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The title compound, {(C8H20N)[CdFe(CN)6(C2H8N2)2]·4H2O}n, was isolated from the aqueous system Cd2+/ethyl­ene­diamine (en)/[Fe(CN)6]3− in the presence of [Et4N]Br. The crystal structure is dominated by a one-dimensional motif, viz. a negatively charged 2,2-CT (cistrans) [–Cd(en)2—NC—Fe(CN)4—CN–]nn chain. The Cd and Fe atoms of the anion and the N atom of the cation all lie on twofold axes. The ethyl groups of the cation are equally disordered over two orientations. The cationic building block of the chain consists of a CdII atom coordinated by two chelating en ligands, and the distorted octa­hedral coordination is completed by two bridging cyano ligands in cis positions. The anionic building block is an [Fe(CN)6]3− anion in which the FeIII atom is octa­hedrally coordinated by six cyano ligands; two of the cyano ligands, in trans positions, are bridging. The uncoordinated water mol­ecules link neighbouring chains through O—H...N and N—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270106003453/fa3001sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270106003453/fa3001Isup2.hkl
Contains datablock I

CCDC reference: 605655

Comment top

Cyano complexes have been considered attractive subjects for study because of their ability to form host–guest and mineralomimetic systems (Iwamoto, 1996; Iwamoto et al., 1997; Hoskins & Robson, 1990; Dunbar & Heintz, 1997), and also because of their uses in such diverse areas as heterogeneous catalysis and sorption processes (Boellaard et al., 2002; Ayrault et al., 1998; Loos-Neskovic & Fedoroff, 1989). At present, oligomeric and polymeric cyano complexes attract the interest of both chemists and physicists from the point of view of magnetic properties (Larionova et al., 2000; Verdaguer et al., 1999; Bernhardt et al., 2005; Sato et al., 1996).

Polymeric cyano complexes can be built up of cationic and anionic building blocks linked via bridging cyano ligands; the cationic block is a complex cation coordinated by suitable, mainly N-donor, ligands (blocking ligands) and the anionic block is a complex cyano anion. The dimensionality of the cyano complex formed can be tuned to some extent by the number and type of the blocking ligands coordinated to the cationic central atom (Willett or Willet et al., 1993). Following this approach, we have investigated the system Cd2+/ethylenediamine/[Fe(CN)6]3− in the presence of [Et4N]Br (Et is ethyl) for compensation of charge differences between the respective building blocks and have occasionally isolated the title compound, [Et4N][Cd(en)2Fe(CN)6]·4H2O (en is ethylenediamine), (I), along with the main crystalline product [Et4N][Cd(en)]4[Fe(CN)6]3, (II). Compound (II) formed at all Cd:en ratios up to 1:6. It exhibits a three-dimensional crystal structure with [Et4N]+ cations placed in octahedral cavities of the cyano complex skeleton (Maĺarová et al., 2003). Our further attempts to prepare (I) were unsuccessful, but we were able to determine its structure; the results are reported here.

The structure of (I) consists of anionic chains [–Cd(en)2—NC—Fe(CN)4—CN–]nn-, [Et4N]+ cations (the Cd atom, the Fe atom and the N atom of the cation occupy special positions), and two crystalographically independent uncoordinated water molecules, which are located between the chains (Figs. 1, 2 and 3). Heretofore, besides (II), only one crystal structure based on a CdII central atom and an [Fe(CN)6]3− anion has been reported. [Me4N][CdFe(CN)6]·3H2O exhibits a three-dimensional crystal structure, and is built up of [CdN4(OH2)2]2+ octahedra and [CdN5]2+ square pyramids linked via [Fe(CN)6]3− octahedra; tetramethylammonium cations and water molecules are located in the cavities formed (Witzel et al., 2000).

The CdII atoms in (I) are six-coordinated by two chelating en molecules and two N-bound µ2-bridging cyano groups placed in cis (C) positions. As the bridging cyano ligands are in trans (T) positions in the anion, and the connectivities of both building blocks are 2, the chain is of the 2,2-CT type [for details of notation see Černák et al. (2002)]. The Cd—N bond distances are in the range 2.339 (2)–2.376 (2) Å (Table 1). Similar bond distances and N—Cd—N angles were found in the one-dimensional compound [Cd{tet}]2[Fe(CN)6]·3H2O (tet is ?; Zhang, Tong et al., 2000). The Cd—N1—C1 angle is 145.0 (2)°; such a deviation from linearity is usual in this type of structure (Zhang, Cai et al., 2000; Zhang, Tong et al., 2000). Both en ligands are in the δ conformation and exhibit typical values of geometric parameters (Yuge et al., 1995).

The FeIII atom is six-coordinated by six cyano ligands, of which two, located in trans positions, are bridging (Fig. 1). The [FeC6] octahedron is regular and the observed geometric parameters are in line with those reported for other hexacyanoferrates(III) (Witzel et al., 2000).

The tetraethylammonium cations are located between the chains; the cation is disordered about the twofold axis upon which atom N6 lies. Two crystallographically independent water molecules are interconnected via hydrogen bonds of the O—H···O type; moreover, they link neighbouring chains via O—H···N and N—H···O hydrogen bonds (Fig. 3 and Table 2). N—H···N hydrogen bonds between the chains contribute to the stability of the structure (Fig. 4 and Table 2).

Experimental top

Compound (I) crystallized from the same reaction mixture as (II). To an aqueous solution of CdCl22.5H2O (0.23 g, 1 mmol), aqueous solutions of en (0.136 ml, 2 mmol) and [Et4N]Br (0.15 g, 1 mmol) were added, and the mixture was stirred at room temperature for 10 min. To this colourless solution was added an aqueous solution of K3[Fe(CN)6] (0.33 g, 1 mmol). The resulting yellow solution was left to crystallize at two temperatures. From the solution kept at room temperature, red prismatic crystals of (II) were obtained after two days, and from the second solution, kept within the temperature range 281–286 K, yellow prismatic crystals of (I) separated after two weeks (yield 30%). Analysis calculated for C18H44CdFeN11O4 (Mr = 646.9): C 23.70, H 6.89, N 33.05%; found: C 23.82, H 6.86, N 33.42%. IR (cm−1; Nicolet Magna 750 spectrometer, KBr disc): 3430, 3358, 3295, 2934, 2122, 1604, 1463, 1186, 1001, 961, 415, 398.

Refinement top

In the tetraethylammonium cation the ethyl groups are disordered over two positions related by a twofold axis parallel to [110]. Accordingly, the site occupation factors of all atoms of the relevant ethyl groups were set to 0.5. Owing to the observed disorder, the N—C bonds in the cation were restrained to be the same, and the anisotropic displacement parameters of the C atoms of methyl groups were assumed to have the same values. The H atoms of the water molecules were located in a difference Fourier map; their positional parameters were refined, while their Uiso(H) values were set at 1.5Ueq(O). For the remaining H atoms, a riding model was used with constrained displacement parameters [C—H = 0.98 and 0.99 Å, and Uiso(H) = 1.2Ueq(C,N) and 1.5Ueq(Cmethyl)].

Computing details top

Data collection: WinExpose in X-AREA (Stoe & Cie, 2002); cell refinement: WinCell in X-AREA; data reduction: WinIntegrate in X-AREA; program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Crystal Impact, 2000).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
Fig. 1.

The structure of the anion of (I), with the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (A) y, x, −z; (B) 1 − y, 1 − x, 1/2 − z.]

Fig. 2. A view of the [Et4N]+ cation (only one disordered congener shown).

Fig. 3. Packing diagram of (I), displaying its one-dimensional character. Large black balls: Fe; large white balls: Cd; medium white balls: O; small black balls: N; small white balls: C. For the sake of clarity, the [Et4N]+ cations are represented only by N atoms (medium grey balls); H atoms have been omitted.

Fig. 4. Hydrogen bonds in (I). [Et4N]+ cations and H atoms not involved in hydrogen-bond formation have been omitted for clarity. [Symmetry codes: (A) 1 − y, 1 − x, 1/2 − z; (b) 1/2 − y, 1/2 + x, −1/4 + z; (C) 1/2 − x, 1/2 + y, 3/4 − z; (D) −y, 1 − x, 1/2 − z; (E) x, 1 + y, z; (F) y, x, 1 − z; (G) 1 − x, 1 − y, 1/2 + z; (H) y, x, −z; (I) 1 − x, 1 − y, z − 1/2; (J) 1/2 − y, 1/2 + x, 3/4 + z; (K) 1/2 − x, 1/2 + y, −1/4 − z.]
catena-poly[tetraethylammonium [tetracyanoiron(III)-µ-cyano-[bis(ethylenediamine)cadmium(II)]-µ-cyano] tetrahydrate] top
Crystal data top
(C8H20N)[CdFe(CN)6(C2H8N2)2]·4H2ODx = 1.414 Mg m3
Dm = 1.390 Mg m3
Dm measured by flotation in what?
Mr = 646.89Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P43212Cell parameters from 29777 reflections
Hall symbol: P 4nw 2abwθ = 1.9–29.4°
a = 13.0444 (5) ŵ = 1.22 mm1
c = 17.8599 (9) ÅT = 173 K
V = 3039.0 (2) Å3Prism, yellow
Z = 40.2 × 0.18 × 0.1 mm
F(000) = 1340
Data collection top
Stoe IPDS-II
diffractometer
4164 independent reflections
Radiation source: fine-focus sealed tube4043 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
Detector resolution: 150 pixels mm-1θmax = 29.4°, θmin = 1.9°
ω scansh = 1617
Absorption correction: numerical
(XPREP in SHELXTL; Sheldrick, 1996)
k = 1718
Tmin = 0.610, Tmax = 0.701l = 2424
29777 measured reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.023 w = 1/[σ2(Fo2) + (0.0383P)2 + 1.3052P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.063(Δ/σ)max = 0.001
S = 1.03Δρmax = 0.46 e Å3
4164 reflectionsΔρmin = 0.42 e Å3
191 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
6 restraintsExtinction coefficient: 0.0026 (6)
Primary atom site location: structure-invariant direct methodsAbsolute structure: refinement of absolute structure parameter (Flack, 1983)
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.02 (2)
Crystal data top
(C8H20N)[CdFe(CN)6(C2H8N2)2]·4H2OZ = 4
Mr = 646.89Mo Kα radiation
Tetragonal, P43212µ = 1.22 mm1
a = 13.0444 (5) ÅT = 173 K
c = 17.8599 (9) Å0.2 × 0.18 × 0.1 mm
V = 3039.0 (2) Å3
Data collection top
Stoe IPDS-II
diffractometer
4164 independent reflections
Absorption correction: numerical
(XPREP in SHELXTL; Sheldrick, 1996)
4043 reflections with I > 2σ(I)
Tmin = 0.610, Tmax = 0.701Rint = 0.028
29777 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.023H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.063Δρmax = 0.46 e Å3
S = 1.03Δρmin = 0.42 e Å3
4164 reflectionsAbsolute structure: refinement of absolute structure parameter (Flack, 1983)
191 parametersAbsolute structure parameter: 0.02 (2)
6 restraints
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cd0.360847 (10)0.360847 (10)0.00000.02790 (7)
Fe0.519498 (18)0.480502 (18)0.25000.02141 (8)
O10.04027 (17)0.4925 (3)0.17663 (14)0.0674 (8)
H110.095 (4)0.496 (4)0.192 (3)0.101*
H120.008 (5)0.485 (4)0.213 (3)0.101*
O20.04976 (17)0.57278 (15)0.05274 (11)0.0442 (4)
H210.036 (3)0.644 (3)0.046 (2)0.066*
H220.003 (3)0.563 (3)0.092 (2)0.066*
N10.48289 (18)0.4216 (2)0.08508 (12)0.0439 (5)
N20.28563 (17)0.48589 (19)0.27826 (15)0.0478 (5)
N30.5128 (2)0.24732 (18)0.27864 (14)0.0489 (5)
C10.49676 (17)0.44742 (18)0.14588 (12)0.0309 (4)
C20.37320 (16)0.48426 (16)0.26827 (12)0.0299 (4)
C30.51689 (18)0.33468 (16)0.26844 (11)0.0302 (4)
C40.2616 (2)0.2747 (2)0.14962 (14)0.0455 (6)
H4C0.30660.30770.18720.055*
H4D0.22350.21890.17490.055*
C50.1867 (2)0.3523 (2)0.12002 (14)0.0463 (6)
H5C0.13910.31860.08460.056*
H5D0.14590.38040.16200.056*
N40.3249 (2)0.23100 (17)0.08950 (13)0.0477 (5)
H4A0.29060.17770.06690.057*
H4B0.38520.20600.10910.057*
N50.24030 (18)0.43599 (17)0.08185 (12)0.0409 (5)
H5A0.27300.47720.11620.049*
H5B0.19450.47540.05530.049*
N60.68909 (13)0.68909 (13)0.00000.0344 (5)
C60.6950 (4)0.6864 (4)0.08420 (19)0.0428 (10)0.50
H61A0.74780.63530.09820.051*0.50
H61B0.62850.66070.10320.051*0.50
C100.7189 (6)0.7838 (10)0.1248 (6)0.0552 (9)0.50
H10A0.69450.77880.17660.083*0.50
H10B0.79310.79520.12470.083*0.50
H10C0.68470.84130.09980.083*0.50
C70.6479 (4)0.5908 (3)0.0311 (3)0.0465 (11)0.50
H71A0.58090.57520.00760.056*0.50
H71B0.63700.59790.08570.056*0.50
C110.7243 (6)0.5013 (8)0.0157 (4)0.0552 (9)0.50
H11A0.68710.43600.01610.083*0.50
H11B0.77720.50050.05460.083*0.50
H11C0.75650.51120.03330.083*0.50
C80.6044 (4)0.7705 (4)0.0169 (3)0.0434 (11)0.50
H81A0.59070.76960.07140.052*0.50
H81B0.63230.83900.00450.052*0.50
C120.5042 (8)0.7584 (6)0.0230 (4)0.0552 (9)0.50
H12A0.50720.69800.05550.083*0.50
H12B0.49080.81950.05330.083*0.50
H12C0.44920.74970.01380.083*0.50
C90.7843 (4)0.7331 (5)0.0350 (3)0.0481 (12)0.50
H91A0.79790.80110.01250.058*0.50
H91B0.84310.68810.02280.058*0.50
C130.7778 (11)0.7451 (6)0.1206 (6)0.0552 (9)0.50
H13A0.84380.76930.13980.083*0.50
H13B0.76120.67870.14330.083*0.50
H13C0.72420.79490.13310.083*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd0.02974 (8)0.02974 (8)0.02420 (9)0.00288 (7)0.00028 (6)0.00028 (6)
Fe0.02232 (11)0.02232 (11)0.01961 (15)0.00077 (11)0.00003 (10)0.00003 (10)
O10.0320 (9)0.119 (2)0.0518 (12)0.0075 (12)0.0093 (9)0.0267 (14)
O20.0546 (11)0.0333 (9)0.0446 (9)0.0056 (7)0.0088 (9)0.0052 (7)
N10.0439 (11)0.0608 (13)0.0269 (9)0.0147 (10)0.0019 (8)0.0011 (9)
N20.0297 (10)0.0459 (12)0.0678 (15)0.0026 (9)0.0093 (9)0.0137 (10)
N30.0614 (14)0.0297 (10)0.0557 (13)0.0050 (10)0.0077 (11)0.0038 (9)
C10.0309 (9)0.0379 (10)0.0241 (9)0.0049 (8)0.0032 (7)0.0027 (7)
C20.0276 (9)0.0262 (8)0.0358 (10)0.0012 (7)0.0020 (7)0.0032 (7)
C30.0343 (10)0.0271 (9)0.0291 (9)0.0011 (7)0.0009 (7)0.0004 (7)
C40.0592 (17)0.0406 (13)0.0368 (11)0.0070 (11)0.0114 (11)0.0010 (9)
C50.0400 (12)0.0589 (16)0.0400 (12)0.0067 (12)0.0102 (10)0.0052 (12)
N40.0642 (15)0.0313 (10)0.0475 (12)0.0001 (9)0.0127 (11)0.0032 (9)
N50.0422 (11)0.0405 (10)0.0399 (11)0.0074 (9)0.0025 (9)0.0029 (8)
N60.0369 (7)0.0369 (7)0.0294 (11)0.0085 (10)0.0016 (9)0.0016 (9)
C60.050 (3)0.052 (3)0.0267 (18)0.007 (2)0.0037 (19)0.0069 (19)
C100.059 (2)0.0537 (18)0.0531 (14)0.012 (3)0.0061 (16)0.0124 (16)
C70.048 (3)0.039 (2)0.052 (3)0.008 (2)0.005 (2)0.008 (2)
C110.059 (2)0.0537 (18)0.0531 (14)0.012 (3)0.0061 (16)0.0124 (16)
C80.042 (2)0.043 (2)0.045 (3)0.0018 (19)0.0012 (19)0.008 (2)
C120.059 (2)0.0537 (18)0.0531 (14)0.012 (3)0.0061 (16)0.0124 (16)
C90.046 (3)0.055 (3)0.044 (3)0.013 (2)0.003 (2)0.009 (2)
C130.059 (2)0.0537 (18)0.0531 (14)0.012 (3)0.0061 (16)0.0124 (16)
Geometric parameters (Å, º) top
Cd—N12.339 (2)N6—C61.506 (3)
Cd—N52.360 (2)N6—C81.562 (4)
Cd—N42.376 (2)C6—C101.496 (13)
Fe—C31.931 (2)C6—H61A0.9900
Fe—C11.932 (2)C6—H61B0.9900
Fe—C21.937 (2)C10—H10A0.9800
O1—H110.77 (6)C10—H10B0.9800
O1—H120.91 (6)C10—H10C0.9800
O2—H210.95 (4)C7—C111.559 (11)
O2—H220.94 (4)C7—H71A0.9900
N1—C11.151 (3)C7—H71B0.9900
N2—C21.156 (3)C11—H11A0.9800
N3—C31.155 (3)C11—H11B0.9800
C4—N41.470 (3)C11—H11C0.9800
C4—C51.502 (4)C8—C121.496 (12)
C4—H4C0.9900C8—H81A0.9900
C4—H4D0.9900C8—H81B0.9900
C5—N51.464 (4)C12—H12A0.9800
C5—H5C0.9900C12—H12B0.9800
C5—H5D0.9900C12—H12C0.9800
N4—H4A0.9200C9—C131.539 (12)
N4—H4B0.9200C9—H91A0.9900
N5—H5A0.9200C9—H91B0.9900
N5—H5B0.9200C13—H13A0.9800
N6—C71.497 (4)C13—H13B0.9800
N6—C91.504 (4)C13—H13C0.9800
N1—Cd—N1i87.74 (11)C7—N6—C8104.9 (3)
N1—Cd—N5i110.21 (8)C9—N6—C8104.1 (3)
N1—Cd—N584.86 (8)C6—N6—C8104.2 (3)
N5i—Cd—N5159.56 (11)N6—C6—C10118.4 (5)
N1—Cd—N4i171.56 (9)N6—C6—H61A107.7
N1—Cd—N486.50 (9)C10—C6—H61A107.7
N5i—Cd—N491.36 (8)N6—C6—H61B107.7
N5—Cd—N475.40 (8)C10—C6—H61B107.7
N4i—Cd—N499.86 (14)H61A—C6—H61B107.1
C3ii—Fe—C393.66 (14)C6—C10—H10A109.5
C3ii—Fe—C189.49 (9)C6—C10—H10B109.5
C3—Fe—C186.64 (9)H10A—C10—H10B109.5
C1—Fe—C1ii174.34 (14)C6—C10—H10C109.5
C3ii—Fe—C2177.54 (9)H10A—C10—H10C109.5
C3—Fe—C288.79 (9)H10B—C10—H10C109.5
C1—Fe—C290.95 (9)N6—C7—C11110.2 (5)
C1—Fe—C2ii93.10 (9)N6—C7—H71A109.6
C2—Fe—C2ii88.77 (12)C11—C7—H71A109.6
H11—O1—H12113 (5)N6—C7—H71B109.6
H21—O2—H2297 (3)C11—C7—H71B109.6
C1—N1—Cd145.0 (2)H71A—C7—H71B108.1
N1—C1—Fe175.9 (2)C7—C11—H11A109.5
N2—C2—Fe179.1 (2)C7—C11—H11B109.5
N3—C3—Fe178.2 (2)H11A—C11—H11B109.5
N4—C4—C5111.7 (2)C7—C11—H11C109.5
N4—C4—H4C109.3H11A—C11—H11C109.5
C5—C4—H4C109.3H11B—C11—H11C109.5
N4—C4—H4D109.3C12—C8—N6117.0 (5)
C5—C4—H4D109.3C12—C8—H81A108.1
H4C—C4—H4D107.9N6—C8—H81A108.1
N5—C5—C4110.9 (2)C12—C8—H81B108.1
N5—C5—H5C109.5N6—C8—H81B108.1
C4—C5—H5C109.5H81A—C8—H81B107.3
N5—C5—H5D109.5C8—C12—H12A109.5
C4—C5—H5D109.5C8—C12—H12B109.5
H5C—C5—H5D108.1H12A—C12—H12B109.5
C4—N4—Cd109.03 (16)C8—C12—H12C109.5
C4—N4—H4A109.9H12A—C12—H12C109.5
Cd—N4—H4A109.9H12B—C12—H12C109.5
C4—N4—H4B109.9N6—C9—C13114.0 (6)
Cd—N4—H4B109.9N6—C9—H91A108.8
H4A—N4—H4B108.3C13—C9—H91A108.8
C5—N5—Cd107.25 (16)N6—C9—H91B108.8
C5—N5—H5A110.3C13—C9—H91B108.8
Cd—N5—H5A110.3H91A—C9—H91B107.7
C5—N5—H5B110.3C9—C13—H13A109.5
Cd—N5—H5B110.3C9—C13—H13B109.5
H5A—N5—H5B108.5H13A—C13—H13B109.5
C7—N6—C9118.0 (3)C9—C13—H13C109.5
C7—N6—C6111.6 (3)H13A—C13—H13C109.5
C9—N6—C6112.4 (3)H13B—C13—H13C109.5
Symmetry codes: (i) y, x, z; (ii) y+1, x+1, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H11···N3iii0.77 (6)2.06 (6)2.817 (3)171 (6)
O1—H12···O2iv0.91 (6)1.87 (6)2.748 (3)162 (5)
O2—H21···N2v0.95 (4)1.90 (4)2.849 (3)178 (4)
O2—H22···O10.94 (4)1.86 (4)2.715 (3)152 (4)
N4—H4A···N3vi0.922.313.190 (4)160
N5—H5B···O20.922.283.103 (3)150
Symmetry codes: (iii) y, x+1, z+1/2; (iv) y1/2, x+1/2, z+1/4; (v) y+1/2, x+1/2, z1/4; (vi) y+1/2, x1/2, z1/4.

Experimental details

Crystal data
Chemical formula(C8H20N)[CdFe(CN)6(C2H8N2)2]·4H2O
Mr646.89
Crystal system, space groupTetragonal, P43212
Temperature (K)173
a, c (Å)13.0444 (5), 17.8599 (9)
V3)3039.0 (2)
Z4
Radiation typeMo Kα
µ (mm1)1.22
Crystal size (mm)0.2 × 0.18 × 0.1
Data collection
DiffractometerStoe IPDS-II
diffractometer
Absorption correctionNumerical
(XPREP in SHELXTL; Sheldrick, 1996)
Tmin, Tmax0.610, 0.701
No. of measured, independent and
observed [I > 2σ(I)] reflections
29777, 4164, 4043
Rint0.028
(sin θ/λ)max1)0.690
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.023, 0.063, 1.03
No. of reflections4164
No. of parameters191
No. of restraints6
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.46, 0.42
Absolute structureRefinement of absolute structure parameter (Flack, 1983)
Absolute structure parameter0.02 (2)

Computer programs: WinExpose in X-AREA (Stoe & Cie, 2002), WinCell in X-AREA, WinIntegrate in X-AREA, SHELXS86 (Sheldrick, 1985), SHELXL97 (Sheldrick, 1997), DIAMOND (Crystal Impact, 2000).

Selected geometric parameters (Å, º) top
Cd—N12.339 (2)Fe—C31.931 (2)
Cd—N52.360 (2)Fe—C11.932 (2)
Cd—N42.376 (2)Fe—C21.937 (2)
N1—Cd—N1i87.74 (11)C3—Fe—C186.64 (9)
N1—Cd—N5i110.21 (8)C1—Fe—C1ii174.34 (14)
N1—Cd—N584.86 (8)C3ii—Fe—C2177.54 (9)
N5i—Cd—N5159.56 (11)C3—Fe—C288.79 (9)
N1—Cd—N4i171.56 (9)C1—Fe—C290.95 (9)
N1—Cd—N486.50 (9)C1—Fe—C2ii93.10 (9)
N5i—Cd—N491.36 (8)C2—Fe—C2ii88.77 (12)
N5—Cd—N475.40 (8)C1—N1—Cd145.0 (2)
N4i—Cd—N499.86 (14)N1—C1—Fe175.9 (2)
C3ii—Fe—C393.66 (14)N2—C2—Fe179.1 (2)
C3ii—Fe—C189.49 (9)N3—C3—Fe178.2 (2)
Symmetry codes: (i) y, x, z; (ii) y+1, x+1, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H11···N3iii0.77 (6)2.06 (6)2.817 (3)171 (6)
O1—H12···O2iv0.91 (6)1.87 (6)2.748 (3)162 (5)
O2—H21···N2v0.95 (4)1.90 (4)2.849 (3)178 (4)
O2—H22···O10.94 (4)1.86 (4)2.715 (3)152 (4)
N4—H4A···N3vi0.922.313.190 (4)159.7
N5—H5B···O20.922.283.103 (3)150
Symmetry codes: (iii) y, x+1, z+1/2; (iv) y1/2, x+1/2, z+1/4; (v) y+1/2, x+1/2, z1/4; (vi) y+1/2, x1/2, z1/4.
 

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