Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807047460/zl2066sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807047460/zl2066Isup2.hkl |
CCDC reference: 667101
AgNO3 (0.51 g, 3.0 mmol), NH4SCN (0.68 g, 4.5 mmol) and ina (1.11 g, 4.5 mmol) were added to a stirred solution of FeCl3.6H2O (0.41 g, 1.5 mmol) in water. The mixture was stirred at room temperature for 12 h. The solution was filtered and the filtrate was left to evaporate slowly in air. After a few days, purple-red crystals suitable for X-ray diffraction analysis were obtained.
Water and N—H hydrogen atoms were located from the difference density Fourier maps and were refined with Uiso(H) = 1.5Ueq(O) and Uiso(H) = 1.2Ueq(N). All other H atoms were placed geometrically with C–H and O—H distances of 0.96 and 0.82 Å and Uiso(H) = 1.2Ueq(C) or 1.5Ueq(O). Hydroxyl H atoms were allowed to rotate to best fit the experimental electron density.
Isothiocyanate anions exhibit a large variety of different coordination modes towards metal cations and, partially due to this, they are widely used as versatile ligands in many areas of coordination chemistry (Li, Tong et al., 2004; Li, Zhao et al., 2004 and Li et al., 2007). Herein we describe the crystal structure of the iron(III) isothiocyanate complex [inaH]2[Fe(H2O)(NCS)5].2[ina] (ina = isonicotinic acid).
A thermal ellipsoid drawing of the complex with the atomic numbering scheme is shown in Fig. 1. The iron complex lies on a mirror plane with the six-coordinated FeIII ion, a coordinated water molecule and three of the five isothiocyanate ligands located directly within this plane (atoms Fe1, O1W, N1, C1, S1, N2, C2, S2, N4, C4 and S4). The coordination geometry around the FeIII ion is slightly distorted octahedral. All the isothiocyanate anions coordinate to the iron(III) center through the nitrogen atoms in a slightly bent mode with C—N—Fe angles in the range of 150.7 (5)–166.8 (5)°. The ina molecules and the protonated inaH+ cations interact with each other through N—H···O and O—H···O hydrogen bonds which leads to the formation of a 2-D layer perpendicular to the b axis. One of this sublayers is shown in Fig. 2. Each two of these layers sandwich another layer of {[Fe(H2O)(NCS)5]2-}n anions with which they interact via electrostatic attraction and O—H···O hydrogen bonds, resulting in sheets of triple-layers perpendicular to the b axis. One of these triple-layers is shown in Fig. 3.
For related compounds, see Li, Tong et al. (2004); Li, Zhao et al. (2004); Li et al. (2007).
Data collection: SMART (Siemens, 1996); cell refinement: SMART (Siemens, 1996) and SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996) and XPREP (Siemens, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1999); software used to prepare material for publication: SHELXTL (Bruker, 1999).
(C6H6NO2)2[Fe(NCS)5(H2O)]·2C6H5NO2 | F(000) = 1756 |
Mr = 858.72 | Dx = 1.519 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 6815 reflections |
a = 14.8713 (3) Å | θ = 1.9–25.1° |
b = 21.0882 (3) Å | µ = 0.74 mm−1 |
c = 11.9741 (2) Å | T = 297 K |
V = 3755.18 (11) Å3 | Prism, purple red |
Z = 4 | 0.36 × 0.30 × 0.20 mm |
Siemens SMART CCD diffractometer | 3405 independent reflections |
Radiation source: fine-focus sealed tube | 2589 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
φ and ω scans | θmax = 25.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −15→17 |
Tmin = 0.776, Tmax = 0.866 | k = −19→25 |
18247 measured reflections | l = −12→14 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.049 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.132 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.054P)2 + 5.0802P] where P = (Fo2 + 2Fc2)/3 |
3405 reflections | (Δ/σ)max < 0.001 |
265 parameters | Δρmax = 0.71 e Å−3 |
0 restraints | Δρmin = −0.62 e Å−3 |
(C6H6NO2)2[Fe(NCS)5(H2O)]·2C6H5NO2 | V = 3755.18 (11) Å3 |
Mr = 858.72 | Z = 4 |
Orthorhombic, Pnma | Mo Kα radiation |
a = 14.8713 (3) Å | µ = 0.74 mm−1 |
b = 21.0882 (3) Å | T = 297 K |
c = 11.9741 (2) Å | 0.36 × 0.30 × 0.20 mm |
Siemens SMART CCD diffractometer | 3405 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2589 reflections with I > 2σ(I) |
Tmin = 0.776, Tmax = 0.866 | Rint = 0.043 |
18247 measured reflections |
R[F2 > 2σ(F2)] = 0.049 | 0 restraints |
wR(F2) = 0.132 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | Δρmax = 0.71 e Å−3 |
3405 reflections | Δρmin = −0.62 e Å−3 |
265 parameters |
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 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 > σ(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 | 0.04898 (5) | 0.7500 | 0.46892 (6) | 0.0447 (2) | |
S1 | 0.35902 (12) | 0.7500 | 0.57736 (16) | 0.0711 (5) | |
S2 | −0.26880 (10) | 0.7500 | 0.44506 (14) | 0.0618 (4) | |
S3 | 0.11872 (8) | 0.53111 (5) | 0.42450 (10) | 0.0666 (3) | |
S4 | 0.08889 (14) | 0.7500 | 0.84926 (17) | 0.0966 (7) | |
N1 | 0.1841 (3) | 0.7500 | 0.4965 (4) | 0.0642 (13) | |
N2 | −0.0851 (3) | 0.7500 | 0.4331 (5) | 0.0666 (14) | |
N3 | 0.0549 (2) | 0.65311 (16) | 0.4608 (3) | 0.0571 (9) | |
N4 | 0.0261 (4) | 0.7500 | 0.6327 (4) | 0.0671 (14) | |
C1 | 0.2566 (4) | 0.7500 | 0.5337 (4) | 0.0492 (13) | |
C2 | −0.1609 (4) | 0.7500 | 0.4375 (4) | 0.0481 (13) | |
C3 | 0.0825 (3) | 0.6021 (2) | 0.4464 (3) | 0.0476 (9) | |
C4 | 0.0520 (4) | 0.7500 | 0.7235 (5) | 0.0577 (15) | |
O1W | 0.0739 (3) | 0.7500 | 0.2978 (3) | 0.0556 (11) | |
H1WA | 0.079 (3) | 0.718 (2) | 0.268 (4) | 0.083* | |
O11 | 0.08724 (13) | 0.63784 (11) | 0.1885 (2) | 0.0400 (6) | |
O12 | 0.13720 (17) | 0.57069 (15) | 0.0600 (2) | 0.0676 (9) | |
N11 | 0.41185 (19) | 0.61060 (15) | 0.2733 (3) | 0.0465 (8) | |
H11A | 0.468 (3) | 0.6149 (18) | 0.292 (3) | 0.056* | |
C11 | 0.1473 (2) | 0.60535 (16) | 0.1433 (3) | 0.0390 (8) | |
C12 | 0.24110 (19) | 0.60742 (15) | 0.1927 (3) | 0.0348 (7) | |
C13 | 0.3076 (2) | 0.56935 (17) | 0.1478 (3) | 0.0439 (9) | |
H13A | 0.2943 | 0.5423 | 0.0888 | 0.053* | |
C14 | 0.3928 (2) | 0.57152 (18) | 0.1900 (3) | 0.0500 (10) | |
H14A | 0.4374 | 0.5456 | 0.1603 | 0.060* | |
C15 | 0.3498 (2) | 0.64714 (18) | 0.3203 (3) | 0.0490 (9) | |
H15A | 0.3652 | 0.6735 | 0.3796 | 0.059* | |
C16 | 0.2630 (2) | 0.64613 (17) | 0.2814 (3) | 0.0451 (9) | |
H16A | 0.2192 | 0.6714 | 0.3147 | 0.054* | |
O21 | 0.48392 (16) | 0.57804 (13) | 0.5311 (2) | 0.0567 (7) | |
H21 | 0.5353 | 0.5759 | 0.5065 | 0.085* | |
O22 | 0.55326 (17) | 0.58175 (18) | 0.6951 (2) | 0.0807 (10) | |
N21 | 0.2356 (2) | 0.61800 (19) | 0.7871 (3) | 0.0648 (10) | |
H21A | 0.185 (3) | 0.622 (2) | 0.817 (4) | 0.078* | |
C21 | 0.4867 (2) | 0.58419 (18) | 0.6386 (3) | 0.0479 (9) | |
C22 | 0.3962 (2) | 0.59533 (15) | 0.6907 (3) | 0.0374 (8) | |
C23 | 0.3176 (2) | 0.58314 (18) | 0.6341 (3) | 0.0471 (9) | |
H23A | 0.3195 | 0.5671 | 0.5617 | 0.057* | |
C24 | 0.2371 (2) | 0.5946 (2) | 0.6843 (3) | 0.0600 (11) | |
H24A | 0.1837 | 0.5861 | 0.6469 | 0.072* | |
C25 | 0.3097 (3) | 0.6308 (2) | 0.8439 (3) | 0.0625 (11) | |
H25A | 0.3058 | 0.6477 | 0.9155 | 0.075* | |
C26 | 0.3918 (2) | 0.61910 (18) | 0.7975 (3) | 0.0505 (9) | |
H26A | 0.4442 | 0.6271 | 0.8376 | 0.061* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0430 (4) | 0.0435 (4) | 0.0475 (5) | 0.000 | 0.0058 (3) | 0.000 |
S1 | 0.0721 (11) | 0.0533 (9) | 0.0880 (12) | 0.000 | −0.0363 (9) | 0.000 |
S2 | 0.0435 (8) | 0.0693 (10) | 0.0727 (11) | 0.000 | −0.0010 (7) | 0.000 |
S3 | 0.0743 (8) | 0.0469 (6) | 0.0786 (8) | 0.0132 (5) | −0.0133 (6) | 0.0099 (5) |
S4 | 0.0857 (13) | 0.1384 (19) | 0.0659 (12) | 0.000 | −0.0134 (10) | 0.000 |
N1 | 0.052 (3) | 0.069 (3) | 0.071 (4) | 0.000 | −0.003 (3) | 0.000 |
N2 | 0.046 (3) | 0.070 (3) | 0.084 (4) | 0.000 | −0.002 (3) | 0.000 |
N3 | 0.071 (2) | 0.045 (2) | 0.055 (2) | −0.0017 (17) | 0.0016 (17) | 0.0027 (16) |
N4 | 0.083 (4) | 0.069 (3) | 0.049 (3) | 0.000 | 0.010 (3) | 0.000 |
C1 | 0.065 (4) | 0.040 (3) | 0.043 (3) | 0.000 | 0.001 (3) | 0.000 |
C2 | 0.055 (4) | 0.042 (3) | 0.047 (3) | 0.000 | 0.003 (3) | 0.000 |
C3 | 0.049 (2) | 0.053 (2) | 0.041 (2) | −0.0067 (19) | −0.0052 (16) | 0.0108 (17) |
C4 | 0.049 (3) | 0.060 (4) | 0.064 (4) | 0.000 | 0.012 (3) | 0.000 |
O1W | 0.078 (3) | 0.038 (2) | 0.050 (2) | 0.000 | 0.011 (2) | 0.000 |
O11 | 0.0217 (11) | 0.0482 (14) | 0.0502 (15) | 0.0011 (10) | 0.0022 (10) | −0.0036 (11) |
O12 | 0.0392 (15) | 0.085 (2) | 0.078 (2) | 0.0187 (14) | −0.0255 (14) | −0.0423 (17) |
N11 | 0.0213 (14) | 0.059 (2) | 0.059 (2) | −0.0046 (14) | −0.0074 (14) | 0.0054 (16) |
C11 | 0.0261 (16) | 0.046 (2) | 0.045 (2) | 0.0029 (15) | −0.0061 (15) | −0.0062 (16) |
C12 | 0.0229 (15) | 0.0407 (18) | 0.0407 (19) | −0.0011 (13) | −0.0005 (13) | −0.0001 (14) |
C13 | 0.0303 (17) | 0.051 (2) | 0.050 (2) | 0.0044 (15) | −0.0023 (16) | −0.0119 (17) |
C14 | 0.0283 (18) | 0.056 (2) | 0.066 (3) | 0.0076 (16) | 0.0033 (17) | −0.003 (2) |
C15 | 0.0357 (18) | 0.064 (2) | 0.048 (2) | 0.0000 (18) | −0.0113 (16) | −0.0103 (18) |
C16 | 0.0301 (17) | 0.058 (2) | 0.047 (2) | 0.0069 (16) | −0.0019 (15) | −0.0123 (17) |
O21 | 0.0323 (13) | 0.087 (2) | 0.0512 (17) | 0.0029 (13) | 0.0102 (11) | 0.0048 (14) |
O22 | 0.0307 (15) | 0.149 (3) | 0.0622 (19) | 0.0025 (16) | −0.0062 (14) | 0.0092 (19) |
N21 | 0.0378 (19) | 0.093 (3) | 0.064 (2) | 0.0102 (18) | 0.0123 (17) | −0.011 (2) |
C21 | 0.0315 (19) | 0.058 (2) | 0.054 (2) | −0.0050 (16) | 0.0036 (17) | 0.0099 (18) |
C22 | 0.0290 (17) | 0.0373 (18) | 0.046 (2) | −0.0035 (14) | 0.0001 (14) | 0.0040 (15) |
C23 | 0.0335 (18) | 0.064 (2) | 0.044 (2) | −0.0017 (17) | 0.0034 (16) | −0.0057 (18) |
C24 | 0.031 (2) | 0.092 (3) | 0.058 (3) | −0.001 (2) | −0.0012 (18) | −0.007 (2) |
C25 | 0.062 (3) | 0.074 (3) | 0.051 (2) | 0.003 (2) | 0.010 (2) | −0.018 (2) |
C26 | 0.043 (2) | 0.060 (2) | 0.049 (2) | −0.0076 (17) | −0.0031 (17) | −0.0084 (18) |
Fe1—N4 | 1.991 (5) | C12—C13 | 1.383 (4) |
Fe1—N1 | 2.037 (5) | C13—C14 | 1.365 (5) |
Fe1—N2 | 2.039 (5) | C13—H13A | 0.9300 |
Fe1—N3 | 2.047 (3) | C14—H14A | 0.9300 |
Fe1—N3i | 2.047 (3) | C15—C16 | 1.373 (5) |
Fe1—O1W | 2.082 (4) | C15—H15A | 0.9300 |
S1—C1 | 1.610 (6) | C16—H16A | 0.9300 |
S2—C2 | 1.607 (6) | O21—C21 | 1.294 (4) |
S3—C3 | 1.613 (4) | O21—H21 | 0.8200 |
S4—C4 | 1.602 (7) | O22—C21 | 1.201 (4) |
N1—C1 | 1.167 (7) | N21—C25 | 1.323 (5) |
N2—C2 | 1.129 (7) | N21—C24 | 1.325 (5) |
N3—C3 | 1.164 (5) | N21—H21A | 0.84 (4) |
N4—C4 | 1.153 (7) | C21—C22 | 1.502 (5) |
O1W—H1WA | 0.76 (4) | C22—C26 | 1.375 (5) |
O11—C11 | 1.249 (4) | C22—C23 | 1.375 (5) |
O12—C11 | 1.246 (4) | C23—C24 | 1.361 (5) |
N11—C14 | 1.325 (5) | C23—H23A | 0.9300 |
N11—C15 | 1.327 (5) | C24—H24A | 0.9300 |
N11—H11A | 0.86 (4) | C25—C26 | 1.364 (5) |
C11—C12 | 1.515 (4) | C25—H25A | 0.9300 |
C12—C16 | 1.378 (5) | C26—H26A | 0.9300 |
N4—Fe1—N1 | 90.5 (2) | C14—C13—H13A | 120.0 |
N4—Fe1—N2 | 92.3 (2) | C12—C13—H13A | 120.0 |
N1—Fe1—N2 | 177.2 (2) | N11—C14—C13 | 119.9 (3) |
N4—Fe1—N3 | 93.10 (10) | N11—C14—H14A | 120.1 |
N1—Fe1—N3 | 87.99 (10) | C13—C14—H14A | 120.1 |
N2—Fe1—N3 | 91.85 (10) | N11—C15—C16 | 120.1 (3) |
N4—Fe1—N3i | 93.10 (10) | N11—C15—H15A | 120.0 |
N1—Fe1—N3i | 87.99 (10) | C16—C15—H15A | 120.0 |
N2—Fe1—N3i | 91.85 (10) | C15—C16—C12 | 119.5 (3) |
N3—Fe1—N3i | 172.64 (19) | C15—C16—H16A | 120.3 |
N4—Fe1—O1W | 179.6 (2) | C12—C16—H16A | 120.3 |
N1—Fe1—O1W | 89.1 (2) | C21—O21—H21 | 109.5 |
N2—Fe1—O1W | 88.1 (2) | C25—N21—C24 | 122.6 (3) |
N3—Fe1—O1W | 86.88 (10) | C25—N21—H21A | 120 (3) |
N3i—Fe1—O1W | 86.88 (10) | C24—N21—H21A | 117 (3) |
C1—N1—Fe1 | 166.8 (5) | O22—C21—O21 | 125.6 (3) |
C2—N2—Fe1 | 165.2 (5) | O22—C21—C22 | 120.7 (3) |
C3—N3—Fe1 | 160.8 (3) | O21—C21—C22 | 113.6 (3) |
C4—N4—Fe1 | 150.7 (5) | C26—C22—C23 | 119.1 (3) |
N1—C1—S1 | 176.4 (5) | C26—C22—C21 | 119.1 (3) |
N2—C2—S2 | 179.5 (6) | C23—C22—C21 | 121.8 (3) |
N3—C3—S3 | 178.7 (4) | C24—C23—C22 | 119.7 (3) |
N4—C4—S4 | 179.5 (6) | C24—C23—H23A | 120.2 |
Fe1—O1W—H1WA | 118 (4) | C22—C23—H23A | 120.2 |
C14—N11—C15 | 122.1 (3) | N21—C24—C23 | 119.5 (4) |
C14—N11—H11A | 118 (3) | N21—C24—H24A | 120.3 |
C15—N11—H11A | 120 (3) | C23—C24—H24A | 120.3 |
O12—C11—O11 | 125.6 (3) | N21—C25—C26 | 120.0 (4) |
O12—C11—C12 | 116.1 (3) | N21—C25—H25A | 120.0 |
O11—C11—C12 | 118.3 (3) | C26—C25—H25A | 120.0 |
C16—C12—C13 | 118.4 (3) | C25—C26—C22 | 119.1 (3) |
C16—C12—C11 | 122.3 (3) | C25—C26—H26A | 120.4 |
C13—C12—C11 | 119.3 (3) | C22—C26—H26A | 120.4 |
C14—C13—C12 | 120.0 (3) |
Symmetry code: (i) x, −y+3/2, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O11 | 0.76 (4) | 1.95 (4) | 2.711 (3) | 178 (5) |
N11—H11A···O11ii | 0.86 (4) | 1.86 (4) | 2.710 (3) | 168 (4) |
O21—H21···O12ii | 0.82 | 1.72 | 2.532 (3) | 173 |
N21—H21A···O22iii | 0.84 (4) | 2.14 (5) | 2.825 (4) | 138 (4) |
Symmetry codes: (ii) x+1/2, y, −z+1/2; (iii) x−1/2, y, −z+3/2. |
Experimental details
Crystal data | |
Chemical formula | (C6H6NO2)2[Fe(NCS)5(H2O)]·2C6H5NO2 |
Mr | 858.72 |
Crystal system, space group | Orthorhombic, Pnma |
Temperature (K) | 297 |
a, b, c (Å) | 14.8713 (3), 21.0882 (3), 11.9741 (2) |
V (Å3) | 3755.18 (11) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.74 |
Crystal size (mm) | 0.36 × 0.30 × 0.20 |
Data collection | |
Diffractometer | Siemens SMART CCD |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.776, 0.866 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 18247, 3405, 2589 |
Rint | 0.043 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.049, 0.132, 1.05 |
No. of reflections | 3405 |
No. of parameters | 265 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.71, −0.62 |
Computer programs: SMART (Siemens, 1996) and SAINT (Siemens, 1996), SAINT (Siemens, 1996) and XPREP (Siemens, 1995), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1999).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O11 | 0.76 (4) | 1.95 (4) | 2.711 (3) | 178 (5) |
N11—H11A···O11i | 0.86 (4) | 1.86 (4) | 2.710 (3) | 168 (4) |
O21—H21···O12i | 0.82 | 1.72 | 2.532 (3) | 173.4 |
N21—H21A···O22ii | 0.84 (4) | 2.14 (5) | 2.825 (4) | 138 (4) |
Symmetry codes: (i) x+1/2, y, −z+1/2; (ii) x−1/2, y, −z+3/2. |
Isothiocyanate anions exhibit a large variety of different coordination modes towards metal cations and, partially due to this, they are widely used as versatile ligands in many areas of coordination chemistry (Li, Tong et al., 2004; Li, Zhao et al., 2004 and Li et al., 2007). Herein we describe the crystal structure of the iron(III) isothiocyanate complex [inaH]2[Fe(H2O)(NCS)5].2[ina] (ina = isonicotinic acid).
A thermal ellipsoid drawing of the complex with the atomic numbering scheme is shown in Fig. 1. The iron complex lies on a mirror plane with the six-coordinated FeIII ion, a coordinated water molecule and three of the five isothiocyanate ligands located directly within this plane (atoms Fe1, O1W, N1, C1, S1, N2, C2, S2, N4, C4 and S4). The coordination geometry around the FeIII ion is slightly distorted octahedral. All the isothiocyanate anions coordinate to the iron(III) center through the nitrogen atoms in a slightly bent mode with C—N—Fe angles in the range of 150.7 (5)–166.8 (5)°. The ina molecules and the protonated inaH+ cations interact with each other through N—H···O and O—H···O hydrogen bonds which leads to the formation of a 2-D layer perpendicular to the b axis. One of this sublayers is shown in Fig. 2. Each two of these layers sandwich another layer of {[Fe(H2O)(NCS)5]2-}n anions with which they interact via electrostatic attraction and O—H···O hydrogen bonds, resulting in sheets of triple-layers perpendicular to the b axis. One of these triple-layers is shown in Fig. 3.