catena-Poly[[[di-aqua-bis-(seleno-cyanato-κN)iron(II)]-μ-1,2-bis-(pyridin-4-yl)ethane-κ(2) N:N'] 1,2-bis-(pyridin-4-yl)ethane disolvate dihydrate].

The title compound, {[Fe(NCSe)2(C12H12N2)(H2O)2]·2C12H12N2·2H2O} n , was obtained by the reaction of iron(II) sulfate hepta-hydrate and potassium seleno-cyanate with 1,2-bis-(pyridin-4-yl)ethane (bpa) in water. The Fe(II) cation is coordinated by two N-bonded seleno-cyanate anions, two water mol-ecules and two 1,2-bis-(pyridin-4-yl)ethane (bpa) ligands in a slightly distorted octa-hedral geometry. In addition, two non-coordinating bpa mol-ecules and two water mol-ecules are present. The Fe(II) cation is located on a center of inversion while the coordinating bpa ligand is located on a twofold rotation axis. The Fe(II) cations are linked by the bpa ligands into chains along the b-axis direction, which are further connected into layers perpedicular to the c axis by O-H⋯N and O-H⋯O hydrogen bonds to the non-coordin-ating bpa and the water mol-ecules. The crystal studied was twinned by pseudo-merohedry (180° rotation along c*; contribution of the minor twin component 3.7%).

Related literature

For background to this work see: Boeckmann & Näther (2011 ▶); Wöhlert et al. (2012 ▶); Boeckmann et al. (2012 ▶).

Experimental

Crystal data

[Fe(NCSe)2(C12H12N2)(H2O)2]·2C12H12N2·2H2O

M = 890.58

Monoclinic,

a = 8.0790 (6) Å

b = 14.1870 (7) Å

c = 17.6553 (12) Å

β = 102.645 (8)°

V = 1974.5 (2) Å3

Z = 2

Mo Kα radiation

μ = 2.28 mm−1

T = 293 K

0.23 × 0.16 × 0.09 mm

Data collection

Stoe IPDS-2 diffractometer

Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008 ▶) T min = 0.645, T max = 0.818

20183 measured reflections

4540 independent reflections

3659 reflections with I > 2σ(I)

R int = 0.095

Refinement

R[F 2 > 2σ(F 2)] = 0.045

wR(F 2) = 0.119

S = 1.09

4540 reflections

242 parameters

H-atom parameters constrained

Δρmax = 0.58 e Å−3

Δρmin = −0.88 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, 2011 ▶); software used to prepare material for publication: XCIF in SHELXTL and publCIF (Westrip, 2010 ▶).

Click here for additional data file.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536813012312/zl2548sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813012312/zl2548Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Fe(NCSe)2(C12H12N2)(H2O)2]·2C12H12N2·2H2O	F(000) = 908
Mr = 890.58	Dx = 1.498 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 20183 reflections
a = 8.0790 (6) Å	θ = 2.4–27.5°
b = 14.1870 (7) Å	µ = 2.28 mm−1
c = 17.6553 (12) Å	T = 293 K
β = 102.645 (8)°	Block, red
V = 1974.5 (2) Å3	0.23 × 0.16 × 0.09 mm
Z = 2

Stoe IPDS-2 diffractometer	4540 independent reflections
Radiation source: fine-focus sealed tube	3659 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.095
ω scan	θmax = 27.5°, θmin = 2.4°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	h = −10→10
Tmin = 0.645, Tmax = 0.818	k = −18→18
20183 measured reflections	l = −22→22

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)] = 0.045	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.119	H-atom parameters constrained
S = 1.09	w = 1/[σ2(Fo2) + (0.0393P)2 + 4.2316P] where P = (Fo2 + 2Fc2)/3
4540 reflections	(Δ/σ)max = 0.001
242 parameters	Δρmax = 0.58 e Å−3
0 restraints	Δρmin = −0.88 e Å−3

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	1.0000	0.0000	0.5000	0.01501 (15)
N1	1.0298 (4)	−0.0036 (2)	0.62294 (18)	0.0224 (6)
C1	0.9954 (4)	−0.0081 (2)	0.6834 (2)	0.0174 (7)
Se1	0.94592 (5)	−0.01632 (3)	0.77704 (2)	0.02554 (12)
N10	0.9925 (4)	0.16528 (19)	0.50356 (18)	0.0189 (6)
C10	1.0341 (5)	0.2181 (2)	0.4477 (2)	0.0229 (8)
H10	1.0757	0.1878	0.4090	0.028*
C11	1.0186 (5)	0.3159 (2)	0.4442 (2)	0.0246 (8)
H11	1.0494	0.3489	0.4040	0.030*
C12	0.9576 (5)	0.3639 (2)	0.5007 (2)	0.0223 (8)
C13	0.9174 (6)	0.3093 (2)	0.5604 (2)	0.0251 (8)
H13	0.8780	0.3379	0.6004	0.030*
C14	0.9370 (5)	0.2119 (2)	0.5591 (2)	0.0229 (8)
H14	0.9099	0.1770	0.5994	0.027*
C15	0.9243 (6)	0.4693 (2)	0.4954 (3)	0.0353 (11)
H15A	0.8506	0.4826	0.4454	0.042*
H15B	0.8631	0.4864	0.5349	0.042*
N20	0.5764 (5)	0.1671 (2)	0.6762 (2)	0.0319 (8)
C20	0.6829 (6)	0.2156 (3)	0.7307 (3)	0.0319 (9)
H20	0.7699	0.1830	0.7635	0.038*
C21	0.6708 (6)	0.3120 (3)	0.7410 (3)	0.0296 (9)
H21	0.7474	0.3429	0.7801	0.036*
C22	0.5421 (5)	0.3616 (2)	0.6920 (2)	0.0254 (8)
C23	0.4316 (6)	0.3110 (3)	0.6357 (3)	0.0320 (9)
H23	0.3433	0.3414	0.6020	0.038*
C24	0.4532 (6)	0.2150 (3)	0.6300 (3)	0.0342 (10)
H24	0.3775	0.1821	0.5918	0.041*
C25	0.5290 (6)	0.4669 (3)	0.6976 (2)	0.0291 (9)
H25A	0.6028	0.4888	0.7453	0.035*
H25B	0.4135	0.4844	0.6987	0.035*
C26	0.5799 (6)	0.5132 (3)	0.6283 (2)	0.0277 (8)
H26A	0.6899	0.4891	0.6241	0.033*
H26B	0.4986	0.4955	0.5815	0.033*
C27	0.5889 (5)	0.6193 (2)	0.6332 (2)	0.0229 (8)
C28	0.6949 (5)	0.6639 (3)	0.6955 (2)	0.0253 (8)
H28	0.7595	0.6288	0.7359	0.030*
C29	0.7026 (5)	0.7616 (3)	0.6964 (2)	0.0283 (8)
H29	0.7759	0.7909	0.7376	0.034*
C30	0.5083 (7)	0.7723 (3)	0.5820 (3)	0.0365 (10)
H30	0.4436	0.8091	0.5429	0.044*
C31	0.4938 (6)	0.6753 (3)	0.5756 (3)	0.0329 (9)
H31	0.4209	0.6480	0.5332	0.039*
N21	0.6101 (5)	0.8156 (2)	0.6412 (2)	0.0309 (8)
O1	1.2588 (3)	0.00213 (19)	0.50632 (15)	0.0241 (5)
H1O1	1.2976	−0.0004	0.4672	0.036*
H2O1	1.3430	−0.0061	0.5412	0.036*
O2	1.4393 (4)	0.00140 (17)	0.39471 (15)	0.0227 (5)
H1O2	1.3985	−0.0371	0.3612	0.034*
H2O2	1.3942	0.0526	0.3828	0.034*

	U11	U22	U33	U12	U13	U23
Fe1	0.0173 (3)	0.0124 (3)	0.0164 (3)	0.0008 (2)	0.0059 (3)	0.0003 (2)
N1	0.0271 (16)	0.0203 (14)	0.0197 (15)	0.0008 (12)	0.0049 (13)	0.0006 (11)
C1	0.0183 (16)	0.0117 (14)	0.0204 (17)	0.0007 (12)	0.0007 (13)	−0.0002 (11)
Se1	0.0285 (2)	0.03071 (19)	0.01874 (19)	−0.00250 (16)	0.00811 (15)	−0.00011 (14)
N10	0.0242 (15)	0.0135 (13)	0.0199 (14)	0.0008 (11)	0.0067 (12)	0.0008 (10)
C10	0.032 (2)	0.0146 (15)	0.0268 (19)	−0.0005 (14)	0.0168 (17)	−0.0018 (13)
C11	0.034 (2)	0.0159 (15)	0.029 (2)	−0.0030 (14)	0.0198 (18)	0.0026 (13)
C12	0.0263 (19)	0.0118 (15)	0.032 (2)	−0.0015 (13)	0.0132 (17)	−0.0007 (13)
C13	0.037 (2)	0.0166 (16)	0.0266 (19)	0.0007 (15)	0.0166 (17)	−0.0031 (14)
C14	0.034 (2)	0.0151 (15)	0.0214 (17)	0.0023 (14)	0.0110 (16)	0.0017 (13)
C15	0.045 (3)	0.0125 (16)	0.059 (3)	0.0014 (16)	0.034 (2)	−0.0004 (16)
N20	0.044 (2)	0.0205 (15)	0.0312 (18)	0.0000 (14)	0.0075 (17)	−0.0019 (13)
C20	0.034 (2)	0.0256 (19)	0.036 (2)	0.0033 (16)	0.0073 (19)	0.0017 (16)
C21	0.033 (2)	0.0226 (18)	0.034 (2)	−0.0059 (15)	0.0077 (18)	−0.0015 (15)
C22	0.031 (2)	0.0181 (16)	0.032 (2)	−0.0014 (14)	0.0172 (18)	−0.0003 (14)
C23	0.038 (2)	0.0248 (19)	0.032 (2)	0.0006 (16)	0.0034 (19)	0.0013 (15)
C24	0.048 (3)	0.0226 (18)	0.029 (2)	−0.0054 (17)	0.003 (2)	−0.0039 (15)
C25	0.034 (2)	0.0204 (17)	0.037 (2)	−0.0012 (15)	0.0168 (19)	−0.0042 (15)
C26	0.037 (2)	0.0181 (16)	0.030 (2)	0.0010 (15)	0.0115 (18)	−0.0013 (14)
C27	0.0235 (19)	0.0179 (16)	0.029 (2)	0.0002 (13)	0.0098 (16)	−0.0015 (13)
C28	0.025 (2)	0.0213 (17)	0.032 (2)	0.0019 (14)	0.0101 (17)	0.0002 (14)
C29	0.031 (2)	0.0211 (17)	0.034 (2)	−0.0025 (15)	0.0099 (18)	−0.0030 (15)
C30	0.047 (3)	0.0242 (19)	0.037 (2)	0.0062 (18)	0.007 (2)	0.0079 (16)
C31	0.040 (2)	0.0262 (19)	0.030 (2)	−0.0027 (17)	0.0022 (19)	0.0004 (15)
N21	0.040 (2)	0.0194 (15)	0.036 (2)	0.0017 (14)	0.0137 (17)	0.0011 (13)
O1	0.0186 (13)	0.0350 (14)	0.0195 (12)	0.0013 (10)	0.0059 (11)	0.0015 (10)
O2	0.0271 (14)	0.0174 (11)	0.0231 (13)	0.0031 (10)	0.0043 (11)	−0.0012 (9)

Fe1—O1	2.069 (3)	C21—H21	0.9300
Fe1—O1i	2.069 (3)	C22—C23	1.383 (6)
Fe1—N1i	2.132 (3)	C22—C25	1.503 (5)
Fe1—N1	2.132 (3)	C23—C24	1.379 (6)
Fe1—N10i	2.347 (3)	C23—H23	0.9300
Fe1—N10	2.347 (3)	C24—H24	0.9300
N1—C1	1.162 (5)	C25—C26	1.522 (6)
C1—Se1	1.788 (4)	C25—H25A	0.9700
N10—C10	1.339 (5)	C25—H25B	0.9700
N10—C14	1.339 (5)	C26—C27	1.508 (5)
C10—C11	1.393 (5)	C26—H26A	0.9700
C10—H10	0.9300	C26—H26B	0.9700
C11—C12	1.384 (5)	C27—C31	1.383 (6)
C11—H11	0.9300	C27—C28	1.390 (5)
C12—C13	1.402 (5)	C28—C29	1.388 (5)
C12—C15	1.519 (5)	C28—H28	0.9300
C13—C14	1.392 (5)	C29—N21	1.333 (5)
C13—H13	0.9300	C29—H29	0.9300
C14—H14	0.9300	C30—N21	1.330 (6)
C15—C15ii	1.481 (9)	C30—C31	1.384 (6)
C15—H15A	0.9700	C30—H30	0.9300
C15—H15B	0.9700	C31—H31	0.9300
N20—C24	1.327 (6)	O1—H1O1	0.8201
N20—C20	1.333 (6)	O1—H2O1	0.8201
C20—C21	1.386 (5)	O2—H1O2	0.8199
C20—H20	0.9300	O2—H2O2	0.8200
C21—C22	1.390 (6)
O1—Fe1—O1i	180.000 (1)	C20—C21—C22	118.9 (4)
O1—Fe1—N1i	86.68 (12)	C20—C21—H21	120.5
O1i—Fe1—N1i	93.32 (12)	C22—C21—H21	120.5
O1—Fe1—N1	93.32 (12)	C23—C22—C21	117.5 (3)
O1i—Fe1—N1	86.68 (12)	C23—C22—C25	121.3 (4)
N1i—Fe1—N1	180.000 (1)	C21—C22—C25	121.1 (4)
O1—Fe1—N10i	89.09 (11)	C24—C23—C22	119.6 (4)
O1i—Fe1—N10i	90.91 (11)	C24—C23—H23	120.2
N1i—Fe1—N10i	89.69 (11)	C22—C23—H23	120.2
N1—Fe1—N10i	90.31 (11)	N20—C24—C23	123.4 (4)
O1—Fe1—N10	90.91 (11)	N20—C24—H24	118.3
O1i—Fe1—N10	89.09 (11)	C23—C24—H24	118.3
N1i—Fe1—N10	90.31 (11)	C22—C25—C26	109.9 (3)
N1—Fe1—N10	89.69 (11)	C22—C25—H25A	109.7
N10i—Fe1—N10	180.000 (1)	C26—C25—H25A	109.7
C1—N1—Fe1	160.1 (3)	C22—C25—H25B	109.7
N1—C1—Se1	178.9 (3)	C26—C25—H25B	109.7
C10—N10—C14	116.2 (3)	H25A—C25—H25B	108.2
C10—N10—Fe1	121.8 (2)	C27—C26—C25	113.8 (3)
C14—N10—Fe1	121.8 (2)	C27—C26—H26A	108.8
N10—C10—C11	123.7 (3)	C25—C26—H26A	108.8
N10—C10—H10	118.1	C27—C26—H26B	108.8
C11—C10—H10	118.1	C25—C26—H26B	108.8
C12—C11—C10	120.1 (3)	H26A—C26—H26B	107.7
C12—C11—H11	120.0	C31—C27—C28	117.9 (3)
C10—C11—H11	120.0	C31—C27—C26	121.3 (4)
C11—C12—C13	116.5 (3)	C28—C27—C26	120.8 (3)
C11—C12—C15	121.8 (3)	C29—C28—C27	118.8 (4)
C13—C12—C15	121.6 (3)	C29—C28—H28	120.6
C14—C13—C12	119.4 (3)	C27—C28—H28	120.6
C14—C13—H13	120.3	N21—C29—C28	123.3 (4)
C12—C13—H13	120.3	N21—C29—H29	118.3
N10—C14—C13	124.0 (3)	C28—C29—H29	118.3
N10—C14—H14	118.0	N21—C30—C31	123.3 (4)
C13—C14—H14	118.0	N21—C30—H30	118.3
C15ii—C15—C12	116.2 (5)	C31—C30—H30	118.3
C15ii—C15—H15A	108.2	C27—C31—C30	119.2 (4)
C12—C15—H15A	108.2	C27—C31—H31	120.4
C15ii—C15—H15B	108.2	C30—C31—H31	120.4
C12—C15—H15B	108.2	C30—N21—C29	117.4 (3)
H15A—C15—H15B	107.4	Fe1—O1—H1O1	121.5
C24—N20—C20	117.3 (3)	Fe1—O1—H2O1	134.5
N20—C20—C21	123.4 (4)	H1O1—O1—H2O1	102.6
N20—C20—H20	118.3	H1O2—O2—H2O2	108.6
C21—C20—H20	118.3

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1O1···O2	0.82	1.89	2.696 (4)	166
O1—H2O1···O2iii	0.82	1.87	2.672 (4)	165
O2—H1O2···N20i	0.82	1.98	2.688 (4)	144
O2—H2O2···N21ii	0.82	1.92	2.682 (4)	155

Table 1

Selected bond lengths (Å)

Fe1—O1	2.069 (3)
Fe1—N1	2.132 (3)
Fe1—N10	2.347 (3)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1O1⋯O2	0.82	1.89	2.696 (4)	166
O1—H2O1⋯O2i	0.82	1.87	2.672 (4)	165
O2—H1O2⋯N20ii	0.82	1.98	2.688 (4)	144
O2—H2O2⋯N21iii	0.82	1.92	2.682 (4)	155

Symmetry codes: (i) ; (ii) ; (iii) .