Tris[4-(dimethyl­amino)­pyridinium] hexa­kis­(thio­cyanato-κN)ferrate(III) monohydrate

Wöhlert, S.; Jess, I.; Näther, C.

doi:10.1107/S1600536812049574

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 69| Part 1| January 2013| Page m33

https://doi.org/10.1107/S1600536812049574

Open

access

Tris[4-(dimethylamino)pyridinium] hexakis(thiocyanato-κN)ferrate(III) monohydrate

Susanne Wöhlert,^a ^* Inke Jess ^a and Christian Näther ^a

^aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Strasse 2, 24118 Kiel, Germany
^*Correspondence e-mail: swoehlert@ac.uni-kiel.de

(Received 13 November 2012; accepted 3 December 2012; online 8 December 2012)

In the title compound, (C₇H₁₁N₂)₃[Fe(NCS)₆]·H₂O, the Fe^III 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 Fe^III cation, six thiocyanate anions, three 4-(dimethylamino)pyridinium cations and one water molecule, all of them located in general positions.

Related literature

For general background to our work on the synthesis and characterization of coordination compounds based on transition metal thiocyanates and neutral N-donor co-ligands such as pyridine, see: Boeckmann & Näther (2011 , 2012 ).

Experimental

Crystal data

(C₇H₁₁N₂)₃[Fe(NCS)₆]·H₂O
M_r = 791.88
Triclinic, $[P \overline 1]$
a = 11.5780 (7) Å
b = 11.7620 (7) Å
c = 16.5450 (11) Å
α = 81.260 (7)°
β = 71.550 (7)°
γ = 62.950 (6)°
V = 1903.4 (2) Å³
Z = 2
Mo Kα radiation
μ = 0.77 mm⁻¹
T = 180 K
0.13 × 0.08 × 0.06 mm

Data collection

Stoe IPDS-1 diffractometer
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ) T_min = 0.808, T_max = 0.947
13617 measured reflections
7356 independent reflections
4936 reflections with I > 2σ(I)
R_int = 0.075

Refinement

R[F² > 2σ(F²)] = 0.042
wR(F²) = 0.104
S = 0.95
7356 reflections
431 parameters
H-atom parameters constrained
Δρ_max = 0.34 e Å⁻³
Δρ_min = −0.50 e Å⁻³

Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA; data reduction: X-AREA; 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.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536812049574/hp2051sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812049574/hp2051Isup2.hkl

checkCIF report

Comment top

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).

Related literature top

Experimental top

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.

Structure description top

Computing details top

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).

Figures top

	Fig. 1. : Crystal structure of the title compound with labeling and displacement ellipsoids drawn at the 50% probability level.
	Fig. 2. : Crystal structure of the title compound with view along the crystallographic c-axis. Intermolecular hydrogen bonding is shown as dashed lines.

Tris[4-(dimethylamino)pyridinium] hexakis(thiocyanato-κN)ferrate(III) monohydrate top

Crystal data top

(C₇H₁₁N₂)₃[Fe(NCS)₆]·H₂O	Z = 2
M_r = 791.88	F(000) = 822
Triclinic, P1	D_x = 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

Data collection top

Stoe IPDS-1 diffractometer	7356 independent reflections
Radiation source: fine-focus sealed tube	4936 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.075
phi scan	θ_max = 26.0°, θ_min = 2.4°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −14→14
T_min = 0.808, T_max = 0.947	k = −14→14
13617 measured reflections	l = −20→20

Refinement top

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(F_o²) + (0.052P)²] where P = (F_o² + 2F_c²)/3
S = 0.95	(Δ/σ)_max = 0.001
7356 reflections	Δρ_max = 0.34 e Å⁻³
431 parameters	Δρ_min = −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)

Crystal data top

(C₇H₁₁N₂)₃[Fe(NCS)₆]·H₂O	γ = 62.950 (6)°
M_r = 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)°

Data collection top

Stoe IPDS-1 diffractometer	7356 independent reflections
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	4936 reflections with I > 2σ(I)
T_min = 0.808, T_max = 0.947	R_int = 0.075
13617 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.042	0 restraints
wR(F²) = 0.104	H-atom parameters constrained
S = 0.95	Δρ_max = 0.34 e Å⁻³
7356 reflections	Δρ_min = −0.50 e Å⁻³
431 parameters

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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*

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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)

Experimental details

Crystal data
Chemical formula	(C₇H₁₁N₂)₃[Fe(NCS)₆]·H₂O
M_r	791.88
Crystal system, space group	Triclinic, P1
Temperature (K)	180
a, b, c (Å)	11.5780 (7), 11.7620 (7), 16.5450 (11)
α, β, γ (°)	81.260 (7), 71.550 (7), 62.950 (6)
V (Å³)	1903.4 (2)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.77
Crystal size (mm)	0.13 × 0.08 × 0.06

Data collection
Diffractometer	Stoe IPDS1
Absorption correction	Numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)
T_min, T_max	0.808, 0.947
No. of measured, independent and observed [I > 2σ(I)] reflections	13617, 7356, 4936
R_int	0.075
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.042, 0.104, 0.95
No. of reflections	7356
No. of parameters	431
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.34, −0.50

Computer programs: X-AREA (Stoe & Cie, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2012), XCIF in SHELXTL (Sheldrick, 2008).

Acknowledgements

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.

References

Boeckmann, J. & Näther, C. (2011). Dalton Trans. 39, 11019–11026. Web of Science CSD CrossRef Google Scholar
Boeckmann, J. & Näther, C. (2012). Polyhedron, 31 587–595. Web of Science CSD CrossRef CAS Google Scholar
Brandenburg, K. (2012). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany. Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.