Acta Cryst. (2013). E69, m33 [ doi:10.1107/S1600536812049574 ]
![[kappa]](/logos/entities/kappa_rmgif.gif)
N)ferrate(III) monohydrateIn the title compound, (C7H11N2)3[Fe(NCS)6]·H2O, the FeIII cation is coordinated by six terminal N-bonded thiocyanate anions into a discrete threefold negatively charged complex. Charge balance is achieved by three protonated 4-(dimethylamino)pyridine cations. The asymmetric unit consists of one FeIII cation, six thiocyanate anions, three 4-(dimethylamino)pyridinium cations and one water molecule, all of them located in general positions.
FeCl2.4H2O and N,N'-dimethylaminopyridine were obtained from Sigma Aldrich. KNCS are obtained from Alfa Aesar. 0.3 mmol (59.6 mg) FeCl2.4H2O, 0.6 mmol (58.3 mg) KNCS and 0.15 mmol (18.3 mg) dimethylaminopyridine were reacted with 1 mL H2O in a snap cap vial. After one week red colored block-shaped single crystals of the title compound were obtained.
All C-H and N-H H atoms were located in difference map but were positioned with idealized geometry (methyl H atoms allowed to rotate but not to tip) and were refined isotropic with Uiso(H) = 1.2 Ueq(C, N) (1.5 for the methyl H atoms) using a riding model with Caromatic = 0.95 Å, CmethylH = 0.98 Å and N—H = 0.88 Å. The O-H H were located in difference map, their bond lengths were set to ideal values and finally they were refined isotropic with Uiso(H) = 1.5 Ueq(O) using a riding model with O-H = 0.84 Å.
Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA (Stoe & Cie, 2008); data reduction: X-AREA (Stoe & Cie, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2012); software used to prepare material for publication: XCIF in SHELXTL (Sheldrick, 2008).
![[Figure 1]](./hp2051fig1thm.gif)
| Fig. 1. : Crystal structure of the title compound with labeling and displacement ellipsoids drawn at the 50% probability level. |
![[Figure 2]](./hp2051fig2thm.gif)
| Fig. 2. : Crystal structure of the title compound with view along the crystallographic c-axis. Intermolecular hydrogen bonding is shown as dashed lines. |
| (C7H11N2)3[Fe(NCS)6]·H2O | Z = 2 |
| Mr = 791.88 | F(000) = 822 |
| Triclinic, P1 | Dx = 1.382 Mg m−3 |
| Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
| a = 11.5780 (7) Å | Cell parameters from 13617 reflections |
| b = 11.7620 (7) Å | θ = 2.4–26.0° |
| c = 16.5450 (11) Å | µ = 0.77 mm−1 |
| α = 81.260 (7)° | T = 180 K |
| β = 71.550 (7)° | Block, red |
| γ = 62.950 (6)° | 0.13 × 0.08 × 0.06 mm |
| V = 1903.4 (2) Å3 |
| Stoe IPDS-1 diffractometer | 7356 independent reflections |
| Radiation source: fine-focus sealed tube | 4936 reflections with I > 2σ(I) |
| Graphite monochromator | Rint = 0.075 |
| phi scan | θmax = 26.0°, θmin = 2.4° |
| Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008) | h = −14→14 |
| Tmin = 0.808, Tmax = 0.947 | k = −14→14 |
| 13617 measured reflections | l = −20→20 |
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| R[F2 > 2σ(F2)] = 0.042 | H-atom parameters constrained |
| wR(F2) = 0.104 | w = 1/[σ2(Fo2) + (0.052P)2] where P = (Fo2 + 2Fc2)/3 |
| S = 0.95 | (Δ/σ)max = 0.001 |
| 7356 reflections | Δρmax = 0.34 e Å−3 |
| 431 parameters | Δρmin = −0.50 e Å−3 |
| 0 restraints | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
| Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0045 (11) |
| (C7H11N2)3[Fe(NCS)6]·H2O | γ = 62.950 (6)° |
| Mr = 791.88 | V = 1903.4 (2) Å3 |
| Triclinic, P1 | Z = 2 |
| a = 11.5780 (7) Å | Mo Kα radiation |
| b = 11.7620 (7) Å | µ = 0.77 mm−1 |
| c = 16.5450 (11) Å | T = 180 K |
| α = 81.260 (7)° | 0.13 × 0.08 × 0.06 mm |
| β = 71.550 (7)° |
| Stoe IPDS-1 diffractometer | 7356 independent reflections |
| Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008) | 4936 reflections with I > 2σ(I) |
| Tmin = 0.808, Tmax = 0.947 | Rint = 0.075 |
| 13617 measured reflections | θmax = 26.0° |
| R[F2 > 2σ(F2)] = 0.042 | H-atom parameters constrained |
| wR(F2) = 0.104 | Δρmax = 0.34 e Å−3 |
| S = 0.95 | Δρmin = −0.50 e Å−3 |
| 7356 reflections | Absolute structure: ? |
| 431 parameters | Flack parameter: ? |
| 0 restraints | Rogers parameter: ? |
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. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
| x | y | z | Uiso*/Ueq | ||
| Fe1 | 0.98269 (4) | 0.75134 (4) | 0.75439 (2) | 0.01991 (12) | |
| N1 | 1.1616 (3) | 0.7621 (3) | 0.68821 (16) | 0.0302 (6) | |
| C1 | 1.2706 (3) | 0.7490 (3) | 0.65317 (18) | 0.0254 (6) | |
| S1 | 1.42277 (9) | 0.72966 (11) | 0.60257 (6) | 0.0479 (2) | |
| N2 | 0.9072 (2) | 0.8295 (2) | 0.65142 (16) | 0.0281 (5) | |
| C2 | 0.8775 (3) | 0.8660 (3) | 0.58809 (18) | 0.0226 (6) | |
| S2 | 0.83393 (8) | 0.91910 (8) | 0.50092 (5) | 0.0360 (2) | |
| N3 | 0.8051 (3) | 0.7391 (3) | 0.82393 (16) | 0.0291 (6) | |
| C3 | 0.6995 (3) | 0.7518 (3) | 0.86786 (17) | 0.0250 (6) | |
| S3 | 0.55149 (8) | 0.77201 (10) | 0.93009 (5) | 0.0430 (2) | |
| N4 | 1.0601 (2) | 0.5739 (2) | 0.70384 (16) | 0.0276 (5) | |
| C4 | 1.0898 (3) | 0.4916 (3) | 0.65919 (17) | 0.0223 (6) | |
| S4 | 1.12768 (8) | 0.37586 (7) | 0.59908 (5) | 0.02920 (18) | |
| N5 | 1.0629 (2) | 0.6720 (2) | 0.85664 (16) | 0.0280 (5) | |
| C5 | 1.1078 (3) | 0.6329 (3) | 0.91418 (18) | 0.0243 (6) | |
| S5 | 1.17023 (8) | 0.57453 (8) | 0.99515 (5) | 0.0352 (2) | |
| N6 | 0.9021 (3) | 0.9292 (2) | 0.80598 (15) | 0.0279 (5) | |
| C6 | 0.8648 (3) | 1.0174 (3) | 0.84754 (17) | 0.0233 (6) | |
| S6 | 0.81802 (9) | 1.14057 (7) | 0.90350 (5) | 0.0349 (2) | |
| N10 | 0.8102 (3) | 0.6969 (2) | 1.06431 (16) | 0.0300 (6) | |
| H10 | 0.8080 | 0.6393 | 1.0374 | 0.036* | |
| C11 | 0.8352 (3) | 0.6680 (3) | 1.14068 (19) | 0.0287 (6) | |
| H11 | 0.8516 | 0.5851 | 1.1642 | 0.034* | |
| C12 | 0.8376 (3) | 0.7546 (3) | 1.18468 (17) | 0.0232 (6) | |
| H12 | 0.8539 | 0.7326 | 1.2390 | 0.028* | |
| C13 | 0.8157 (3) | 0.8783 (3) | 1.14994 (16) | 0.0198 (5) | |
| C14 | 0.7897 (3) | 0.9043 (3) | 1.06899 (18) | 0.0289 (6) | |
| H14 | 0.7731 | 0.9860 | 1.0432 | 0.035* | |
| C15 | 0.7884 (3) | 0.8131 (3) | 1.02853 (19) | 0.0310 (7) | |
| H15 | 0.7719 | 0.8313 | 0.9742 | 0.037* | |
| C16 | 0.8466 (3) | 0.9423 (3) | 1.27260 (18) | 0.0295 (6) | |
| H16A | 0.7616 | 0.9703 | 1.3185 | 0.044* | |
| H16B | 0.8965 | 0.9894 | 1.2756 | 0.044* | |
| H16C | 0.9012 | 0.8507 | 1.2789 | 0.044* | |
| C17 | 0.7972 (4) | 1.0927 (3) | 1.1516 (2) | 0.0345 (7) | |
| H17A | 0.8679 | 1.0823 | 1.0977 | 0.052* | |
| H17B | 0.8018 | 1.1450 | 1.1902 | 0.052* | |
| H17C | 0.7085 | 1.1347 | 1.1407 | 0.052* | |
| N11 | 0.8174 (2) | 0.9670 (2) | 1.19072 (15) | 0.0252 (5) | |
| N20 | 0.8066 (3) | 0.2006 (3) | 0.55337 (16) | 0.0324 (6) | |
| H20 | 0.8113 | 0.1424 | 0.5231 | 0.039* | |
| C21 | 0.7879 (3) | 0.3170 (3) | 0.51934 (19) | 0.0337 (7) | |
| H21 | 0.7819 | 0.3344 | 0.4625 | 0.040* | |
| C22 | 0.7775 (3) | 0.4096 (3) | 0.56454 (19) | 0.0290 (6) | |
| H22 | 0.7631 | 0.4915 | 0.5395 | 0.035* | |
| C23 | 0.7880 (3) | 0.3847 (3) | 0.64942 (17) | 0.0221 (6) | |
| C24 | 0.8093 (3) | 0.2608 (3) | 0.68218 (18) | 0.0247 (6) | |
| H24 | 0.8173 | 0.2392 | 0.7385 | 0.030* | |
| C25 | 0.8183 (3) | 0.1721 (3) | 0.6331 (2) | 0.0299 (7) | |
| H25 | 0.8331 | 0.0889 | 0.6556 | 0.036* | |
| C26 | 0.7592 (4) | 0.6008 (3) | 0.6599 (2) | 0.0384 (8) | |
| H26A | 0.8331 | 0.5927 | 0.6081 | 0.058* | |
| H26B | 0.7588 | 0.6519 | 0.7017 | 0.058* | |
| H26C | 0.6729 | 0.6429 | 0.6458 | 0.058* | |
| C27 | 0.8000 (3) | 0.4446 (3) | 0.78040 (19) | 0.0327 (7) | |
| H27A | 0.7285 | 0.4235 | 0.8192 | 0.049* | |
| H27B | 0.7979 | 0.5188 | 0.8020 | 0.049* | |
| H27C | 0.8880 | 0.3716 | 0.7768 | 0.049* | |
| N21 | 0.7785 (2) | 0.4741 (2) | 0.69564 (15) | 0.0253 (5) | |
| N30 | 0.4772 (3) | 0.3824 (4) | 0.7836 (2) | 0.0598 (10) | |
| H30 | 0.4722 | 0.4477 | 0.8067 | 0.072* | |
| C31 | 0.5092 (4) | 0.2694 (5) | 0.8242 (3) | 0.0573 (12) | |
| H31 | 0.5254 | 0.2614 | 0.8781 | 0.069* | |
| C32 | 0.5190 (3) | 0.1663 (4) | 0.7905 (2) | 0.0459 (9) | |
| H32 | 0.5446 | 0.0866 | 0.8199 | 0.055* | |
| C33 | 0.4912 (3) | 0.1771 (3) | 0.7116 (2) | 0.0328 (7) | |
| C34 | 0.4594 (3) | 0.2978 (3) | 0.6703 (2) | 0.0399 (8) | |
| H34 | 0.4428 | 0.3095 | 0.6162 | 0.048* | |
| C35 | 0.4524 (4) | 0.3966 (4) | 0.7073 (3) | 0.0530 (10) | |
| H35 | 0.4298 | 0.4773 | 0.6792 | 0.064* | |
| C36 | 0.4696 (4) | 0.0904 (4) | 0.5952 (2) | 0.0456 (9) | |
| H36A | 0.5426 | 0.1023 | 0.5505 | 0.068* | |
| H36B | 0.3832 | 0.1638 | 0.5954 | 0.068* | |
| H36C | 0.4665 | 0.0124 | 0.5842 | 0.068* | |
| C37 | 0.5321 (4) | −0.0459 (4) | 0.7194 (3) | 0.0544 (10) | |
| H37A | 0.4772 | −0.0370 | 0.7790 | 0.082* | |
| H37B | 0.6279 | −0.0837 | 0.7172 | 0.082* | |
| H37C | 0.5163 | −0.1014 | 0.6898 | 0.082* | |
| N31 | 0.4946 (3) | 0.0793 (3) | 0.67822 (18) | 0.0371 (6) | |
| O1 | 0.4555 (3) | 0.5701 (4) | 0.8757 (3) | 0.0986 (15) | |
| H1O1 | 0.4927 | 0.6104 | 0.8866 | 0.148* | |
| H2O1 | 0.4004 | 0.5649 | 0.9218 | 0.148* |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Fe1 | 0.0247 (2) | 0.0191 (2) | 0.0198 (2) | −0.01218 (16) | −0.00614 (15) | −0.00240 (14) |
| N1 | 0.0341 (14) | 0.0365 (15) | 0.0283 (13) | −0.0208 (12) | −0.0074 (11) | −0.0083 (11) |
| C1 | 0.0323 (16) | 0.0266 (15) | 0.0241 (14) | −0.0169 (12) | −0.0104 (12) | 0.0002 (11) |
| S1 | 0.0299 (4) | 0.0642 (6) | 0.0518 (5) | −0.0269 (4) | −0.0040 (4) | −0.0013 (5) |
| N2 | 0.0338 (13) | 0.0265 (13) | 0.0273 (13) | −0.0148 (11) | −0.0110 (11) | 0.0017 (10) |
| C2 | 0.0217 (13) | 0.0208 (14) | 0.0264 (15) | −0.0090 (11) | −0.0067 (11) | −0.0044 (11) |
| S2 | 0.0438 (4) | 0.0392 (5) | 0.0268 (4) | −0.0141 (4) | −0.0178 (3) | −0.0017 (3) |
| N3 | 0.0332 (13) | 0.0349 (15) | 0.0273 (13) | −0.0215 (11) | −0.0065 (11) | −0.0043 (11) |
| C3 | 0.0336 (16) | 0.0305 (15) | 0.0203 (13) | −0.0187 (13) | −0.0124 (12) | −0.0001 (11) |
| S3 | 0.0322 (4) | 0.0695 (6) | 0.0321 (4) | −0.0292 (4) | −0.0023 (3) | −0.0044 (4) |
| N4 | 0.0339 (13) | 0.0223 (12) | 0.0309 (13) | −0.0154 (11) | −0.0085 (10) | −0.0027 (11) |
| C4 | 0.0268 (13) | 0.0198 (14) | 0.0214 (13) | −0.0117 (11) | −0.0074 (11) | 0.0029 (11) |
| S4 | 0.0450 (4) | 0.0209 (4) | 0.0222 (3) | −0.0143 (3) | −0.0089 (3) | −0.0030 (3) |
| N5 | 0.0342 (13) | 0.0249 (13) | 0.0293 (13) | −0.0135 (11) | −0.0136 (11) | 0.0004 (10) |
| C5 | 0.0279 (14) | 0.0224 (14) | 0.0271 (15) | −0.0139 (12) | −0.0066 (12) | −0.0058 (12) |
| S5 | 0.0428 (4) | 0.0408 (5) | 0.0301 (4) | −0.0193 (4) | −0.0193 (3) | 0.0007 (3) |
| N6 | 0.0359 (13) | 0.0257 (13) | 0.0258 (12) | −0.0173 (11) | −0.0066 (10) | −0.0022 (10) |
| C6 | 0.0322 (14) | 0.0204 (14) | 0.0190 (13) | −0.0138 (12) | −0.0069 (11) | 0.0020 (11) |
| S6 | 0.0600 (5) | 0.0223 (4) | 0.0203 (4) | −0.0178 (4) | −0.0078 (3) | −0.0022 (3) |
| N10 | 0.0403 (14) | 0.0309 (14) | 0.0256 (13) | −0.0194 (11) | −0.0085 (10) | −0.0081 (11) |
| C11 | 0.0323 (15) | 0.0252 (15) | 0.0304 (15) | −0.0148 (12) | −0.0068 (12) | −0.0013 (12) |
| C12 | 0.0280 (14) | 0.0235 (14) | 0.0202 (13) | −0.0132 (11) | −0.0074 (11) | 0.0019 (11) |
| C13 | 0.0214 (12) | 0.0244 (14) | 0.0160 (12) | −0.0131 (11) | −0.0026 (10) | −0.0015 (10) |
| C14 | 0.0411 (16) | 0.0313 (16) | 0.0210 (14) | −0.0206 (14) | −0.0116 (12) | 0.0031 (12) |
| C15 | 0.0397 (16) | 0.0410 (18) | 0.0215 (14) | −0.0240 (14) | −0.0113 (12) | 0.0018 (13) |
| C16 | 0.0463 (17) | 0.0311 (16) | 0.0231 (14) | −0.0233 (14) | −0.0173 (13) | 0.0042 (12) |
| C17 | 0.0528 (19) | 0.0267 (16) | 0.0351 (17) | −0.0228 (15) | −0.0206 (15) | 0.0050 (13) |
| N11 | 0.0372 (13) | 0.0233 (12) | 0.0227 (12) | −0.0169 (11) | −0.0136 (10) | 0.0027 (10) |
| N20 | 0.0379 (14) | 0.0362 (15) | 0.0299 (13) | −0.0198 (12) | −0.0073 (11) | −0.0119 (11) |
| C21 | 0.0413 (17) | 0.046 (2) | 0.0214 (14) | −0.0245 (15) | −0.0095 (12) | −0.0028 (13) |
| C22 | 0.0389 (16) | 0.0320 (16) | 0.0243 (14) | −0.0217 (14) | −0.0130 (12) | 0.0068 (12) |
| C23 | 0.0216 (13) | 0.0240 (14) | 0.0226 (13) | −0.0119 (11) | −0.0049 (10) | −0.0020 (11) |
| C24 | 0.0274 (14) | 0.0264 (15) | 0.0215 (13) | −0.0136 (12) | −0.0055 (11) | −0.0001 (11) |
| C25 | 0.0332 (15) | 0.0250 (15) | 0.0342 (16) | −0.0156 (13) | −0.0060 (12) | −0.0051 (13) |
| C26 | 0.056 (2) | 0.0208 (15) | 0.050 (2) | −0.0160 (15) | −0.0328 (17) | 0.0054 (14) |
| C27 | 0.0446 (18) | 0.0310 (16) | 0.0286 (15) | −0.0173 (14) | −0.0153 (13) | −0.0037 (13) |
| N21 | 0.0325 (12) | 0.0214 (12) | 0.0271 (12) | −0.0126 (10) | −0.0135 (10) | −0.0003 (10) |
| N30 | 0.0410 (18) | 0.078 (3) | 0.065 (2) | −0.0339 (18) | 0.0046 (16) | −0.029 (2) |
| C31 | 0.039 (2) | 0.098 (4) | 0.037 (2) | −0.035 (2) | −0.0031 (16) | −0.005 (2) |
| C32 | 0.0353 (17) | 0.067 (3) | 0.0351 (18) | −0.0254 (18) | −0.0102 (14) | 0.0108 (17) |
| C33 | 0.0196 (13) | 0.0413 (18) | 0.0308 (16) | −0.0127 (13) | −0.0040 (11) | 0.0096 (13) |
| C34 | 0.0363 (17) | 0.0393 (19) | 0.0416 (19) | −0.0166 (15) | −0.0113 (14) | 0.0073 (15) |
| C35 | 0.0395 (19) | 0.047 (2) | 0.068 (3) | −0.0205 (18) | −0.0082 (18) | 0.002 (2) |
| C36 | 0.0387 (18) | 0.050 (2) | 0.043 (2) | −0.0155 (17) | −0.0080 (15) | −0.0057 (17) |
| C37 | 0.043 (2) | 0.037 (2) | 0.069 (3) | −0.0123 (17) | −0.0146 (18) | 0.0185 (19) |
| N31 | 0.0301 (13) | 0.0305 (14) | 0.0393 (15) | −0.0082 (11) | −0.0050 (11) | 0.0044 (12) |
| O1 | 0.066 (2) | 0.123 (3) | 0.122 (3) | −0.065 (2) | 0.020 (2) | −0.064 (3) |
| Fe1—N4 | 2.052 (2) | N20—H20 | 0.8800 |
| Fe1—N6 | 2.059 (2) | C21—C22 | 1.353 (4) |
| Fe1—N2 | 2.061 (3) | C21—H21 | 0.9500 |
| Fe1—N1 | 2.065 (3) | C22—C23 | 1.422 (4) |
| Fe1—N3 | 2.072 (3) | C22—H22 | 0.9500 |
| Fe1—N5 | 2.079 (2) | C23—N21 | 1.338 (4) |
| N1—C1 | 1.157 (4) | C23—C24 | 1.413 (4) |
| C1—S1 | 1.618 (3) | C24—C25 | 1.365 (4) |
| N2—C2 | 1.165 (4) | C24—H24 | 0.9500 |
| C2—S2 | 1.620 (3) | C25—H25 | 0.9500 |
| N3—C3 | 1.162 (4) | C26—N21 | 1.461 (4) |
| C3—S3 | 1.625 (3) | C26—H26A | 0.9800 |
| N4—C4 | 1.164 (4) | C26—H26B | 0.9800 |
| C4—S4 | 1.621 (3) | C26—H26C | 0.9800 |
| N5—C5 | 1.162 (4) | C27—N21 | 1.464 (4) |
| C5—S5 | 1.634 (3) | C27—H27A | 0.9800 |
| N6—C6 | 1.165 (4) | C27—H27B | 0.9800 |
| C6—S6 | 1.620 (3) | C27—H27C | 0.9800 |
| N10—C11 | 1.345 (4) | N30—C31 | 1.339 (6) |
| N10—C15 | 1.347 (4) | N30—C35 | 1.351 (6) |
| N10—H10 | 0.8800 | N30—H30 | 0.8800 |
| C11—C12 | 1.353 (4) | C31—C32 | 1.355 (7) |
| C11—H11 | 0.9500 | C31—H31 | 0.9500 |
| C12—C13 | 1.419 (4) | C32—C33 | 1.415 (5) |
| C12—H12 | 0.9500 | C32—H32 | 0.9500 |
| C13—N11 | 1.336 (4) | C33—N31 | 1.330 (5) |
| C13—C14 | 1.423 (4) | C33—C34 | 1.418 (5) |
| C14—C15 | 1.356 (4) | C34—C35 | 1.354 (6) |
| C14—H14 | 0.9500 | C34—H34 | 0.9500 |
| C15—H15 | 0.9500 | C35—H35 | 0.9500 |
| C16—N11 | 1.454 (4) | C36—N31 | 1.467 (5) |
| C16—H16A | 0.9800 | C36—H36A | 0.9800 |
| C16—H16B | 0.9800 | C36—H36B | 0.9800 |
| C16—H16C | 0.9800 | C36—H36C | 0.9800 |
| C17—N11 | 1.466 (4) | C37—N31 | 1.457 (5) |
| C17—H17A | 0.9800 | C37—H37A | 0.9800 |
| C17—H17B | 0.9800 | C37—H37B | 0.9800 |
| C17—H17C | 0.9800 | C37—H37C | 0.9800 |
| N20—C25 | 1.344 (4) | O1—H1O1 | 0.8400 |
| N20—C21 | 1.346 (4) | O1—H2O1 | 0.8401 |
| N4—Fe1—N6 | 179.11 (11) | N20—C21—H21 | 119.3 |
| N4—Fe1—N2 | 88.68 (10) | C22—C21—H21 | 119.3 |
| N6—Fe1—N2 | 91.24 (10) | C21—C22—C23 | 120.1 (3) |
| N4—Fe1—N1 | 89.09 (10) | C21—C22—H22 | 119.9 |
| N6—Fe1—N1 | 91.80 (10) | C23—C22—H22 | 119.9 |
| N2—Fe1—N1 | 90.15 (10) | N21—C23—C24 | 121.8 (3) |
| N4—Fe1—N3 | 91.19 (10) | N21—C23—C22 | 121.6 (3) |
| N6—Fe1—N3 | 87.92 (10) | C24—C23—C22 | 116.6 (3) |
| N2—Fe1—N3 | 91.48 (10) | C25—C24—C23 | 120.1 (3) |
| N1—Fe1—N3 | 178.35 (10) | C25—C24—H24 | 119.9 |
| N4—Fe1—N5 | 91.08 (10) | C23—C24—H24 | 119.9 |
| N6—Fe1—N5 | 89.02 (10) | N20—C25—C24 | 121.1 (3) |
| N2—Fe1—N5 | 178.77 (10) | N20—C25—H25 | 119.5 |
| N1—Fe1—N5 | 88.64 (10) | C24—C25—H25 | 119.5 |
| N3—Fe1—N5 | 89.73 (10) | N21—C26—H26A | 109.5 |
| C1—N1—Fe1 | 170.0 (3) | N21—C26—H26B | 109.5 |
| N1—C1—S1 | 178.9 (3) | H26A—C26—H26B | 109.5 |
| C2—N2—Fe1 | 173.1 (2) | N21—C26—H26C | 109.5 |
| N2—C2—S2 | 178.9 (3) | H26A—C26—H26C | 109.5 |
| C3—N3—Fe1 | 168.7 (2) | H26B—C26—H26C | 109.5 |
| N3—C3—S3 | 178.9 (3) | N21—C27—H27A | 109.5 |
| C4—N4—Fe1 | 162.8 (2) | N21—C27—H27B | 109.5 |
| N4—C4—S4 | 178.3 (3) | H27A—C27—H27B | 109.5 |
| C5—N5—Fe1 | 176.9 (2) | N21—C27—H27C | 109.5 |
| N5—C5—S5 | 178.4 (3) | H27A—C27—H27C | 109.5 |
| C6—N6—Fe1 | 167.6 (2) | H27B—C27—H27C | 109.5 |
| N6—C6—S6 | 177.9 (3) | C23—N21—C26 | 120.9 (2) |
| C11—N10—C15 | 120.8 (2) | C23—N21—C27 | 121.1 (2) |
| C11—N10—H10 | 119.6 | C26—N21—C27 | 117.7 (2) |
| C15—N10—H10 | 119.6 | C31—N30—C35 | 120.3 (4) |
| N10—C11—C12 | 121.4 (3) | C31—N30—H30 | 119.9 |
| N10—C11—H11 | 119.3 | C35—N30—H30 | 119.9 |
| C12—C11—H11 | 119.3 | N30—C31—C32 | 121.8 (4) |
| C11—C12—C13 | 120.2 (3) | N30—C31—H31 | 119.1 |
| C11—C12—H12 | 119.9 | C32—C31—H31 | 119.1 |
| C13—C12—H12 | 119.9 | C31—C32—C33 | 120.1 (4) |
| N11—C13—C12 | 122.5 (2) | C31—C32—H32 | 120.0 |
| N11—C13—C14 | 121.2 (3) | C33—C32—H32 | 120.0 |
| C12—C13—C14 | 116.3 (2) | N31—C33—C32 | 121.8 (3) |
| C15—C14—C13 | 120.4 (3) | N31—C33—C34 | 121.9 (3) |
| C15—C14—H14 | 119.8 | C32—C33—C34 | 116.3 (3) |
| C13—C14—H14 | 119.8 | C35—C34—C33 | 120.4 (4) |
| N10—C15—C14 | 120.9 (3) | C35—C34—H34 | 119.8 |
| N10—C15—H15 | 119.5 | C33—C34—H34 | 119.8 |
| C14—C15—H15 | 119.5 | N30—C35—C34 | 121.1 (4) |
| N11—C16—H16A | 109.5 | N30—C35—H35 | 119.4 |
| N11—C16—H16B | 109.5 | C34—C35—H35 | 119.4 |
| H16A—C16—H16B | 109.5 | N31—C36—H36A | 109.5 |
| N11—C16—H16C | 109.5 | N31—C36—H36B | 109.5 |
| H16A—C16—H16C | 109.5 | H36A—C36—H36B | 109.5 |
| H16B—C16—H16C | 109.5 | N31—C36—H36C | 109.5 |
| N11—C17—H17A | 109.5 | H36A—C36—H36C | 109.5 |
| N11—C17—H17B | 109.5 | H36B—C36—H36C | 109.5 |
| H17A—C17—H17B | 109.5 | N31—C37—H37A | 109.5 |
| N11—C17—H17C | 109.5 | N31—C37—H37B | 109.5 |
| H17A—C17—H17C | 109.5 | H37A—C37—H37B | 109.5 |
| H17B—C17—H17C | 109.5 | N31—C37—H37C | 109.5 |
| C13—N11—C16 | 122.4 (2) | H37A—C37—H37C | 109.5 |
| C13—N11—C17 | 120.6 (2) | H37B—C37—H37C | 109.5 |
| C16—N11—C17 | 116.9 (2) | C33—N31—C37 | 121.7 (3) |
| C25—N20—C21 | 120.7 (3) | C33—N31—C36 | 121.3 (3) |
| C25—N20—H20 | 119.6 | C37—N31—C36 | 116.8 (3) |
| C21—N20—H20 | 119.6 | H1O1—O1—H2O1 | 105.9 |
| N20—C21—C22 | 121.3 (3) |
We gratefully acknowledge financial support by the State of Schleswig-Holstein and the Deutsche Forschungsgemeinschaft (project 720/3-1). We thank Professor Dr Wolfgang Bensch for access to his experimental facility.
Boeckmann, J. & Näther, C. (2011). Dalton Trans. 39, 11019–11026.
Boeckmann, J. & Näther, C. (2012). Polyhedron, 31 587–595.
Brandenburg, K. (2012). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.
Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany.
Recently we have reported on the synthesis and characterization of coordination compounds based on transition metal thiocyanates and neutral N-donor co-ligands like e.g. pyridine (Boeckmann & Näther, 2011, 2012). To investigate the influence of the co-ligand we tried to prepare similar compounds with N,N'-dimethylaminopyridine. Therefore, we have reacted iron(II) chloride tetrahydrate with potassium thiocyanate and N,N'-dimethylaminopyridine in water, which lead to the formation of single crystals of the title compound by accident. To identify the product of this reaction a single crystal structure determination was performed.
The crystal structure of the title compound consists of discrete [Fe(NCS)6]3- anions, three N,N'dimethylaminopyridinium cations as well as one water molecule (Fig. 1). In the discrete complexes the iron(III) cations are coordinated by six thiocyanato anions within slightly distorted octahedra with distances in the range of 2.052 (2) Å to 2.079 (2) Å and angles ranging from 87.92 (10) ° to 91.80 (10) ° and from 178.35 (10) ° to 179.11 (10) ° (Tab. 1). The building blocks are connected via intermolecular N—H···S, N—H···O and O—H···S hydrogen bonding, in which the protonated N atom is involved (Tab. 2). These blocks are elongated in the direction of the crystallographic a-axis (Fig. 2).