The crystal structures of the title compounds consist of discrete complexes, in which the metal cations are octahedrally coordinated.
Keywords: crystal structure, manganese(II)thiocyanate, 3-methylpyridine, IR spectra, thermal properties
Abstract
The reaction of Mn(NCS)2 or Fe(NCS)2 with 3-methylpyridine (C6H7N) leads to the formation of two isostructural compounds with compositions [Mn(NCS)2(C6H7N)4] (1) and [Fe(NCS)2(C6H7N)4] (2). IR spectroscopic investigations indicate that only terminally coordinated thiocyanate anions are present. This is confirmed by single-crystal structure analysis, which shows that their crystal structures consist of discrete centrosymmetric complexes, in which the metal cations are octahedrally coordinated by two N-bonded thiocyanate anions and four 3-methylpyridine ligands. X-ray powder diffraction (XRPD) proves that pure samples have been obtained. Thermogravimetric measurements show that decomposition starts at about 90°C and that the two coligands are removed in one step for 1 whereas for 2 no clearly resolved steps are visible. XRPD measurements of the residue obtained after the first mass loss of 1 show that a new and unknown crystalline compound has been formed.
1. Chemical context
For many years we and others have been interested in the synthesis of coordination compounds based on thiocyanate anions. In this context, we are especially interested in compounds where paramagnetic metal cations are linked by the anionic ligands into networks, because they can show interesting magnetic properties (Mautner et al., 2018 ▸; Rams et al., 2020 ▸; Böhme et al., 2020 ▸). Unfortunately, the synthesis of such compounds is sometimes difficult to achieve, because metal cations such as, for example MnII, FeII, CoII or NiII are not very chalcophilic and prefer to coordinate only to the terminal thiocyanate N atom. With mono-coordinating ligands this leads to the formation of discrete complexes instead of the desired networks. In several cases, this problem can be solved by using discrete complexes as precursors that on heating lose their coligands stepwise, which can lead to the desired compounds with bridging coordination (Werner et al., 2015a
▸; Suckert et al., 2016 ▸).
In the past, many such compounds were prepared following this route, using predominantly pyridine-based ligands that are substituted at the 4-position. In the course of our systematic work, we became interested in 3-methylpyridine (3-picoline; C6H7N) as a coligand. Some compounds have already been reported with this ligand, but bridging coordination of the anionic ligands is observed in only a very few of them (see Database survey). This includes compounds with chalcophilic metal cations like CuII, HgII or CdII (see Database survey). Some time ago we tried to prepare compounds based on cobalt and 3-methylpyridine as a coligand, but only octahedral discrete complexes were observed (Boeckmann et al., 2011a ▸). When the compound Co(NCS)2(3-methylpyridine)4 is investigated by thermogravimetry, the removal of two 3-methylpyridine molecules can be detected but, instead of the desired compounds with bridging thiocyanate anions, only a mononuclear tetrahedral complex is obtained in which the CoII cations are coordinated by two terminal N-bonded thiocyanate anions and two 3-methylpyridine coligands. With Ni(NCS)2, many compounds are known, but all of them consist of discrete complexes with the composition Ni(NCS)2(3-methylpyridine)4 that form channels in which additional solvate molecules are embedded. Two compounds are reported in the Cambridge Structural Database with Mn(NCS)2 and Fe(NCS)2 and 3-methylpyridine as ligand, except for one mixed-metal compound based on manganese and mercury (Małecki, 2017a ▸) and therefore, we tried to prepare compounds based on these metal cations. From the reaction of Mn(NCS)2 and Fe(NCS)2 with 3-methylpyridine, two compounds with the composition Mn(NCS)2(3-methylpyridine)4 (1) and Fe(NCS)2(3-methylpyridine)4 (2) where obtained. IR spectroscopic investigations reveal that the CN stretching vibration of the anionic ligands is observed at 2048 cm−1 for 1 and 2046 cm−1 for 2, indicating that only terminal N-bonded thiocyanate anions are present (Figures S1 and S2 in the supporting information), which was confirmed by structural analysis. Comparison of the experimental X-ray powder diffraction pattern with that calculated from the structure analysis using lattice parameters obtained by measurements performed at room-temperature proves that pure samples have been obtained (Figs. 1 ▸ and 2 ▸). Measurements simultaneously using thermogravimetry and differential thermoanalysis (TG–DTA) reveal that decomposition already starts at about 90°C for both compounds (Figures S3 and S4). Compound 1 shows a mass loss of 34.8%, which is in reasonable agreement with that calculated for the removal of two 3-methylpyridine ligands. For compound 2, a poorly resolved TG curve is observed where the sample mass decreases continuously. The residue of 1 isolated after this mass loss was investigated by XRPD, but the pattern could neither be indexed nor assigned to the possibly isotypic phase Cd(NCS)2(3-methylpyridine)2 (Figure S5; Taniguchi et al., 1987 ▸).
Figure 1.
Experimental (top) and calculated (bottom) X-ray powder patterns of compound 1 measured with Cu Kα radiation.
Figure 2.
Experimental (top) and calculated (bottom) X-ray powder patterns of compound 2 measured with Cu Kα radiation.
2. Structural commentary
Mn(NCS)2(3-methylpyridine)4 (1) and Fe(NCS)2(3-methylpyridine)4 (2) are isotypic to Co(NCS)2(3-methylpyridine)4 reported in the literature (Boeckmann et al., 2011a ▸) and form discrete complexes, in which the metal cations are octahedrally coordinated by two terminal N-bonded thiocyanate anions and two 3-methylpyridine coligands (Figs. 3 ▸ and 4 ▸). The asymmetric unit consists of one metal cation that is located on a crystallographic center of inversion as well as one thiocyanate anion and two 3-methylpyridine ligands in general positions. As expected, the M—N bond lengths to the negatively charged thiocyanate anions are shorter than those to the 3-methylpyridine coligands and all M—N bond lengths are shorter for the Fe compound 2 than for the Mn compound 1 (Tables 1 ▸ and 2 ▸). From the N—M—N bonding angles, it is obvious that both octahedra are slightly distorted, which can also be seen from the mean octahedral quadratic elongation (1.0018 for 1 and 1.0023 for 2) and the octahedral angle variance (1.259°2 for 1 and 1.096°2 for 2) calculated by the method of Robinson et al. (1971 ▸).
Figure 3.
The molecular structure of compound 1 with displacement ellipsoids drawn at the 50% probability level. [Symmetry code: (A) 1 − x, 1 − y, 1 − z.]
Figure 4.
The molecular structure of compound 2 with displacement ellipsoids drawn at the 50% probability level. [Symmetry code: (A) 1 − x, 1 − y, 1 − z.]
Table 1. Selected geometric parameters (Å, °) for 1 .
| Mn1—N1 | 2.1830 (11) | Mn1—N21 | 2.2866 (11) |
| Mn1—N11 | 2.3306 (11) | ||
| N1—Mn1—N11i | 91.56 (4) | N21—Mn1—N11 | 89.06 (4) |
| N1—Mn1—N11 | 88.44 (4) | N21i—Mn1—N11 | 90.94 (4) |
| N1i—Mn1—N21 | 90.37 (4) | C1—N1—Mn1 | 153.96 (10) |
| N1—Mn1—N21 | 89.63 (4) |
Symmetry code: (i)
.
Table 2. Selected geometric parameters (Å, °) for 2 .
| Fe1—N1 | 2.1103 (10) | Fe1—N21 | 2.2253 (10) |
| Fe1—N11 | 2.2779 (10) | ||
| N1—Fe1—N11i | 91.23 (4) | N21—Fe1—N11 | 89.03 (4) |
| N1—Fe1—N11 | 88.77 (4) | N21i—Fe1—N11 | 90.97 (4) |
| N1i—Fe1—N21 | 90.75 (4) | C1—N1—Fe1 | 157.12 (10) |
| N1—Fe1—N21 | 89.25 (4) |
Symmetry code: (i)
.
3. Supramolecular features
In the extended structures of both compounds, the discrete complexes are arranged into columns that propagate along the crystallographic b-axis direction (Fig. 5 ▸). Between these columns, neighboring 3-methylpyridine ligands overlap but their ring planes are not parallel, which would be indicative of π–π stacking interactions (Fig. 5 ▸). There are some contacts between the C—H hydrogen atoms and the thiocyanate N and S atoms, but at distances and angles far from those expected for hydrogen bonding (Tables 3 ▸ and 4 ▸).
Figure 5.
The packing of compound 1 viewed along the crystallographic b-axis.
Table 3. Hydrogen-bond geometry (Å, °) for 1 .
| D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A |
|---|---|---|---|---|
| C11—H11⋯N1i | 0.95 | 2.60 | 3.2484 (17) | 126 |
| C15—H15⋯S1ii | 0.95 | 3.00 | 3.5588 (14) | 119 |
| C15—H15⋯N1 | 0.95 | 2.52 | 3.1535 (17) | 125 |
Symmetry codes: (i)
; (ii)
.
Table 4. Hydrogen-bond geometry (Å, °) for 2 .
| D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A |
|---|---|---|---|---|
| C11—H11⋯N1i | 0.95 | 2.54 | 3.1668 (16) | 124 |
| C15—H15⋯S1ii | 0.95 | 3.00 | 3.5523 (13) | 119 |
| C15—H15⋯N1 | 0.95 | 2.48 | 3.0961 (16) | 123 |
Symmetry codes: (i)
; (ii)
.
4. Database survey
In the Cambridge Structure Database (CSD, version 5.43, last update November 2021; Groom et al., 2016 ▸) no Fe(NCS)2-based compounds with 3-methylpyridine as a coligand are reported. With Mn(NCS)2 there is only the mixed-metal compound catena-[tetrakis(thiocyanato)bis(3-methylpyridine)manganesemercury] (refcode NAQYOW), in which the MnII cations are octahedrally coordinated by two 3-methylpyridine-N-oxide ligands and two N-bonding μ-1,3-bridging thiocyanate anions and are linked to HgII cations via the thiocyanate S-atoms (Małecki, 2017a ▸). The HgII cations act as tetrahedral nodes, connecting the MnII cations into a three-dimensional network.
However, several thiocyanate compounds with other transition-metal cations and 3-methylpyridine as coligand are found in the CSD. With cobalt, three different discrete complexes with the composition Co(NCS)2(3-methylpyridine)2(H2O)2 (EYAREC), Co(NCS)2(3-methylpyridine)4, isotypic to the title compounds (EYAROM and EYAROM01) as well as Co(NCS)2(3-methylpyridine)2 (EYARIG) are reported, in which the CoII cations are octahedrally or tetrahedrally coordinated (Boeckmann et al., 2011a ▸; Małecki et al., 2012 ▸). Discrete complexes, in which NiII cations are octahedrally coordinated by two terminal N-bonded thiocyanate anions and two 3-methylpyridine coligands are also known (CIVJEW, CIVJEW10, JICMIR, LAYLAY, LAYLEC, LAYLIG, LAYLOM and LAYLUS) but in their structures cavities are formed, in which additional solvent molecules are embedded (Nassimbeni et al., 1984 ▸, 1986 ▸; Pang et al., 1990 ▸, 1992 ▸). Moreover, one compound with the composition Ni(NCS)2(3-methylpyridine)2(H2O)2 is also reported (MEGCEH; Tan et al., 2006 ▸).
With CuII, the discrete complexes Cu(NCS)2(3-methylpyridine)2 (ABOTET) and Cu(NCS)2(3-methylpyridine)3 (VEPBAT) with fourfold and fivefold coordinations, respectively, and the chain compound Cu(NCS)(3-methylpyridine)2 (CUHBEM) are reported (Handy et al., 2017 ▸; Healy et al., 1984 ▸; Kabešová & Kožíšková, 1989 ▸). With Zn(NCS)2, the discrete tetrahedral complex Zn(NCS)2(3-methylpyridine)2 (ETUSAO) is reported (Boeckmann & Näther, 2011b ▸), which is isotypic to the corresponding Co(NCS)2 compound.
With Cd(NCS)2, one compound with the composition Cd(NCS)2(3-methylpyridine)2 (FIYGUP) is observed in which the CdII cations are linked by pairs of thiocyanate anions into chains (Taniguchi et al., 1987 ▸). This corresponds exactly to the structural motif in which we are interested and for which many paramagnetic compounds are known with pyridine-based ligands (Werner et al., 2014 ▸, 2015b ▸). Finally, two compounds with mercury are also found, viz. catena-[tetrakis(thiocyanato)bis(3-methylpyridine)manganesemercury] (NAQYOW; Małecki, 2017a ▸) mentioned above and the isotypic compound where MnII is replaced by ZnII (QAMSIJ; Małecki, 2017b ▸).
5. Synthesis and crystallization
Synthesis
Ba(SCN)2·3H2O and 3-picoline were purchased from Alfa Aesar. MnSO4·H2O was purchased from Merck. A reaction of equimolar amounts of Ba(SCN)2·3H2O with MnSO4·H2O in deionized water was performed. After that, the precipitate of BaSO4 was filtered off. The filtrate was dried in a rotary evaporator and as a result, a powder of Mn(NCS)2 was obtained.
Mn(NCS)2(3-methylpyridine)4: 0.25 mmol of Mn(NCS)2 (42.8 mg) were dissolved in 0.5 ml of water and then 1.0 mmol of 3-methylpyridine (97.3 µl) were added. The mixture was then heated to 333 K and left at this temperature for 2 d. Afterwards, some colorless crystals were obtained that were suitable for single-crystal X-ray analysis. To obtain powder samples, 0.5 mmol of Mn(NCS)2 (85.6 mg) were dissolved in 1.0 ml of ethanol and then 2.0 mmol of 3-methylpyridine (194.6 µl) were added. The reaction mixture was stirred for 1 d and the colorless powder was filtered off and dried in the air.
Fe(NCS)2(3-methylpyridine)4: A mixture of 0.25 mmol of FeCl2·4H2O (49.7 mg) and 0.5 mmol of KSCN (48.6 mg) was dissolved in a mixture of 0.5 ml of water and 0.5 ml of ether. Afterwards, 1.25 mmol of 3-methylpyridine (121.6 µl) were added. The mixture was left for 3 d at room temperature, leading to some yellow crystals suitable for single-crystal X-ray diffraction measurements. To obtain powder samples, a mixture of 0.5 mmol of FeCl2·4H2O (98.6 mg) and 1.0 mmol of KSCN (97.2 mg) was dissolved in 0.5 ml of water. Afterwards, 2.0 mmol of 3-methylpyridine (194.6 µl) were added and the reaction mixture was stirred for 1 d. The yellow-colored powder was filtered off and dried in the air.
Experimental details
The data collection for single-crystal structure analysis was performed using an XtaLAB Synergy, Dualflex, HyPix diffractometer from Rigaku with Cu Kα radiation.
The IR spectrum was measured using an ATI Mattson Genesis Series FTIR Spectrometer, control software: WINFIRST, from ATI Mattson.
The PXRD measurement was performed with Cu Kα1 radiation (λ = 1.540598 Å) using a Stoe Transmission Powder Diffraction System (STADI P) that is equipped with a MYTHEN 1K detector and a Johansson-type Ge(111) monochromator.
Thermogravimetry and differential thermoanalysis (TG–DTA) measurements were performed in a dynamic nitrogen atmosphere in Al2O3 crucibles using a STA-PT 1000 thermobalance from Linseis. The instrument was calibrated using standard reference materials.
6. Refinement
Crystal data, data collection and structure refinement details are summarized in Table 5 ▸. The C-bound H atoms were positioned with idealized geometry (methyl H atoms allowed to rotate but not to tip) and were refined isotropically with U iso(H) = 1.2U eq(C) (1.5 for methyl H atoms) using a riding model.
Table 5. Experimental details.
| 1 | 2 | |
|---|---|---|
| Crystal data | ||
| Chemical formula | [Mn(NCS)2(C6H7N)4] | [Fe(NCS)2(C6H7N)4] |
| M r | 543.60 | 544.51 |
| Crystal system, space group | Orthorhombic, P b c n | Orthorhombic, P b c n |
| Temperature (K) | 100 | 100 |
| a, b, c (Å) | 17.47811 (10), 8.93570 (6), 17.36177 (10) | 17.3733 (1), 8.94119 (5), 17.24862 (10) |
| V (Å3) | 2711.55 (3) | 2679.37 (3) |
| Z | 4 | 4 |
| Radiation type | Cu Kα | Cu Kα |
| μ (mm−1) | 5.60 | 6.17 |
| Crystal size (mm) | 0.18 × 0.15 × 0.1 | 0.16 × 0.15 × 0.15 |
| Data collection | ||
| Diffractometer | XtaLAB Synergy, Dualflex, HyPix | XtaLAB Synergy, Dualflex, HyPix |
| Absorption correction | Multi-scan (CrysAlis PRO; Rigaku OD, 2021 ▸) | Multi-scan (CrysAlis PRO; Rigaku OD, 2021 ▸) |
| T min, T max | 0.786, 1.000 | 0.555, 1.000 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 23041, 2918, 2841 | 22225, 2875, 2804 |
| R int | 0.021 | 0.020 |
| (sin θ/λ)max (Å−1) | 0.638 | 0.638 |
| Refinement | ||
| R[F 2 > 2σ(F 2)], wR(F 2), S | 0.028, 0.078, 1.07 | 0.026, 0.073, 1.06 |
| No. of reflections | 2918 | 2875 |
| No. of parameters | 162 | 163 |
| H-atom treatment | H-atom parameters constrained | H-atom parameters constrained |
| Δρmax, Δρmin (e Å−3) | 0.45, −0.35 | 0.39, −0.28 |
Supplementary Material
Figure S1. IR spectrum of compound 1. The value of the CN-stretching vibration is given. DOI: 10.1107/S2056989022006491/hb8024sup4.png
Figure S2. IR spectrum of compound 2. The value of the CN-stretching vibration is given. DOI: 10.1107/S2056989022006491/hb8024sup5.png
Figure S3. TG-DTA curve of compound 1 measured with 4 degC/min in an nitrogen atmosphere. DOI: 10.1107/S2056989022006491/hb8024sup6.png
Figure S4. TG-DTA curve of compound 2 measured with 4 degC/min in an nitrogen atmosphere. DOI: 10.1107/S2056989022006491/hb8024sup7.png
Figure S5. Experimental XRPD pattern of the product obtained after the first mass loss in a TG measurement of compound 1 (top) and calculated powder pattern of Cd(NCS)2(3-methylpyridine)2 (bottom). DOI: 10.1107/S2056989022006491/hb8024sup8.jpg
Crystal structure: contains datablock(s) 1, 2. DOI: 10.1107/S2056989022006491/hb8024sup1.cif
Structure factors: contains datablock(s) 1. DOI: 10.1107/S2056989022006491/hb80241sup2.hkl
Structure factors: contains datablock(s) 2. DOI: 10.1107/S2056989022006491/hb80242sup3.hkl
Additional supporting information: crystallographic information; 3D view; checkCIF report
supplementary crystallographic information
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)manganese(II) (1) . Crystal data
| [Mn(NCS)2(C6H7N)4] | Dx = 1.332 Mg m−3 |
| Mr = 543.60 | Cu Kα radiation, λ = 1.54184 Å |
| Orthorhombic, Pbcn | Cell parameters from 12231 reflections |
| a = 17.47811 (10) Å | θ = 5.1–79.2° |
| b = 8.93570 (6) Å | µ = 5.60 mm−1 |
| c = 17.36177 (10) Å | T = 100 K |
| V = 2711.55 (3) Å3 | Block, intense colourless |
| Z = 4 | 0.18 × 0.15 × 0.1 mm |
| F(000) = 1132 |
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)manganese(II) (1) . Data collection
| XtaLAB Synergy, Dualflex, HyPix diffractometer | 2918 independent reflections |
| Radiation source: micro-focus sealed X-ray tube, PhotonJet (Cu) X-ray Source | 2841 reflections with I > 2σ(I) |
| Mirror monochromator | Rint = 0.021 |
| Detector resolution: 10.0000 pixels mm-1 | θmax = 79.8°, θmin = 5.1° |
| ω scans | h = −16→22 |
| Absorption correction: multi-scan (CrysalisPro; Rigaku OD, 2021) | k = −10→11 |
| Tmin = 0.786, Tmax = 1.000 | l = −22→22 |
| 23041 measured reflections |
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)manganese(II) (1) . Refinement
| Refinement on F2 | Primary atom site location: dual |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| R[F2 > 2σ(F2)] = 0.028 | H-atom parameters constrained |
| wR(F2) = 0.078 | w = 1/[σ2(Fo2) + (0.0428P)2 + 1.4595P] where P = (Fo2 + 2Fc2)/3 |
| S = 1.07 | (Δ/σ)max = 0.001 |
| 2918 reflections | Δρmax = 0.45 e Å−3 |
| 162 parameters | Δρmin = −0.35 e Å−3 |
| 0 restraints |
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)manganese(II) (1) . Special details
| 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. |
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)manganese(II) (1) . Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
| x | y | z | Uiso*/Ueq | ||
| Mn1 | 0.500000 | 0.500000 | 0.500000 | 0.01493 (10) | |
| S1 | 0.37925 (2) | 0.28776 (4) | 0.72629 (2) | 0.02871 (11) | |
| C1 | 0.43007 (7) | 0.32513 (14) | 0.65000 (8) | 0.0197 (3) | |
| N1 | 0.46439 (6) | 0.35374 (13) | 0.59412 (6) | 0.0213 (2) | |
| N11 | 0.62368 (6) | 0.40622 (13) | 0.51371 (6) | 0.0187 (2) | |
| C11 | 0.68099 (7) | 0.45625 (15) | 0.46930 (8) | 0.0211 (3) | |
| H11 | 0.668777 | 0.523569 | 0.428777 | 0.025* | |
| C12 | 0.75732 (8) | 0.41561 (15) | 0.47890 (8) | 0.0230 (3) | |
| C13 | 0.77419 (8) | 0.31480 (16) | 0.53720 (9) | 0.0260 (3) | |
| H13 | 0.825438 | 0.283210 | 0.545420 | 0.031* | |
| C14 | 0.71595 (8) | 0.26057 (16) | 0.58327 (8) | 0.0262 (3) | |
| H14 | 0.726560 | 0.191037 | 0.623264 | 0.031* | |
| C15 | 0.64179 (8) | 0.30937 (15) | 0.57014 (8) | 0.0210 (3) | |
| H15 | 0.602055 | 0.272809 | 0.602382 | 0.025* | |
| C16 | 0.81796 (9) | 0.48323 (18) | 0.42866 (10) | 0.0328 (3) | |
| H16A | 0.805388 | 0.465065 | 0.374453 | 0.049* | |
| H16B | 0.867527 | 0.437548 | 0.440654 | 0.049* | |
| H16C | 0.820602 | 0.591251 | 0.438045 | 0.049* | |
| N21 | 0.52897 (6) | 0.68274 (12) | 0.58746 (6) | 0.0188 (2) | |
| C21 | 0.56837 (7) | 0.65317 (14) | 0.65216 (7) | 0.0198 (3) | |
| H21 | 0.579930 | 0.551668 | 0.663532 | 0.024* | |
| C22 | 0.59328 (8) | 0.76267 (16) | 0.70361 (8) | 0.0228 (3) | |
| C23 | 0.57305 (8) | 0.91022 (16) | 0.68741 (8) | 0.0264 (3) | |
| H23 | 0.588277 | 0.988617 | 0.721038 | 0.032* | |
| C24 | 0.53065 (8) | 0.94200 (15) | 0.62205 (9) | 0.0260 (3) | |
| H24 | 0.515523 | 1.041791 | 0.610919 | 0.031* | |
| C25 | 0.51069 (8) | 0.82605 (15) | 0.57323 (8) | 0.0220 (3) | |
| H25 | 0.482864 | 0.848780 | 0.527706 | 0.026* | |
| C26 | 0.63924 (10) | 0.72132 (18) | 0.77362 (9) | 0.0320 (3) | |
| H26A | 0.688861 | 0.772265 | 0.771841 | 0.048* | |
| H26B | 0.647277 | 0.612794 | 0.774556 | 0.048* | |
| H26C | 0.611546 | 0.751935 | 0.820100 | 0.048* |
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)manganese(II) (1) . Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Mn1 | 0.01338 (16) | 0.01517 (16) | 0.01624 (17) | −0.00031 (10) | −0.00030 (9) | 0.00049 (9) |
| S1 | 0.0353 (2) | 0.02628 (19) | 0.02457 (18) | −0.00033 (14) | 0.00961 (14) | 0.00401 (13) |
| C1 | 0.0195 (6) | 0.0158 (6) | 0.0238 (6) | 0.0011 (5) | −0.0029 (5) | 0.0002 (5) |
| N1 | 0.0202 (5) | 0.0216 (5) | 0.0220 (5) | −0.0006 (4) | 0.0010 (4) | 0.0034 (4) |
| N11 | 0.0166 (5) | 0.0185 (5) | 0.0209 (5) | 0.0003 (4) | −0.0011 (4) | −0.0022 (4) |
| C11 | 0.0194 (6) | 0.0201 (6) | 0.0238 (6) | 0.0004 (5) | 0.0000 (5) | 0.0003 (5) |
| C12 | 0.0177 (6) | 0.0220 (6) | 0.0292 (6) | −0.0003 (5) | 0.0015 (5) | −0.0028 (5) |
| C13 | 0.0166 (6) | 0.0272 (7) | 0.0341 (8) | 0.0029 (5) | −0.0045 (5) | −0.0007 (6) |
| C14 | 0.0235 (7) | 0.0268 (7) | 0.0282 (7) | 0.0034 (5) | −0.0050 (5) | 0.0044 (6) |
| C15 | 0.0203 (6) | 0.0205 (6) | 0.0222 (6) | −0.0002 (5) | −0.0016 (5) | 0.0000 (5) |
| C16 | 0.0231 (7) | 0.0369 (8) | 0.0384 (9) | −0.0003 (6) | 0.0074 (6) | 0.0014 (6) |
| N21 | 0.0168 (5) | 0.0180 (5) | 0.0217 (5) | −0.0006 (4) | 0.0008 (4) | −0.0008 (4) |
| C21 | 0.0199 (6) | 0.0190 (6) | 0.0206 (6) | −0.0009 (5) | 0.0006 (5) | −0.0012 (5) |
| C22 | 0.0241 (6) | 0.0235 (6) | 0.0209 (6) | −0.0037 (5) | 0.0024 (5) | −0.0031 (5) |
| C23 | 0.0296 (7) | 0.0215 (6) | 0.0279 (7) | −0.0059 (5) | 0.0049 (5) | −0.0073 (5) |
| C24 | 0.0272 (7) | 0.0163 (6) | 0.0343 (7) | −0.0002 (5) | 0.0054 (6) | −0.0008 (5) |
| C25 | 0.0196 (6) | 0.0198 (6) | 0.0266 (7) | 0.0007 (5) | 0.0008 (5) | 0.0018 (5) |
| C26 | 0.0387 (8) | 0.0329 (8) | 0.0243 (7) | −0.0053 (7) | −0.0066 (6) | −0.0055 (6) |
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)manganese(II) (1) . Geometric parameters (Å, º)
| Mn1—N1i | 2.1830 (11) | C15—H15 | 0.9500 |
| Mn1—N1 | 2.1830 (11) | C16—H16A | 0.9800 |
| Mn1—N11i | 2.3307 (11) | C16—H16B | 0.9800 |
| Mn1—N11 | 2.3306 (11) | C16—H16C | 0.9800 |
| Mn1—N21 | 2.2866 (11) | N21—C21 | 1.3439 (17) |
| Mn1—N21i | 2.2866 (11) | N21—C25 | 1.3427 (17) |
| S1—C1 | 1.6293 (14) | C21—H21 | 0.9500 |
| C1—N1 | 1.1690 (18) | C21—C22 | 1.3945 (18) |
| N11—C11 | 1.3408 (17) | C22—C23 | 1.394 (2) |
| N11—C15 | 1.3450 (17) | C22—C26 | 1.503 (2) |
| C11—H11 | 0.9500 | C23—H23 | 0.9500 |
| C11—C12 | 1.3926 (18) | C23—C24 | 1.385 (2) |
| C12—C13 | 1.387 (2) | C24—H24 | 0.9500 |
| C12—C16 | 1.500 (2) | C24—C25 | 1.383 (2) |
| C13—H13 | 0.9500 | C25—H25 | 0.9500 |
| C13—C14 | 1.382 (2) | C26—H26A | 0.9800 |
| C14—H14 | 0.9500 | C26—H26B | 0.9800 |
| C14—C15 | 1.3864 (19) | C26—H26C | 0.9800 |
| N1i—Mn1—N1 | 180.0 | N11—C15—H15 | 118.6 |
| N1—Mn1—N11i | 91.56 (4) | C14—C15—H15 | 118.6 |
| N1—Mn1—N11 | 88.44 (4) | C12—C16—H16A | 109.5 |
| N1i—Mn1—N11i | 88.44 (4) | C12—C16—H16B | 109.5 |
| N1i—Mn1—N11 | 91.56 (4) | C12—C16—H16C | 109.5 |
| N1i—Mn1—N21 | 90.37 (4) | H16A—C16—H16B | 109.5 |
| N1—Mn1—N21i | 90.37 (4) | H16A—C16—H16C | 109.5 |
| N1i—Mn1—N21i | 89.63 (4) | H16B—C16—H16C | 109.5 |
| N1—Mn1—N21 | 89.63 (4) | C21—N21—Mn1 | 121.88 (8) |
| N11—Mn1—N11i | 180.00 (5) | C25—N21—Mn1 | 120.41 (9) |
| N21—Mn1—N11 | 89.06 (4) | C25—N21—C21 | 117.59 (11) |
| N21i—Mn1—N11 | 90.94 (4) | N21—C21—H21 | 118.1 |
| N21—Mn1—N11i | 90.94 (4) | N21—C21—C22 | 123.88 (12) |
| N21i—Mn1—N11i | 89.06 (4) | C22—C21—H21 | 118.1 |
| N21—Mn1—N21i | 180.0 | C21—C22—C26 | 120.82 (13) |
| N1—C1—S1 | 177.78 (12) | C23—C22—C21 | 117.08 (13) |
| C1—N1—Mn1 | 153.96 (10) | C23—C22—C26 | 122.10 (13) |
| C11—N11—Mn1 | 120.95 (9) | C22—C23—H23 | 120.2 |
| C11—N11—C15 | 117.23 (11) | C24—C23—C22 | 119.68 (12) |
| C15—N11—Mn1 | 121.61 (9) | C24—C23—H23 | 120.2 |
| N11—C11—H11 | 118.0 | C23—C24—H24 | 120.5 |
| N11—C11—C12 | 124.05 (13) | C25—C24—C23 | 118.92 (13) |
| C12—C11—H11 | 118.0 | C25—C24—H24 | 120.5 |
| C11—C12—C16 | 120.16 (13) | N21—C25—C24 | 122.79 (13) |
| C13—C12—C11 | 117.41 (13) | N21—C25—H25 | 118.6 |
| C13—C12—C16 | 122.41 (13) | C24—C25—H25 | 118.6 |
| C12—C13—H13 | 120.2 | C22—C26—H26A | 109.5 |
| C14—C13—C12 | 119.58 (12) | C22—C26—H26B | 109.5 |
| C14—C13—H13 | 120.2 | C22—C26—H26C | 109.5 |
| C13—C14—H14 | 120.6 | H26A—C26—H26B | 109.5 |
| C13—C14—C15 | 118.88 (13) | H26A—C26—H26C | 109.5 |
| C15—C14—H14 | 120.6 | H26B—C26—H26C | 109.5 |
| N11—C15—C14 | 122.84 (13) |
Symmetry code: (i) −x+1, −y+1, −z+1.
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)manganese(II) (1) . Hydrogen-bond geometry (Å, º)
| D—H···A | D—H | H···A | D···A | D—H···A |
| C11—H11···N1i | 0.95 | 2.60 | 3.2484 (17) | 126 |
| C15—H15···S1ii | 0.95 | 3.00 | 3.5588 (14) | 119 |
| C15—H15···N1 | 0.95 | 2.52 | 3.1535 (17) | 125 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, y, −z+3/2.
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)iron(II) (2) . Crystal data
| [Fe(NCS)2(C6H7N)4] | Dx = 1.350 Mg m−3 |
| Mr = 544.51 | Cu Kα radiation, λ = 1.54184 Å |
| Orthorhombic, Pbcn | Cell parameters from 17643 reflections |
| a = 17.3733 (1) Å | θ = 2.6–79.3° |
| b = 8.94119 (5) Å | µ = 6.17 mm−1 |
| c = 17.24862 (10) Å | T = 100 K |
| V = 2679.37 (3) Å3 | Prism, intense colourless |
| Z = 4 | 0.16 × 0.15 × 0.15 mm |
| F(000) = 1136 |
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)iron(II) (2) . Data collection
| XtaLAB Synergy, Dualflex, HyPix diffractometer | 2875 independent reflections |
| Radiation source: micro-focus sealed X-ray tube, PhotonJet (Cu) X-ray Source | 2804 reflections with I > 2σ(I) |
| Mirror monochromator | Rint = 0.020 |
| Detector resolution: 10.0000 pixels mm-1 | θmax = 79.8°, θmin = 5.1° |
| ω scans | h = −22→22 |
| Absorption correction: multi-scan (CrysalisPro; Rigaku OD, 2021) | k = −11→7 |
| Tmin = 0.555, Tmax = 1.000 | l = −22→20 |
| 22225 measured reflections |
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)iron(II) (2) . Refinement
| Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
| Least-squares matrix: full | H-atom parameters constrained |
| R[F2 > 2σ(F2)] = 0.026 | w = 1/[σ2(Fo2) + (0.0401P)2 + 1.5203P] where P = (Fo2 + 2Fc2)/3 |
| wR(F2) = 0.073 | (Δ/σ)max = 0.001 |
| S = 1.06 | Δρmax = 0.39 e Å−3 |
| 2875 reflections | Δρmin = −0.28 e Å−3 |
| 163 parameters | Extinction correction: SHELXL2016/6 (Sheldrick 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
| 0 restraints | Extinction coefficient: 0.00049 (7) |
| Primary atom site location: dual |
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)iron(II) (2) . Special details
| 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. |
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)iron(II) (2) . Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
| x | y | z | Uiso*/Ueq | ||
| Fe1 | 0.500000 | 0.500000 | 0.500000 | 0.01130 (10) | |
| S1 | 0.38206 (2) | 0.28452 (4) | 0.72572 (2) | 0.02425 (11) | |
| C1 | 0.43143 (7) | 0.32807 (13) | 0.64874 (7) | 0.0156 (2) | |
| N1 | 0.46454 (6) | 0.36130 (12) | 0.59232 (6) | 0.0167 (2) | |
| N11 | 0.62142 (6) | 0.40757 (12) | 0.51376 (6) | 0.0149 (2) | |
| C11 | 0.67967 (7) | 0.45813 (14) | 0.46972 (7) | 0.0177 (2) | |
| H11 | 0.667825 | 0.526986 | 0.429511 | 0.021* | |
| C12 | 0.75625 (7) | 0.41613 (15) | 0.47922 (8) | 0.0191 (3) | |
| C13 | 0.77283 (7) | 0.31360 (15) | 0.53734 (8) | 0.0219 (3) | |
| H13 | 0.824265 | 0.281211 | 0.545588 | 0.026* | |
| C14 | 0.71377 (8) | 0.25904 (15) | 0.58315 (8) | 0.0220 (3) | |
| H14 | 0.724078 | 0.188658 | 0.623079 | 0.026* | |
| C15 | 0.63926 (7) | 0.30874 (14) | 0.56985 (7) | 0.0175 (2) | |
| H15 | 0.599047 | 0.271369 | 0.601743 | 0.021* | |
| C16 | 0.81754 (8) | 0.48373 (17) | 0.42911 (10) | 0.0285 (3) | |
| H16A | 0.806439 | 0.461886 | 0.374566 | 0.043* | |
| H16B | 0.867663 | 0.441242 | 0.443056 | 0.043* | |
| H16C | 0.818606 | 0.592272 | 0.436935 | 0.043* | |
| N21 | 0.52872 (6) | 0.67812 (12) | 0.58534 (6) | 0.0151 (2) | |
| C21 | 0.56858 (7) | 0.64878 (14) | 0.65039 (7) | 0.0162 (2) | |
| H21 | 0.580676 | 0.547467 | 0.661651 | 0.019* | |
| C22 | 0.59325 (8) | 0.75852 (15) | 0.70240 (7) | 0.0188 (3) | |
| C23 | 0.57244 (8) | 0.90588 (15) | 0.68632 (8) | 0.0222 (3) | |
| H23 | 0.587559 | 0.984287 | 0.720223 | 0.027* | |
| C24 | 0.52958 (8) | 0.93723 (14) | 0.62059 (8) | 0.0215 (3) | |
| H24 | 0.514030 | 1.036811 | 0.609476 | 0.026* | |
| C25 | 0.50971 (7) | 0.82099 (14) | 0.57126 (8) | 0.0182 (3) | |
| H25 | 0.481440 | 0.843481 | 0.525582 | 0.022* | |
| C26 | 0.63958 (9) | 0.71736 (17) | 0.77282 (8) | 0.0274 (3) | |
| H26A | 0.689042 | 0.769994 | 0.771510 | 0.041* | |
| H26B | 0.648640 | 0.609178 | 0.773221 | 0.041* | |
| H26C | 0.611273 | 0.746064 | 0.819661 | 0.041* |
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)iron(II) (2) . Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Fe1 | 0.01186 (15) | 0.01149 (16) | 0.01054 (16) | −0.00048 (9) | 0.00004 (9) | 0.00100 (9) |
| S1 | 0.03164 (19) | 0.02224 (18) | 0.01886 (17) | −0.00132 (13) | 0.00886 (13) | 0.00403 (12) |
| C1 | 0.0169 (6) | 0.0121 (5) | 0.0178 (6) | 0.0006 (4) | −0.0026 (4) | −0.0002 (4) |
| N1 | 0.0174 (5) | 0.0168 (5) | 0.0159 (5) | −0.0005 (4) | 0.0002 (4) | 0.0032 (4) |
| N11 | 0.0149 (5) | 0.0147 (5) | 0.0151 (5) | 0.0006 (4) | −0.0013 (4) | −0.0015 (4) |
| C11 | 0.0176 (6) | 0.0168 (6) | 0.0185 (6) | 0.0003 (5) | −0.0004 (5) | 0.0002 (5) |
| C12 | 0.0157 (6) | 0.0190 (6) | 0.0227 (6) | −0.0008 (5) | 0.0006 (5) | −0.0026 (5) |
| C13 | 0.0153 (6) | 0.0228 (6) | 0.0276 (7) | 0.0027 (5) | −0.0050 (5) | −0.0014 (5) |
| C14 | 0.0217 (6) | 0.0218 (6) | 0.0224 (6) | 0.0039 (5) | −0.0045 (5) | 0.0036 (5) |
| C15 | 0.0185 (6) | 0.0171 (6) | 0.0168 (6) | −0.0001 (5) | −0.0012 (5) | 0.0003 (5) |
| C16 | 0.0209 (7) | 0.0325 (8) | 0.0319 (8) | −0.0001 (6) | 0.0060 (6) | 0.0019 (6) |
| N21 | 0.0153 (5) | 0.0147 (5) | 0.0155 (5) | −0.0007 (4) | 0.0012 (4) | −0.0012 (4) |
| C21 | 0.0174 (6) | 0.0160 (6) | 0.0151 (6) | −0.0011 (5) | 0.0006 (4) | −0.0010 (4) |
| C22 | 0.0209 (6) | 0.0194 (6) | 0.0161 (6) | −0.0036 (5) | 0.0019 (5) | −0.0031 (5) |
| C23 | 0.0265 (6) | 0.0178 (6) | 0.0222 (6) | −0.0051 (5) | 0.0041 (5) | −0.0060 (5) |
| C24 | 0.0241 (6) | 0.0130 (6) | 0.0275 (7) | −0.0004 (5) | 0.0042 (5) | −0.0008 (5) |
| C25 | 0.0174 (6) | 0.0166 (6) | 0.0205 (6) | 0.0008 (5) | 0.0008 (5) | 0.0013 (5) |
| C26 | 0.0352 (8) | 0.0273 (8) | 0.0198 (7) | −0.0040 (6) | −0.0065 (6) | −0.0044 (5) |
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)iron(II) (2) . Geometric parameters (Å, º)
| Fe1—N1i | 2.1103 (10) | C15—H15 | 0.9500 |
| Fe1—N1 | 2.1103 (10) | C16—H16A | 0.9800 |
| Fe1—N11i | 2.2780 (10) | C16—H16B | 0.9800 |
| Fe1—N11 | 2.2779 (10) | C16—H16C | 0.9800 |
| Fe1—N21 | 2.2253 (10) | N21—C21 | 1.3444 (16) |
| Fe1—N21i | 2.2253 (10) | N21—C25 | 1.3416 (16) |
| S1—C1 | 1.6279 (13) | C21—H21 | 0.9500 |
| C1—N1 | 1.1688 (17) | C21—C22 | 1.3968 (17) |
| N11—C11 | 1.3436 (16) | C22—C23 | 1.3942 (19) |
| N11—C15 | 1.3464 (16) | C22—C26 | 1.5030 (19) |
| C11—H11 | 0.9500 | C23—H23 | 0.9500 |
| C11—C12 | 1.3922 (18) | C23—C24 | 1.385 (2) |
| C12—C13 | 1.3887 (19) | C24—H24 | 0.9500 |
| C12—C16 | 1.4987 (19) | C24—C25 | 1.3868 (18) |
| C13—H13 | 0.9500 | C25—H25 | 0.9500 |
| C13—C14 | 1.3838 (19) | C26—H26A | 0.9800 |
| C14—H14 | 0.9500 | C26—H26B | 0.9800 |
| C14—C15 | 1.3878 (18) | C26—H26C | 0.9800 |
| N1i—Fe1—N1 | 180.0 | N11—C15—H15 | 118.5 |
| N1—Fe1—N11i | 91.23 (4) | C14—C15—H15 | 118.5 |
| N1—Fe1—N11 | 88.77 (4) | C12—C16—H16A | 109.5 |
| N1i—Fe1—N11i | 88.77 (4) | C12—C16—H16B | 109.5 |
| N1i—Fe1—N11 | 91.23 (4) | C12—C16—H16C | 109.5 |
| N1i—Fe1—N21 | 90.75 (4) | H16A—C16—H16B | 109.5 |
| N1—Fe1—N21i | 90.75 (4) | H16A—C16—H16C | 109.5 |
| N1i—Fe1—N21i | 89.25 (4) | H16B—C16—H16C | 109.5 |
| N1—Fe1—N21 | 89.25 (4) | C21—N21—Fe1 | 121.87 (8) |
| N11—Fe1—N11i | 180.00 (5) | C25—N21—Fe1 | 120.44 (9) |
| N21—Fe1—N11 | 89.03 (4) | C25—N21—C21 | 117.62 (11) |
| N21i—Fe1—N11 | 90.97 (4) | N21—C21—H21 | 118.1 |
| N21—Fe1—N11i | 90.97 (4) | N21—C21—C22 | 123.85 (12) |
| N21i—Fe1—N11i | 89.03 (4) | C22—C21—H21 | 118.1 |
| N21—Fe1—N21i | 180.00 (4) | C21—C22—C26 | 120.76 (12) |
| N1—C1—S1 | 177.62 (12) | C23—C22—C21 | 117.16 (12) |
| C1—N1—Fe1 | 157.12 (10) | C23—C22—C26 | 122.08 (12) |
| C11—N11—Fe1 | 121.10 (8) | C22—C23—H23 | 120.2 |
| C11—N11—C15 | 116.97 (11) | C24—C23—C22 | 119.58 (12) |
| C15—N11—Fe1 | 121.75 (8) | C24—C23—H23 | 120.2 |
| N11—C11—H11 | 117.9 | C23—C24—H24 | 120.5 |
| N11—C11—C12 | 124.24 (12) | C23—C24—C25 | 118.97 (12) |
| C12—C11—H11 | 117.9 | C25—C24—H24 | 120.5 |
| C11—C12—C16 | 120.16 (12) | N21—C25—C24 | 122.77 (12) |
| C13—C12—C11 | 117.46 (12) | N21—C25—H25 | 118.6 |
| C13—C12—C16 | 122.36 (12) | C24—C25—H25 | 118.6 |
| C12—C13—H13 | 120.3 | C22—C26—H26A | 109.5 |
| C14—C13—C12 | 119.41 (12) | C22—C26—H26B | 109.5 |
| C14—C13—H13 | 120.3 | C22—C26—H26C | 109.5 |
| C13—C14—H14 | 120.5 | H26A—C26—H26B | 109.5 |
| C13—C14—C15 | 118.97 (12) | H26A—C26—H26C | 109.5 |
| C15—C14—H14 | 120.5 | H26B—C26—H26C | 109.5 |
| N11—C15—C14 | 122.94 (12) |
Symmetry code: (i) −x+1, −y+1, −z+1.
Tetrakis(3-methylpyridine-κN)bis(isothiocyanato-κN)iron(II) (2) . Hydrogen-bond geometry (Å, º)
| D—H···A | D—H | H···A | D···A | D—H···A |
| C11—H11···N1i | 0.95 | 2.54 | 3.1668 (16) | 124 |
| C15—H15···S1ii | 0.95 | 3.00 | 3.5523 (13) | 119 |
| C15—H15···N1 | 0.95 | 2.48 | 3.0961 (16) | 123 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, y, −z+3/2.
Funding Statement
Financial support by the State of Schleswig-Holstein and the Deutsche Forschungsgemeinschaft is gratefully acknowledged.
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Associated Data
This section collects any data citations, data availability statements, or supplementary materials included in this article.
Supplementary Materials
Figure S1. IR spectrum of compound 1. The value of the CN-stretching vibration is given. DOI: 10.1107/S2056989022006491/hb8024sup4.png
Figure S2. IR spectrum of compound 2. The value of the CN-stretching vibration is given. DOI: 10.1107/S2056989022006491/hb8024sup5.png
Figure S3. TG-DTA curve of compound 1 measured with 4 degC/min in an nitrogen atmosphere. DOI: 10.1107/S2056989022006491/hb8024sup6.png
Figure S4. TG-DTA curve of compound 2 measured with 4 degC/min in an nitrogen atmosphere. DOI: 10.1107/S2056989022006491/hb8024sup7.png
Figure S5. Experimental XRPD pattern of the product obtained after the first mass loss in a TG measurement of compound 1 (top) and calculated powder pattern of Cd(NCS)2(3-methylpyridine)2 (bottom). DOI: 10.1107/S2056989022006491/hb8024sup8.jpg
Crystal structure: contains datablock(s) 1, 2. DOI: 10.1107/S2056989022006491/hb8024sup1.cif
Structure factors: contains datablock(s) 1. DOI: 10.1107/S2056989022006491/hb80241sup2.hkl
Structure factors: contains datablock(s) 2. DOI: 10.1107/S2056989022006491/hb80242sup3.hkl
Additional supporting information: crystallographic information; 3D view; checkCIF report