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The title compound, [(NH3)2(CH2)2][Fe(SO4)2(H2O)4], contains centrosymmetric [Fe(H2O)4(SO4)2]2− anions, with a coordination octahedron around iron(II) built up from four water mol­ecules and two sulfate groups. The anions are linked by hydrogen bonds of medium strength, forming a three-dimensional framework. The linkage is reinforced by N—H...O bridges from the centrosymmetric [NH3(CH2)2NH3]2+ cations, located in the centre of the interstices.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803004628/na6208sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803004628/na6208Isup2.hkl
Contains datablock I

CCDC reference: 209899

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.022
  • wR factor = 0.062
  • Data-to-parameter ratio = 21.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Comment top

The title compound, (I), crystallize sisostructurally with the analogous manganese compound (Chaabouni et al., 1996). The Fe atom is surrounded by six O atoms of four H2O molecules and of two SO4 groups, forming a slightly distorted octahedron. The Fe atom is placed in special Wykoff position 1a on an inversion centre. The structure is built of [Fe(H2O)4(SO4)2]2− anions, in which the SO4 tetrahedron is vertex-linked to the central Fe2+ ion sharing a common O atom (Fig. 1). Hydrogen bonds of mean strength from H2O molecules to O atoms (O2 and O3) of the SO4 groups interconnect neighbouring [Fe(H2O)4(SO4)2], forming a three-dimensional primitive framework (Fig. 2). Placed at the centre of each interstice, [NH3(CH2)2NH3]2+ cations form N—H···O bonds to six surrounding [Fe(H2O)4(SO4)2] groups. Every NH3 group bounds to two O atoms (O1 and O2) of two different SO4 groups and to one O atom (O4) of an iron–sulfur bridge. The organic ethylenediammonium cation is centrosymmetric with NH3 tails in a trans configuration. Both anionic and cationic structure parts show no deviation from the usual geometry and conformation.

Experimental top

The title compound was prepared in the course of systematic search for new `double salts' of ethylenediammonium and divalent cations with various inorganic acids. It crystallizes from aqueous solution containing iron sulfate, ethylenediamine and sulfuric acid (in ratio 1:1:1) by slow evaporation at room temperature in form of yellow crystals with dimensions up to 4 mm.

Computing details top

Data collection: MACH3 (Enraf-Nonius, 1993); cell refinement: MACH3; data reduction: MolEN (Fair, 1990); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 2002) and ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. ORTEPIII projection (Burnett & Johnson, 1996) of the title compound showing the atom-numbering scheme. Non-H atoms are shown as 50% probability ellipsoids and H atoms are drawn as circles of arbitrary radii.
[Figure 2] Fig. 2. Projection along [100] of the title compound, showing [SO4] tetrahedra (yellow), [Mn(H2O)4O2] octahedra (red), oxygen (blue), nitrogen (green), carbon (grey) and hydrogen (white) atoms. Hydrogen bonds (grey lines) interlink ethylenediammonium cations with different polyhedra.
Iron ethylenediammonium bis(sulfate) tetrahydrate top
Crystal data top
(C2H10N2)[Fe(SO4)2(H2O)4]Z = 1
Mr = 382.15F(000) = 198
Triclinic, P1Dx = 1.974 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.8350 (3) ÅCell parameters from 25 reflections
b = 7.1253 (3) Åθ = 12.3–19.3°
c = 7.2235 (4) ŵ = 1.56 mm1
α = 75.012 (4)°T = 293 K
β = 72.355 (4)°Parallelepiped, pale yellow
γ = 79.185 (4)°0.25 × 0.23 × 0.21 mm
V = 321.55 (3) Å3
Data collection top
Nonius MACH3
diffractometer
2393 reflections with I > 2σ(I)
Radiation source: fine-focus sealed X-ray tubeRint = 0.040
Graphite monochromatorθmax = 34.2°, θmin = 3.0°
ω/2θ scansh = 1010
Absorption correction: ψ scan
(MolEN; Fair, 1990)
k = 1110
Tmin = 0.686, Tmax = 0.721l = 1111
4830 measured reflections3 standard reflections every 100 reflections
2660 independent reflections intensity decay: 4.9%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.022All H-atom parameters refined
wR(F2) = 0.063 w = 1/[σ2(Fo2) + (0.0214P)2 + 0.0617P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max < 0.001
2660 reflectionsΔρmax = 0.74 e Å3
125 parametersΔρmin = 0.43 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.190 (6)
Crystal data top
(C2H10N2)[Fe(SO4)2(H2O)4]γ = 79.185 (4)°
Mr = 382.15V = 321.55 (3) Å3
Triclinic, P1Z = 1
a = 6.8350 (3) ÅMo Kα radiation
b = 7.1253 (3) ŵ = 1.56 mm1
c = 7.2235 (4) ÅT = 293 K
α = 75.012 (4)°0.25 × 0.23 × 0.21 mm
β = 72.355 (4)°
Data collection top
Nonius MACH3
diffractometer
2393 reflections with I > 2σ(I)
Absorption correction: ψ scan
(MolEN; Fair, 1990)
Rint = 0.040
Tmin = 0.686, Tmax = 0.7213 standard reflections every 100 reflections
4830 measured reflections intensity decay: 4.9%
2660 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0220 restraints
wR(F2) = 0.063All H-atom parameters refined
S = 1.07Δρmax = 0.74 e Å3
2660 reflectionsΔρmin = 0.43 e Å3
125 parameters
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*/Ueq
Fe0.00000.00000.00000.01379 (6)
S0.19821 (3)0.22418 (3)0.24875 (3)0.01323 (6)
O10.3119 (1)0.3974 (1)0.1827 (1)0.0215 (1)
O20.0033 (1)0.2640 (2)0.3890 (1)0.0256 (2)
O30.3202 (1)0.0546 (1)0.3414 (1)0.0246 (2)
O40.1634 (1)0.1884 (1)0.0675 (1)0.0220 (2)
OW10.0850 (2)0.2454 (1)0.2089 (1)0.0316 (2)
H1W10.068 (3)0.247 (3)0.327 (3)0.040 (5)*
H2W10.158 (3)0.350 (4)0.196 (3)0.045 (6)*
OW20.2627 (1)0.0627 (2)0.2374 (1)0.0243 (2)
H1W20.259 (3)0.034 (3)0.354 (3)0.042 (5)*
H2W20.380 (3)0.057 (3)0.244 (3)0.037 (5)*
C0.4514 (2)0.4182 (2)0.4187 (1)0.0200 (2)
H1C0.552 (3)0.309 (3)0.369 (3)0.033 (5)*
H2C0.352 (3)0.363 (3)0.465 (2)0.022 (4)*
N0.3282 (2)0.4960 (2)0.2425 (1)0.0209 (2)
H1N0.406 (3)0.548 (3)0.199 (3)0.032 (4)*
H2N0.273 (3)0.400 (3)0.148 (3)0.045 (6)*
H3N0.225 (3)0.588 (4)0.265 (3)0.047 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe0.01487 (9)0.01384 (8)0.01346 (8)0.00331 (6)0.00449 (6)0.00235 (6)
S0.01272 (9)0.0160 (1)0.01160 (9)0.00280 (7)0.00459 (6)0.00177 (6)
O10.0249 (3)0.0193 (3)0.0242 (3)0.0094 (3)0.0100 (3)0.0029 (3)
O20.0171 (3)0.0378 (5)0.0172 (3)0.0012 (3)0.0006 (2)0.0059 (3)
O30.0203 (3)0.0227 (3)0.0264 (4)0.0002 (3)0.0092 (3)0.0041 (3)
O40.0294 (4)0.0278 (4)0.0137 (3)0.0151 (3)0.0067 (2)0.0035 (2)
OW10.0529 (6)0.0218 (4)0.0195 (3)0.0092 (4)0.0169 (3)0.0044 (3)
OW20.0158 (3)0.0380 (5)0.0192 (3)0.0031 (3)0.0034 (2)0.0079 (3)
C0.0246 (4)0.0186 (4)0.0154 (4)0.0064 (3)0.0024 (3)0.0021 (3)
N0.0215 (4)0.0249 (4)0.0145 (3)0.0045 (3)0.0030 (3)0.0021 (3)
Geometric parameters (Å, º) top
Fe—OW1i2.1111 (9)S—O21.4699 (8)
Fe—OW12.1111 (9)S—O11.4782 (8)
Fe—O4i2.1260 (7)S—O41.4899 (7)
Fe—O42.1260 (7)C—N1.476 (1)
Fe—OW2i2.1430 (8)C—Cii1.513 (2)
Fe—OW22.1430 (8)C—H1C1.01 (2)
S—O31.4649 (8)C—H2C1.02 (2)
OW1i—Fe—OW1180.00 (4)O1—S—O4106.54 (4)
OW1i—Fe—O486.39 (4)S—O4—Fe137.20 (4)
OW1—Fe—O493.61 (4)H1W1—OW1—H2W1102 (2)
O4i—Fe—O4180.00 (4)H1W2—OW2—H2W2104 (2)
O4—Fe—OW2i89.51 (3)N—C—Cii109.7 (1)
OW1i—Fe—OW286.44 (4)Cii—C—H1C115 (1)
OW1—Fe—OW293.56 (4)Cii—C—H2C109.9 (9)
O4—Fe—OW290.49 (3)H1C—C—H2C110 (1)
OW2i—Fe—OW2180.00 (4)C—N—H1N110 (1)
O3—S—O2110.32 (5)C—N—H2N109 (2)
O3—S—O1110.17 (5)C—N—H3N114 (2)
O2—S—O1110.32 (5)H1N—N—H2N109 (2)
O3—S—O4110.57 (5)H1N—N—H3N107 (2)
O2—S—O4108.85 (5)H2N—N—H3N107 (3)
Symmetry codes: (i) x, y, z; (ii) x+1, y+1, z1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
OW1—H1W1···O2iii0.82 (2)1.94 (2)2.759 (1)174 (2)
OW1—H2W1···O1iv0.83 (2)1.91 (3)2.741 (1)176 (2)
OW2—H1W2···O3v0.82 (2)2.06 (2)2.862 (1)166 (2)
OW2—H2W2···O3vi0.80 (2)1.96 (2)2.727 (1)162 (2)
N—H1N···O1vii0.87 (2)2.08 (2)2.887 (1)154 (2)
N—H2N···O40.88 (2)1.94 (2)2.818 (1)177 (2)
N—H3N···O2viii0.89 (2)1.98 (2)2.835 (1)159 (2)
Symmetry codes: (iii) x, y, z+1; (iv) x, y1, z; (v) x, y, z1; (vi) x+1, y, z; (vii) x+1, y+1, z; (viii) x, y+1, z.

Experimental details

Crystal data
Chemical formula(C2H10N2)[Fe(SO4)2(H2O)4]
Mr382.15
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)6.8350 (3), 7.1253 (3), 7.2235 (4)
α, β, γ (°)75.012 (4), 72.355 (4), 79.185 (4)
V3)321.55 (3)
Z1
Radiation typeMo Kα
µ (mm1)1.56
Crystal size (mm)0.25 × 0.23 × 0.21
Data collection
DiffractometerNonius MACH3
diffractometer
Absorption correctionψ scan
(MolEN; Fair, 1990)
Tmin, Tmax0.686, 0.721
No. of measured, independent and
observed [I > 2σ(I)] reflections
4830, 2660, 2393
Rint0.040
(sin θ/λ)max1)0.791
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.022, 0.063, 1.07
No. of reflections2660
No. of parameters125
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)0.74, 0.43

Computer programs: MACH3 (Enraf-Nonius, 1993), MACH3, MolEN (Fair, 1990), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ATOMS (Dowty, 2002) and ORTEPIII (Burnett & Johnson, 1996), SHELXL97.

Selected bond lengths (Å) top
Fe—OW12.1111 (9)S—O11.4782 (8)
Fe—O42.1260 (7)S—O41.4899 (7)
Fe—OW22.1430 (8)C—N1.476 (1)
S—O31.4649 (8)C—Ci1.513 (2)
S—O21.4699 (8)
Symmetry code: (i) x+1, y+1, z1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
OW1—H1W1···O2ii0.82 (2)1.94 (2)2.759 (1)174 (2)
OW1—H2W1···O1iii0.83 (2)1.91 (3)2.741 (1)176 (2)
OW2—H1W2···O3iv0.82 (2)2.06 (2)2.862 (1)166 (2)
OW2—H2W2···O3v0.80 (2)1.96 (2)2.727 (1)162 (2)
N—H1N···O1vi0.87 (2)2.08 (2)2.887 (1)154 (2)
N—H2N···O40.88 (2)1.94 (2)2.818 (1)177 (2)
N—H3N···O2vii0.89 (2)1.98 (2)2.835 (1)159 (2)
Symmetry codes: (ii) x, y, z+1; (iii) x, y1, z; (iv) x, y, z1; (v) x+1, y, z; (vi) x+1, y+1, z; (vii) x, y+1, z.
 

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