Crystal structure of di­aqua­bis­(4-cyano­pyridine-κN)bis­(thio­cyanato-κN)iron(II) 4-cyano­pyridine disolvate

Jochim, A.; Jess, I.; Näther, C.

doi:10.1107/S205698901700322X

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Volume 73| Part 4| April 2017| Pages 463-466

https://doi.org/10.1107/S205698901700322X

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Crystal structure of diaquabis(4-cyanopyridine-κN)bis(thiocyanato-κN)iron(II) 4-cyanopyridine disolvate

Aleksej Jochim,^a ^* Inke Jess ^a and Christian Näther ^a

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

Edited by M. Weil, Vienna University of Technology, Austria (Received 21 February 2017; accepted 27 February 2017; online 3 March 2017)

The asymmetric unit of the title compound, [Fe(NCS)₂(C₆H₄N₂)₂(H₂O)₂]·2C₆H₄N₂, comprises one Fe^II cation occupying an inversion centre as well as one thiocyanate anion, one water molecule and two 4-cyanopyridine molecules in general positions. The iron cations are coordinated by two N-bonded thiocyanate anions, two (pyridine)N-bonded 4-cyanopyridine ligands and two water molecules into discrete complexes. The resulting coordination polyhedron can be described as a slightly distorted octahedron. The discrete complexes are connected through centrosymmetric pairs of (pyridine)C—H⋯N(cyano) hydrogen bonds into chains that are further linked into a three-dimensional network through intermolecular O—H⋯N hydrogen bonds involving the 4-cyanopyridine solvent molecules.

Keywords: crystal structure; hydrogen bonding; 4-cyanopyridine; iron; thiocyanate.

CCDC reference: 1534965

1. Chemical context

Thiocyanate anions are versatile ligands that can coordinate in different modes to metal cations. In most cases the anionic ligands are terminally N-bonded to the metal cation but there are also several examples for a μ-_1,3 bridging mode (Werner et al., 2015 ; Boeckmann & Näther, 2012 ; Palion-Gazda et al., 2015 ). The latter coordination is of special interest if the compounds contain paramagnetic metal cations because then cooperative magnetic properties can be expected (Palion-Gazda et al., 2015). In this context, we have reported on several compounds with one- or two-dimensional structures based on Mn, Fe, Co or Ni as metals, thiocyanate ligands and different N-donor co-ligands that show different magnetic properties (Suckert et al., 2016 ; Rams et al., 2017 ; Boeckmann et al., 2012 ). Whereas compounds with a terminal coordination of the anionic ligands can usually be synthesized straightforwardly, compounds with bridging ligands are sometimes difficult to obtain from solution. Therefore, we have developed an alternative procedure which is based on thermal decomposition of precursors with a terminal NCS coordination that frequently transform into the desired polymeric compounds on heating. In the course of our investigations on the synthesis of coordination polymers with iron as metal, thiocyanate ligands and 4-cyanopyridine as co-ligands, we obtained the title compound which was identified by single crystal X-ray diffraction. Unfortunately, all samples were always contaminated with a second unknown crystalline phase, preventing any further investigations.

2. Structural commentary

The asymmetric unit of [Fe(NCS)₂(C₆H₄N₂)₂(H₂O)₂]·2C₆H₄N₂ contains one Fe^II cation that is located on an inversion centre, one thiocyanate anion, one water molecule and two 4-cyanopyridine molecules (Fig. 1). Discrete centrosymmetric [Fe(NCS)₂(C₆H₄N₂)₂(H₂O)₂] complexes are formed, in which the Fe^II cations are octahedrally coordinated by two N-bonded thiocyanate anions, two (pyridine)N-bonded 4-cyanopyridine ligands and two water molecules, each of them in a trans-position (Fig. 1). The disparate bond lengths are similar to those in related thiocyanate compounds. The distortion of the octahedron is also reflected by the deviation of the bond angles from ideal values. The structure contains additional 4-cyanopyridine solvate molecules that are located in the cavities of the structure.

Figure 1
The discrete complex and the solvent molecule of the title compound with labeling and displacement ellipsoids drawn at the 50% probability level. [Symmetry code: (i) 1 − x, 1 − y, 2 − z.]

3. Supramolecular features

The discrete complexes are linked into chains parallel to [101] by centrosymmetric pairs of intermolecular C—H⋯N hydrogen bonds between the cyano group of the coordinating 4-cyanopyridine ligand and one of the pyridine H atoms (Fig. 2, Table 1). These chains are further linked by the 4-cyanopyridine solvate molecules through intermolecular O—H⋯N hydrogen bonding. One water H atom is hydrogen-bonded to the N atom of the cyano group and the other H atom to the pyridine N atom of another 4-cyanopyridine solvate molecule. Since all water H atoms are involved in hydrogen bonding, each of the complexes is surrounded by four 4-cyanopyridine ligands, of which two are hydrogen-bonded via the cyano group, whereas the other two are hydrogen-bonded via the pyridine N atom (Fig. 3, Table 1). This arrangement leads to a three-dimensional network structure. It is noted that there are additional short contacts between the thiocyanate anions and the pyridine H atoms of the coordinating 4-cyanopyridine ligand of a neighbouring complex, which is indicative of weak C—H⋯S hydrogen bonding (Table 1).

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C12—H12⋯N12ⁱ	0.95	2.52	3.437 (3)	162
C14—H14⋯S1ⁱⁱ	0.95	3.01	3.960 (2)	177
O1—H1⋯N22ⁱⁱⁱ	0.84	2.00	2.8380 (19)	177
O1—H2⋯N21^iv	0.84	1.89	2.7159 (19)	168
Symmetry codes: (i) -x, -y+1, -z+1; (ii) $[x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (iii) -x+1, -y+1, -z+2; (iv) $[x-1, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ .

Figure 2
Part of the crystal structure of the title compound in a view along the b axis with emphasis on the connection of discrete complexes and solvent molecules by intermolecular hydrogen bonding (dashed lines).

Figure 3
The crystal structure of the title compound in a view along the a axis. Intermolecular hydrogen bonding is shown as dashed lines.

4. Database survey

In the Cambridge Structure Database (Version 5.38, last update 2016; Groom et al., 2016 ), five structures of coordination polymers with 4-cyanopyridine and thiocyanate as ligands are reported, in which the metal cations are solely connected through μ-_1,3 bridging thiocyanate anions. Two of these compounds contain copper, two cadmium and one is a bimetallic compound in which copper and mercury are present. The two copper-containing compounds are built up of chains, in which the cations are either tetrahedrally (Lin et al., 2004 ) or octahedrally (Machura et al., 2013a ) coordinated. In the bimetallic compound the cations are linked into a three-dimensional structure (Machura et al., 2013b ), whereas the two cadmium-containing compounds exhibit either one-dimensional or three-dimensional coordination networks (Chen et al., 2002 ).

5. Synthesis and crystallization

Iron(II) chloride tetrahydrate, potassium thiocyanate and 4-cyanopyridine were obtained from Alfa Aesar and used without further purification.

29.8 mg iron(II) chloride tetrahydrate (0.15 mmol) and 29.2 mg KSCN (0.30 mmol) were reacted with 62.5 mg 4-cyanopyridine (0.60 mmol) in 1.5 ml water at room temperature. After two days, single crystals suitable for structure analysis were obtained. The batch contained a small amount of an additional crystalline phase that could not be identified.

6. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 2. Hydrogen atoms of the water molecule were located from a difference map, and C-bound hydrogen atoms were refined in calculated positions [C—H = 0.95 Å and O—H = 0.84 Å] with U_iso(H) = 1.2U_eq(C) [1.5 for U_eq(O)] using a riding model (O—H hydrogen atoms were allowed to rotate but not to tip).

Table 2
Experimental details

Crystal data
Chemical formula	[Fe(NCS)₂(C₆H₄N₂)₂(H₂O)₂]·2C₆H₄N₂
M_r	624.49
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	200
a, b, c (Å)	8.5376 (4), 15.220 (1), 12.1214 (6)
β (°)	96.195 (6)
V (Å³)	1565.88 (15)
Z	2
Radiation type	Mo Kα
μ (mm⁻¹)	0.66
Crystal size (mm)	0.13 × 0.10 × 0.06

Data collection
Diffractometer	Stoe IPDS1
Absorption correction	Numerical (X-RED and X-SHAPE; Stoe & Cie, 2008 )
T_min, T_max	0.884, 0.953
No. of measured, independent and observed [I > 2σ(I)] reflections	18486, 3743, 2960
R_int	0.047
(sin θ/λ)_max (Å⁻¹)	0.663

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.094, 1.03
No. of reflections	3743
No. of parameters	188
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.26, −0.46
Computer programs: X-AREA (Stoe & Cie, 2008), SHELXS97 and XP (Sheldrick, 2008 ), SHELXL2014 (Sheldrick, 2015 ), DIAMOND (Brandenburg, 2014 ) and publCIF (Westrip, 2010 ).

Supporting information

CCDC reference: 1534965

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S205698901700322X/wm5371sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S205698901700322X/wm5371Isup2.hkl

checkCIF report

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: SHELXL2014 (Sheldrick, 2015); molecular graphics: XP (Sheldrick, 2008) and DIAMOND (Brandenburg, 2014); software used to prepare material for publication: publCIF (Westrip, 2010).

Diaquabis(4-cyanopyridine-κN)bis(thiocyanato-κN)iron(II) 4-cyanopyridine disolvate top

Crystal data top

[Fe(NCS)₂(C₆H₄N₂)₂(H₂O)₂]·2C₆H₄N₂	F(000) = 640
M_r = 624.49	D_x = 1.324 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 8.5376 (4) Å	Cell parameters from 18864 reflections
b = 15.220 (1) Å	θ = 3.8–56.3°
c = 12.1214 (6) Å	µ = 0.66 mm⁻¹
β = 96.195 (6)°	T = 200 K
V = 1565.88 (15) Å³	Block, yellow
Z = 2	0.13 × 0.10 × 0.06 mm

Data collection top

Stoe IPDS-1 diffractometer	2960 reflections with I > 2σ(I)
Phi scans	R_int = 0.047
Absorption correction: numerical (X-RED and X-SHAPE; Stoe & Cie, 2008)	θ_max = 28.1°, θ_min = 2.7°
T_min = 0.884, T_max = 0.953	h = −11→10
18486 measured reflections	k = −20→20
3743 independent reflections	l = −16→16

Refinement top

Refinement on F²	Hydrogen site location: mixed
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.037	w = 1/[σ²(F_o²) + (0.0581P)² + 0.1102P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.094	(Δ/σ)_max = 0.001
S = 1.03	Δρ_max = 0.26 e Å⁻³
3743 reflections	Δρ_min = −0.46 e Å⁻³
188 parameters	Extinction correction: SHELXL2014 (Sheldrick, 2015), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.019 (3)

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.

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

	x	y	z	U_iso*/U_eq
Fe1	0.5000	0.5000	1.0000	0.02513 (11)
N1	0.58788 (18)	0.62971 (9)	0.99472 (12)	0.0358 (3)
C1	0.62673 (19)	0.69914 (10)	0.96961 (13)	0.0305 (3)
S1	0.68128 (7)	0.79604 (3)	0.93149 (5)	0.05165 (16)
N11	0.42359 (17)	0.50738 (9)	0.81712 (11)	0.0317 (3)
C11	0.2830 (2)	0.47429 (11)	0.77885 (14)	0.0351 (4)
H11	0.2267	0.4414	0.8283	0.042*
C12	0.2158 (2)	0.48550 (11)	0.67119 (15)	0.0390 (4)
H12	0.1150	0.4617	0.6472	0.047*
C13	0.2990 (2)	0.53234 (13)	0.59914 (14)	0.0399 (4)
C14	0.4458 (2)	0.56588 (13)	0.63609 (15)	0.0425 (4)
H14	0.5055	0.5976	0.5877	0.051*
C15	0.5029 (2)	0.55172 (12)	0.74578 (14)	0.0381 (4)
H15	0.6036	0.5747	0.7718	0.046*
C16	0.2332 (3)	0.54478 (18)	0.48511 (18)	0.0570 (6)
N12	0.1795 (3)	0.5537 (2)	0.39540 (17)	0.0837 (8)
O1	0.28045 (13)	0.55033 (7)	1.02877 (9)	0.0320 (2)
H1	0.2201	0.5134	1.0535	0.048*
H2	0.2728	0.5951	1.0684	0.048*
N21	1.2086 (2)	0.80713 (12)	0.64837 (15)	0.0523 (4)
C21	1.0626 (3)	0.7796 (2)	0.6202 (2)	0.0774 (9)
H21	1.0072	0.8031	0.5546	0.093*
C22	0.9863 (3)	0.71950 (19)	0.67912 (19)	0.0685 (8)
H22	0.8813	0.7018	0.6554	0.082*
C23	1.0672 (2)	0.68573 (11)	0.77413 (14)	0.0347 (4)
C24	1.2197 (2)	0.71283 (11)	0.80597 (15)	0.0378 (4)
H24	1.2775	0.6904	0.8713	0.045*
C25	1.2856 (2)	0.77362 (13)	0.73992 (17)	0.0445 (4)
H25	1.3907	0.7923	0.7609	0.053*
C26	0.9913 (2)	0.62137 (12)	0.83758 (14)	0.0361 (4)
N22	0.9307 (2)	0.56987 (11)	0.88643 (14)	0.0460 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.02351 (17)	0.02120 (16)	0.03167 (17)	−0.00047 (11)	0.00745 (11)	0.00057 (11)
N1	0.0402 (9)	0.0231 (6)	0.0448 (8)	−0.0057 (5)	0.0075 (6)	0.0016 (5)
C1	0.0277 (8)	0.0303 (8)	0.0329 (8)	−0.0006 (6)	0.0004 (6)	−0.0007 (6)
S1	0.0599 (3)	0.0304 (2)	0.0628 (3)	−0.0137 (2)	−0.0017 (2)	0.0132 (2)
N11	0.0305 (7)	0.0324 (7)	0.0328 (7)	0.0002 (5)	0.0053 (5)	−0.0015 (5)
C11	0.0343 (9)	0.0308 (8)	0.0408 (9)	−0.0028 (6)	0.0061 (7)	−0.0035 (6)
C12	0.0341 (9)	0.0375 (9)	0.0446 (9)	0.0010 (7)	0.0001 (7)	−0.0080 (7)
C13	0.0397 (10)	0.0458 (10)	0.0338 (8)	0.0094 (8)	0.0022 (7)	−0.0055 (7)
C14	0.0393 (10)	0.0550 (11)	0.0342 (8)	0.0011 (8)	0.0086 (7)	0.0046 (8)
C15	0.0325 (9)	0.0472 (10)	0.0353 (8)	−0.0032 (7)	0.0071 (7)	0.0014 (7)
C16	0.0451 (12)	0.0819 (16)	0.0433 (11)	0.0035 (11)	0.0015 (9)	−0.0003 (10)
N12	0.0618 (14)	0.140 (2)	0.0460 (11)	−0.0095 (14)	−0.0079 (9)	0.0126 (13)
O1	0.0272 (6)	0.0284 (5)	0.0422 (6)	−0.0004 (4)	0.0117 (5)	−0.0031 (4)
N21	0.0464 (10)	0.0518 (10)	0.0607 (10)	−0.0051 (8)	0.0144 (8)	0.0215 (8)
C21	0.0541 (15)	0.111 (2)	0.0643 (15)	−0.0162 (14)	−0.0084 (11)	0.0537 (15)
C22	0.0417 (12)	0.105 (2)	0.0554 (13)	−0.0231 (12)	−0.0112 (10)	0.0401 (13)
C23	0.0313 (9)	0.0379 (9)	0.0351 (8)	−0.0039 (7)	0.0048 (6)	0.0051 (6)
C24	0.0338 (10)	0.0367 (9)	0.0421 (9)	−0.0014 (7)	0.0005 (7)	0.0066 (7)
C25	0.0341 (10)	0.0406 (10)	0.0593 (11)	−0.0058 (7)	0.0068 (8)	0.0074 (8)
C26	0.0315 (9)	0.0419 (9)	0.0351 (8)	−0.0026 (7)	0.0039 (6)	0.0020 (7)
N22	0.0397 (9)	0.0490 (9)	0.0508 (9)	−0.0068 (7)	0.0122 (7)	0.0104 (7)

Geometric parameters (Å, º) top

Fe1—O1ⁱ	2.0888 (11)	C14—H14	0.9500
Fe1—O1	2.0888 (11)	C15—H15	0.9500
Fe1—N1	2.1153 (13)	C16—N12	1.141 (3)
Fe1—N1ⁱ	2.1153 (13)	O1—H1	0.8400
Fe1—N11ⁱ	2.2451 (14)	O1—H2	0.8400
Fe1—N11	2.2451 (14)	N21—C21	1.325 (3)
N1—C1	1.158 (2)	N21—C25	1.329 (3)
C1—S1	1.6286 (16)	C21—C22	1.368 (3)
N11—C15	1.337 (2)	C21—H21	0.9500
N11—C11	1.338 (2)	C22—C23	1.377 (3)
C11—C12	1.378 (3)	C22—H22	0.9500
C11—H11	0.9500	C23—C24	1.380 (3)
C12—C13	1.382 (3)	C23—C26	1.442 (2)
C12—H12	0.9500	C24—C25	1.382 (3)
C13—C14	1.382 (3)	C24—H24	0.9500
C13—C16	1.447 (3)	C25—H25	0.9500
C14—C15	1.383 (3)	C26—N22	1.140 (2)

O1ⁱ—Fe1—O1	180.0	C14—C13—C16	120.42 (19)
O1ⁱ—Fe1—N1	90.55 (5)	C13—C14—C15	117.86 (17)
O1—Fe1—N1	89.45 (5)	C13—C14—H14	121.1
O1ⁱ—Fe1—N1ⁱ	89.45 (5)	C15—C14—H14	121.1
O1—Fe1—N1ⁱ	90.55 (5)	N11—C15—C14	123.35 (17)
N1—Fe1—N1ⁱ	180.0	N11—C15—H15	118.3
O1ⁱ—Fe1—N11ⁱ	88.63 (5)	C14—C15—H15	118.3
O1—Fe1—N11ⁱ	91.37 (5)	N12—C16—C13	179.0 (3)
N1—Fe1—N11ⁱ	90.59 (5)	Fe1—O1—H1	114.2
N1ⁱ—Fe1—N11ⁱ	89.41 (5)	Fe1—O1—H2	121.3
O1ⁱ—Fe1—N11	91.37 (5)	H1—O1—H2	104.5
O1—Fe1—N11	88.63 (5)	C21—N21—C25	117.42 (17)
N1—Fe1—N11	89.41 (5)	N21—C21—C22	124.4 (2)
N1ⁱ—Fe1—N11	90.59 (5)	N21—C21—H21	117.8
N11ⁱ—Fe1—N11	180.0	C22—C21—H21	117.8
C1—N1—Fe1	166.44 (14)	C21—C22—C23	117.5 (2)
N1—C1—S1	178.74 (15)	C21—C22—H22	121.2
C15—N11—C11	117.64 (15)	C23—C22—H22	121.2
C15—N11—Fe1	123.39 (12)	C22—C23—C24	119.69 (17)
C11—N11—Fe1	118.54 (11)	C22—C23—C26	119.08 (17)
N11—C11—C12	123.23 (17)	C24—C23—C26	121.22 (15)
N11—C11—H11	118.4	C23—C24—C25	117.94 (17)
C12—C11—H11	118.4	C23—C24—H24	121.0
C11—C12—C13	118.18 (17)	C25—C24—H24	121.0
C11—C12—H12	120.9	N21—C25—C24	123.03 (18)
C13—C12—H12	120.9	N21—C25—H25	118.5
C12—C13—C14	119.72 (17)	C24—C25—H25	118.5
C12—C13—C16	119.85 (19)	N22—C26—C23	179.1 (2)

Symmetry code: (i) −x+1, −y+1, −z+2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C12—H12···N12ⁱⁱ	0.95	2.52	3.437 (3)	162
C14—H14···S1ⁱⁱⁱ	0.95	3.01	3.960 (2)	177
O1—H1···N22ⁱ	0.84	2.00	2.8380 (19)	177
O1—H2···N21^iv	0.84	1.89	2.7159 (19)	168

Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) −x, −y+1, −z+1; (iii) x, −y+3/2, z−1/2; (iv) x−1, −y+3/2, z+1/2.

Acknowledgements

This project was supported by the Deutsche Forschungsgemeinschaft (Project No. NA 720/5–1) and the State of Schleswig-Holstein. We thank Professor Dr Wolfgang Bensch for access to his experimental facilities.

Funding information

Funding for this research was provided by: Deutsche Forschungsgemeinschaft (award No. NA 720/5–1); State of Schleswig-Holstein.

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