (15) | 0.0002 (14) |
| C6 | 0.0345 (18) | 0.0370 (17) | 0.0307 (17) | 0.0011 (14) | 0.0086 (14) | −0.0002 (14) |
| C7 | 0.0327 (18) | 0.0366 (17) | 0.0365 (19) | 0.0083 (14) | 0.0069 (15) | 0.0067 (15) |
| C10 | 0.0414 (19) | 0.0331 (17) | 0.0327 (18) | −0.0085 (14) | 0.0161 (15) | −0.0065 (14) |
| C18 | 0.051 (2) | 0.0343 (18) | 0.041 (2) | 0.0109 (16) | 0.0169 (17) | 0.0069 (16) |
| C17 | 0.037 (2) | 0.0419 (19) | 0.048 (2) | 0.0089 (15) | 0.0089 (16) | 0.0030 (17) |
| O6 | 0.078 (3) | 0.102 (3) | 0.099 (3) | −0.041 (2) | −0.001 (2) | −0.012 (2) |
| C15 | 0.0362 (19) | 0.0426 (19) | 0.0358 (19) | −0.0062 (15) | 0.0117 (15) | −0.0088 (15) |
| C16 | 0.0281 (17) | 0.050 (2) | 0.0364 (19) | −0.0015 (15) | 0.0051 (14) | −0.0060 (16) |
| C2 | 0.049 (2) | 0.0314 (17) | 0.041 (2) | 0.0011 (15) | 0.0136 (17) | −0.0020 (15) |
| C20 | 0.044 (2) | 0.0340 (17) | 0.043 (2) | 0.0084 (16) | 0.0222 (18) | 0.0087 (16) |
| C5 | 0.0369 (19) | 0.047 (2) | 0.044 (2) | 0.0020 (16) | 0.0080 (16) | −0.0002 (17) |
| C9 | 0.048 (2) | 0.0324 (18) | 0.063 (3) | 0.0054 (16) | 0.0182 (19) | 0.0097 (18) |
| C11 | 0.052 (2) | 0.0371 (19) | 0.046 (2) | −0.0023 (16) | 0.0118 (18) | −0.0015 (16) |
| C8 | 0.046 (2) | 0.0290 (17) | 0.061 (3) | 0.0065 (15) | 0.0132 (18) | 0.0037 (17) |
| C3 | 0.057 (2) | 0.0362 (19) | 0.042 (2) | −0.0074 (17) | 0.0153 (18) | −0.0066 (16) |
| C4 | 0.040 (2) | 0.053 (2) | 0.044 (2) | −0.0118 (17) | 0.0093 (17) | −0.0111 (18) |
| C14 | 0.037 (2) | 0.060 (2) | 0.053 (2) | −0.0152 (18) | 0.0127 (18) | −0.018 (2) |
| C24 | 0.037 (2) | 0.046 (2) | 0.053 (2) | 0.0041 (16) | 0.0040 (18) | 0.0042 (18) |
| C13 | 0.060 (3) | 0.052 (2) | 0.051 (2) | −0.027 (2) | 0.025 (2) | −0.0200 (19) |
| C12 | 0.073 (3) | 0.0360 (19) | 0.052 (2) | −0.0137 (19) | 0.024 (2) | −0.0082 (18) |
| C25 | 0.040 (2) | 0.058 (2) | 0.047 (2) | −0.0010 (18) | 0.0089 (17) | 0.0069 (19) |
| C26 | 0.041 (2) | 0.057 (2) | 0.053 (2) | −0.0026 (18) | 0.0039 (18) | 0.005 (2) |
| C21 | 0.041 (2) | 0.056 (2) | 0.070 (3) | 0.0054 (19) | 0.013 (2) | 0.017 (2) |
| C23 | 0.060 (3) | 0.052 (2) | 0.054 (3) | 0.012 (2) | 0.009 (2) | 0.001 (2) |
| C22 | 0.060 (3) | 0.065 (3) | 0.066 (3) | 0.019 (2) | 0.031 (2) | 0.019 (2) |
| C27 | 0.069 (3) | 0.093 (4) | 0.074 (4) | −0.030 (3) | 0.008 (3) | −0.006 (3) |
| Cu1—O1 | 1.911 (2) | C18—H18B | 0.9700 |
| Cu1—O2 | 2.038 (2) | C18—C17 | 1.508 (5) |
| Cu1—N1 | 1.928 (3) | C17—H17A | 0.9700 |
| Cu1—N3 | 1.952 (3) | C17—H17B | 0.9700 |
| Cu2—O3 | 1.923 (2) | O6—C27 | 1.217 (5) |
| Cu2—O4 | 2.005 (2) | C15—C16 | 1.442 (5) |
| Cu2—N4 | 1.995 (3) | C15—C14 | 1.403 (5) |
| Cu2—N2 | 1.927 (3) | C16—H16 | 0.9300 |
| Br3—C24 | 1.903 (4) | C2—H2A | 0.9300 |
| Br1—C4 | 1.910 (4) | C2—C3 | 1.363 (5) |
| Br2—C13 | 1.902 (4) | C5—H5 | 0.9300 |
| S1—C19 | 1.629 (3) | C5—C4 | 1.358 (5) |
| S2—C20 | 1.643 (4) | C9—H9A | 0.9700 |
| O3—C10 | 1.325 (4) | C9—H9B | 0.9700 |
| O4—H4 | 0.8200 | C9—C8 | 1.490 (5) |
| O4—C18 | 1.430 (4) | C11—H11 | 0.9300 |
| O1—C1 | 1.312 (4) | C11—C12 | 1.380 (5) |
| O2—H2 | 0.8200 | C8—H8A | 0.9700 |
| O2—C9 | 1.437 (4) | C8—H8B | 0.9700 |
| N4—C20 | 1.106 (4) | C3—H3 | 0.9300 |
| N1—C7 | 1.277 (4) | C3—C4 | 1.390 (5) |
| N1—C8 | 1.474 (4) | C14—H14 | 0.9300 |
| N2—C17 | 1.464 (4) | C14—C13 | 1.367 (6) |
| N2—C16 | 1.276 (4) | C24—C25 | 1.350 (5) |
| N3—C19 | 1.153 (4) | C24—C23 | 1.378 (6) |
| O7—H7A | 0.8502 | C13—C12 | 1.375 (6) |
| O7—H7B | 0.8501 | C12—H12 | 0.9300 |
| O5—H5A | 0.8200 | C25—H25 | 0.9300 |
| O5—C21 | 1.343 (5) | C25—C26 | 1.396 (5) |
| C1—C6 | 1.416 (5) | C26—C21 | 1.391 (6) |
| C1—C2 | 1.412 (5) | C26—C27 | 1.445 (7) |
| C6—C7 | 1.431 (5) | C21—C22 | 1.387 (6) |
| C6—C5 | 1.409 (5) | C23—H23 | 0.9300 |
| C7—H7 | 0.9300 | C23—C22 | 1.375 (6) |
| C10—C15 | 1.405 (5) | C22—H22 | 0.9300 |
| C10—C11 | 1.406 (5) | C27—H27 | 0.9300 |
| C18—H18A | 0.9700 | ||
| O1—Cu1—O2 | 166.82 (10) | C15—C16—H16 | 117.3 |
| N3—Cu1—O2 | 89.45 (11) | C1—C2—H2A | 118.8 |
| O1—Cu1—N1 | 93.58 (10) | C3—C2—C1 | 122.4 (3) |
| O1—Cu1—N3 | 94.69 (11) | C3—C2—H2A | 118.8 |
| N1—Cu1—O2 | 82.51 (10) | N4—C20—S2 | 176.2 (3) |
| N1—Cu1—N3 | 171.73 (12) | C6—C5—H5 | 119.7 |
| O3—Cu2—O4 | 166.23 (10) | C4—C5—C6 | 120.6 (3) |
| O3—Cu2—N4 | 91.49 (10) | C4—C5—H5 | 119.7 |
| O3—Cu2—N2 | 93.35 (11) | O2—C9—H9A | 110.2 |
| N4—Cu2—O4 | 92.01 (10) | O2—C9—H9B | 110.2 |
| N2—Cu2—O4 | 82.24 (11) | O2—C9—C8 | 107.5 (3) |
| N2—Cu2—N4 | 173.38 (11) | H9A—C9—H9B | 108.5 |
| C10—O3—Cu2 | 125.5 (2) | C8—C9—H9A | 110.2 |
| Cu2—O4—H4 | 116.5 | C8—C9—H9B | 110.2 |
| C18—O4—Cu2 | 111.8 (2) | C10—C11—H11 | 119.5 |
| C18—O4—H4 | 109.5 | C12—C11—C10 | 121.0 (4) |
| C1—O1—Cu1 | 126.8 (2) | C12—C11—H11 | 119.5 |
| Cu1—O2—H2 | 113.0 | N1—C8—C9 | 107.8 (3) |
| C9—O2—Cu1 | 110.9 (2) | N1—C8—H8A | 110.1 |
| C9—O2—H2 | 109.5 | N1—C8—H8B | 110.1 |
| C20—N4—Cu2 | 150.0 (3) | C9—C8—H8A | 110.1 |
| C7—N1—Cu1 | 126.4 (2) | C9—C8—H8B | 110.1 |
| C7—N1—C8 | 120.9 (3) | H8A—C8—H8B | 108.5 |
| C8—N1—Cu1 | 112.6 (2) | C2—C3—H3 | 120.3 |
| C17—N2—Cu2 | 113.8 (2) | C2—C3—C4 | 119.3 (3) |
| C16—N2—Cu2 | 126.2 (2) | C4—C3—H3 | 120.3 |
| C16—N2—C17 | 119.9 (3) | C5—C4—Br1 | 120.0 (3) |
| C19—N3—Cu1 | 161.4 (3) | C5—C4—C3 | 121.0 (3) |
| H7A—O7—H7B | 104.5 | C3—C4—Br1 | 119.0 (3) |
| C21—O5—H5A | 109.5 | C15—C14—H14 | 120.2 |
| N3—C19—S1 | 178.3 (3) | C13—C14—C15 | 119.6 (4) |
| O1—C1—C6 | 124.2 (3) | C13—C14—H14 | 120.2 |
| O1—C1—C2 | 118.7 (3) | C25—C24—Br3 | 120.1 (3) |
| C2—C1—C6 | 117.1 (3) | C25—C24—C23 | 120.7 (4) |
| C1—C6—C7 | 123.2 (3) | C23—C24—Br3 | 119.2 (3) |
| C5—C6—C1 | 119.6 (3) | C14—C13—Br2 | 119.8 (3) |
| C5—C6—C7 | 117.2 (3) | C14—C13—C12 | 121.5 (3) |
| N1—C7—C6 | 125.5 (3) | C12—C13—Br2 | 118.7 (3) |
| N1—C7—H7 | 117.2 | C11—C12—H12 | 120.2 |
| C6—C7—H7 | 117.2 | C13—C12—C11 | 119.6 (4) |
| O3—C10—C15 | 124.0 (3) | C13—C12—H12 | 120.2 |
| O3—C10—C11 | 117.7 (3) | C24—C25—H25 | 119.9 |
| C15—C10—C11 | 118.2 (3) | C24—C25—C26 | 120.3 (4) |
| O4—C18—H18A | 110.5 | C26—C25—H25 | 119.9 |
| O4—C18—H18B | 110.5 | C25—C26—C27 | 119.6 (4) |
| O4—C18—C17 | 106.2 (3) | C21—C26—C25 | 119.4 (4) |
| H18A—C18—H18B | 108.7 | C21—C26—C27 | 120.9 (4) |
| C17—C18—H18A | 110.5 | O5—C21—C26 | 122.1 (4) |
| C17—C18—H18B | 110.5 | O5—C21—C22 | 118.5 (4) |
| N2—C17—C18 | 108.0 (3) | C22—C21—C26 | 119.3 (4) |
| N2—C17—H17A | 110.1 | C24—C23—H23 | 120.0 |
| N2—C17—H17B | 110.1 | C22—C23—C24 | 120.1 (4) |
| C18—C17—H17A | 110.1 | C22—C23—H23 | 120.0 |
| C18—C17—H17B | 110.1 | C21—C22—H22 | 119.9 |
| H17A—C17—H17B | 108.4 | C23—C22—C21 | 120.1 (4) |
| C10—C15—C16 | 123.3 (3) | C23—C22—H22 | 119.9 |
| C14—C15—C10 | 120.0 (3) | O6—C27—C26 | 125.4 (5) |
| C14—C15—C16 | 116.7 (3) | O6—C27—H27 | 117.3 |
| N2—C16—C15 | 125.4 (3) | C26—C27—H27 | 117.3 |
| N2—C16—H16 | 117.3 | ||
| Cu2—O3—C10—C15 | 15.2 (4) | C10—C15—C14—C13 | 1.7 (6) |
| Cu2—O3—C10—C11 | −165.6 (2) | C10—C11—C12—C13 | 0.8 (6) |
| Cu2—O4—C18—C17 | 39.3 (3) | C17—N2—C16—C15 | −175.2 (3) |
| Cu2—N2—C17—C18 | 31.8 (3) | C15—C10—C11—C12 | −0.2 (5) |
| Cu2—N2—C16—C15 | 0.8 (5) | C15—C14—C13—Br2 | −179.9 (3) |
| Cu1—O1—C1—C6 | −5.0 (5) | C15—C14—C13—C12 | −1.0 (6) |
| Cu1—O1—C1—C2 | 174.7 (2) | C16—N2—C17—C18 | −151.7 (3) |
| Cu1—O2—C9—C8 | −35.9 (3) | C16—C15—C14—C13 | −178.5 (3) |
| Cu1—N1—C7—C6 | −0.5 (5) | C2—C1—C6—C7 | −178.3 (3) |
| Cu1—N1—C8—C9 | −37.5 (4) | C2—C1—C6—C5 | 1.1 (5) |
| Br3—C24—C25—C26 | −179.8 (3) | C2—C3—C4—Br1 | 179.5 (3) |
| Br3—C24—C23—C22 | −179.7 (3) | C2—C3—C4—C5 | 0.5 (6) |
| Br2—C13—C12—C11 | 178.7 (3) | C5—C6—C7—N1 | −177.9 (3) |
| O3—C10—C15—C16 | −1.6 (5) | C11—C10—C15—C16 | 179.1 (3) |
| O3—C10—C15—C14 | 178.2 (3) | C11—C10—C15—C14 | −1.1 (5) |
| O3—C10—C11—C12 | −179.5 (3) | C8—N1—C7—C6 | 175.9 (3) |
| O4—C18—C17—N2 | −45.1 (4) | C14—C15—C16—N2 | 173.2 (3) |
| O1—C1—C6—C7 | 1.5 (5) | C14—C13—C12—C11 | −0.2 (6) |
| O1—C1—C6—C5 | −179.2 (3) | C24—C25—C26—C21 | −0.1 (6) |
| O1—C1—C2—C3 | −180.0 (3) | C24—C25—C26—C27 | −179.9 (4) |
| O2—C9—C8—N1 | 46.9 (4) | C24—C23—C22—C21 | −0.9 (6) |
| O5—C21—C22—C23 | −178.5 (4) | C25—C24—C23—C22 | 0.4 (6) |
| C1—C6—C7—N1 | 1.5 (5) | C25—C26—C21—O5 | 179.1 (4) |
| C1—C6—C5—C4 | −1.2 (5) | C25—C26—C21—C22 | −0.4 (6) |
| C1—C2—C3—C4 | −0.6 (5) | C25—C26—C27—O6 | 179.7 (5) |
| C6—C1—C2—C3 | −0.2 (5) | C26—C21—C22—C23 | 0.9 (6) |
| C6—C5—C4—Br1 | −178.6 (3) | C21—C26—C27—O6 | −0.1 (8) |
| C6—C5—C4—C3 | 0.4 (6) | C23—C24—C25—C26 | 0.2 (6) |
| C7—N1—C8—C9 | 145.7 (3) | C27—C26—C21—O5 | −1.1 (7) |
| C7—C6—C5—C4 | 178.2 (3) | C27—C26—C21—C22 | 179.4 (4) |
| C10—C15—C16—N2 | −7.0 (6) |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O4—H4···O7 | 0.82 | 1.75 | 2.562 (4) | 174 |
| O2—H2···O3 | 0.82 | 1.84 | 2.647 (3) | 169 |
| O7—H7A···O1 | 0.85 | 1.88 | 2.709 (4) | 163 |
| O7—H7B···S2i | 0.85 | 2.64 | 3.290 (3) | 135 |
| O5—H5A···O6 | 0.82 | 1.94 | 2.655 (6) | 146 |
| C18—H18A···Br3ii | 0.97 | 3.32 | 3.856 (4) | 117 |
| C18—H18A···S1 | 0.97 | 2.98 | 3.801 (4) | 143 |
| C18—H18A···N3 | 0.97 | 3.22 | 3.785 (5) | 119 |
| C17—H17A···O5 | 0.97 | 2.73 | 3.368 (5) | 124 |
| C16—H16···O6iii | 0.93 | 2.52 | 3.376 (5) | 153 |
| C2—H2A···O2iv | 0.93 | 2.92 | 3.726 (4) | 146 |
| C2—H2A···O7 | 0.93 | 3.08 | 3.548 (5) | 113 |
| C9—H9A···N4v | 0.97 | 3.20 | 3.851 (4) | 126 |
| C9—H9B···O3v | 0.97 | 3.03 | 3.613 (5) | 120 |
| C9—H9B···N4 | 0.97 | 3.20 | 3.700 (5) | 114 |
| C11—H11···S2v | 0.93 | 3.11 | 3.709 (4) | 124 |
| C8—H8A···S1vi | 0.97 | 3.29 | 3.881 (3) | 121 |
| C8—H8A···O3v | 0.97 | 3.07 | 3.773 (5) | 130 |
| C8—H8B···S2iii | 0.97 | 3.30 | 3.784 (4) | 113 |
| C8—H8B···O7vi | 0.97 | 2.96 | 3.739 (6) | 138 |
| C14—H14···O6iii | 0.93 | 3.12 | 3.827 (6) | 134 |
| C12—H12···S2v | 0.93 | 2.93 | 3.616 (5) | 131 |
| C22—H22···O6iii | 0.93 | 2.97 | 3.847 (6) | 158 |
| C27—H27···Br2vii | 0.93 | 3.04 | 3.949 (6) | 166 |
| Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x, y+1/2, −z+1/2; (iii) x, −y+3/2, z−1/2; (iv) −x+1, y+1/2, −z+1/2; (v) −x+1, −y+1, −z+1; (vi) −x+1, y−1/2, −z+1/2; (vii) −x, −y+1, −z+1. |
Acknowledgements
IET gratefully acknowledges the support of Dr Eugenio Cavallo, Scientific Attaché, and the Italian Embassy in Dakar for their assistance in facilitating participation in the MAECI programme "Contributi per missioni di studio e ricerca 2025/ Contributions for study and research missions 2025", as well as for their continued commitment to fostering scientific collaboration between Senegal and Italy. The authors are grateful to the FAIRE programme provided by the Cambridge Crystallographic Data Centre (CCDC) for the opportunity to use the Cambridge Structural Database (CSD) and associated software.
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