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The reaction of ferric sulfate with ethyl­enediamine in the presence of acid under hydro­thermal conditions results in the title compound, (C2H10N2)2[FeIII(OH)(SO4)2](SO4)·H2O. The six-coordinate ferrate dianion participates in a μ2-hydroxo-di-μ2-sulfate-bridged chain. The component species inter­act with each other by an extensive network of O—H...O and N—H...O hydrogen bonds. The two independent FeIII atoms lie on sites of \overline{1} symmetry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805020866/hb6234sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805020866/hb6234Isup2.hkl
Contains datablock I

CCDC reference: 282365

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.028
  • wR factor = 0.081
  • Data-to-parameter ratio = 11.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 8 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 14 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.840(10) ...... 3.00 su-Rat O1W -H1W2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat N1 -H1N1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.96(3), Rep 0.950(10) ...... 3.00 su-Rat C1 -H1A 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.840(10) ...... 3.00 su-Rat O1W -H2# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat N1 -H3# 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.98(3), Rep 1.990(10) ...... 3.00 su-Rat H2# -O7 1.555 1.545
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
checkCIF publication errors
Alert level A PUBL023_ALERT_1_A There is a mismatched ^ on line 131 [Fe(OH)(SO~4~)~2~]~n~ chain whose Fe^III atoms are bridged by the hydroxo and If you require a ^ then it should be escaped with a \, i.e. \^ Otherwise there must be a matching closing ~, e.g. ^12^C
1 ALERT level A = Data missing that is essential or data in wrong format 0 ALERT level G = General alerts. Data that may be required is missing

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

catena-Poly[[bis(ethane-1,2-diaminium) [ferrate(III)-µ-hydroxo-κ2O:O-di-µ-sulfato-κ4O:O']] sulfate monohydrate] top
Crystal data top
(C2H10N2)2[Fe(OH)(SO4)2](SO4)·2H2OZ = 2
Mr = 503.29F(000) = 522
Triclinic, P1Dx = 2.029 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.1352 (4) ÅCell parameters from 4504 reflections
b = 8.7869 (5) Åθ = 2.3–28.4°
c = 13.1860 (7) ŵ = 1.38 mm1
α = 88.659 (1)°T = 295 K
β = 85.782 (1)°Plate, yellow
γ = 88.145 (1)°0.25 × 0.06 × 0.04 mm
V = 823.86 (8) Å3
Data collection top
Bruker APEX area-detector
diffractometer
3695 independent reflections
Radiation source: fine-focus sealed tube3324 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
φ and ω scansθmax = 27.5°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 99
Tmin = 0.795, Tmax = 0.947k = 1111
9220 measured reflectionsl = 1617
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028Hydrogen site location: difference Fourier map
wR(F2) = 0.081All H-atom parameters refined
S = 1.04 w = 1/[σ2(Fo2) + (0.0499P)2 + 0.2749P]
where P = (Fo2 + 2Fc2)/3
3695 reflections(Δ/σ)max = 0.001
330 parametersΔρmax = 0.43 e Å3
23 restraintsΔρmin = 0.32 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.50000.50000.50000.0130 (1)
Fe20.00000.50000.50000.0121 (1)
S10.26550 (6)0.55848 (5)0.29144 (4)0.01369 (12)
S20.23751 (6)0.79738 (5)0.54691 (4)0.01315 (12)
S30.73865 (7)0.85050 (6)0.07837 (4)0.01864 (13)
O10.4351 (2)0.5136 (2)0.3477 (1)0.0195 (3)
O20.0957 (2)0.4938 (2)0.3502 (1)0.0172 (3)
O30.2837 (2)0.4921 (2)0.1922 (1)0.0252 (3)
O40.2409 (2)0.7239 (2)0.2870 (1)0.0246 (3)
O50.4179 (2)0.7171 (2)0.5119 (1)0.0202 (3)
O60.0775 (2)0.7155 (2)0.5086 (1)0.0174 (3)
O70.2415 (2)0.9501 (2)0.5010 (1)0.0213 (3)
O80.2198 (2)0.8005 (2)0.6568 (1)0.0245 (3)
O90.2475 (2)0.4344 (2)0.5435 (1)0.0149 (3)
O100.7026 (3)0.8595 (2)0.0293 (1)0.0431 (5)
O110.9066 (2)0.7535 (2)0.0953 (1)0.0335 (4)
O120.5764 (2)0.7824 (2)0.1364 (1)0.0267 (4)
O130.7678 (2)1.0042 (2)0.1163 (1)0.0294 (4)
O1w0.1502 (2)0.1695 (2)0.6476 (1)0.0256 (3)
N10.5114 (3)0.0239 (2)0.6893 (2)0.0234 (4)
N20.8743 (3)0.0060 (2)0.8029 (2)0.0276 (4)
N30.7895 (3)0.4967 (2)0.2158 (2)0.0231 (4)
N40.7192 (3)0.2633 (2)0.0123 (2)0.0229 (4)
C10.6050 (3)0.1178 (3)0.7269 (2)0.0255 (5)
C20.8140 (3)0.1085 (3)0.7246 (2)0.0244 (5)
C30.8286 (3)0.3798 (3)0.1378 (2)0.0232 (5)
C40.6896 (3)0.3944 (3)0.0565 (2)0.0222 (4)
H9o0.239 (3)0.3481 (15)0.571 (2)0.021 (6)*
H1w10.038 (2)0.202 (3)0.652 (2)0.04 (1)*
H1w20.150 (4)0.110 (3)0.598 (2)0.03 (1)*
H1n10.522 (5)0.095 (3)0.731 (2)0.05 (1)*
H1n20.393 (2)0.010 (4)0.692 (3)0.06 (1)*
H1n30.553 (4)0.053 (3)0.629 (1)0.04 (1)*
H2n10.841 (4)0.087 (2)0.792 (2)0.03 (1)*
H2n20.993 (2)0.010 (4)0.808 (2)0.04 (1)*
H2n30.818 (4)0.032 (3)0.860 (1)0.04 (1)*
H3n10.806 (4)0.585 (2)0.189 (2)0.04 (1)*
H3n20.874 (3)0.492 (3)0.258 (2)0.04 (1)*
H3n30.685 (3)0.502 (4)0.251 (2)0.06 (1)*
H4n10.827 (2)0.267 (3)0.045 (2)0.04 (1)*
H4n20.634 (3)0.260 (4)0.054 (2)0.04 (1)*
H4n30.722 (4)0.177 (2)0.020 (2)0.04 (1)*
H1a0.587 (4)0.195 (3)0.679 (2)0.04 (1)*
H1b0.551 (3)0.141 (3)0.793 (1)0.03 (1)*
H2a0.877 (4)0.203 (2)0.737 (2)0.05 (1)*
H2b0.863 (3)0.074 (3)0.659 (1)0.03 (1)*
H3a0.820 (4)0.288 (2)0.176 (2)0.02 (1)*
H3b0.952 (2)0.399 (3)0.111 (2)0.05 (1)*
H4a0.566 (2)0.397 (3)0.087 (2)0.02 (1)*
H4b0.708 (4)0.484 (2)0.017 (2)0.04 (1)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0083 (2)0.0142 (2)0.0164 (2)0.0000 (1)0.0007 (1)0.0004 (2)
Fe20.0085 (2)0.0142 (2)0.0136 (2)0.0012 (1)0.0016 (1)0.0002 (1)
S10.0114 (2)0.0167 (2)0.0128 (2)0.0002 (2)0.0003 (2)0.0008 (2)
S20.0118 (2)0.0127 (2)0.0151 (2)0.0009 (2)0.0012 (2)0.0007 (2)
S30.0187 (3)0.0206 (3)0.0168 (3)0.0043 (2)0.0015 (2)0.0015 (2)
O10.013 (1)0.029 (1)0.017 (1)0.001 (1)0.0017 (1)0.002 (1)
O20.013 (1)0.024 (1)0.015 (1)0.005 (1)0.000 (1)0.001 (1)
O30.025 (1)0.035 (1)0.016 (1)0.002 (1)0.001 (1)0.005 (1)
O40.025 (1)0.017 (1)0.031 (1)0.000 (1)0.001 (1)0.004 (1)
O50.013 (1)0.016 (1)0.031 (1)0.000 (1)0.001 (1)0.003 (1)
O60.014 (1)0.016 (1)0.023 (1)0.002 (1)0.006 (1)0.001 (1)
O70.023 (1)0.013 (1)0.028 (1)0.001 (1)0.000 (1)0.002 (1)
O80.023 (1)0.035 (1)0.017 (1)0.005 (1)0.001 (1)0.003 (1)
O90.010 (1)0.015 (1)0.020 (1)0.001 (1)0.002 (1)0.003 (1)
O100.05 (1)0.061 (1)0.017 (1)0.018 (1)0.006 (1)0.006 (1)
O110.023 (1)0.027 (1)0.048 (1)0.004 (1)0.004 (1)0.003 (1)
O120.021 (1)0.035 (1)0.024 (1)0.011 (1)0.001 (1)0.002 (1)
O130.030 (1)0.019 (1)0.041 (1)0.004 (1)0.011 (1)0.002 (1)
O1w0.026 (1)0.022 (1)0.029 (1)0.004 (1)0.006 (1)0.000 (1)
N10.017 (1)0.027 (1)0.027 (1)0.001 (1)0.004 (1)0.004 (1)
N20.025 (1)0.028 (1)0.032 (1)0.008 (1)0.011 (1)0.006 (1)
N30.025 (1)0.025 (1)0.020 (1)0.001 (1)0.005 (1)0.000 (1)
N40.022 (1)0.027 (1)0.021 (1)0.001 (1)0.003 (1)0.003 (1)
C10.022 (1)0.024 (1)0.032 (1)0.004 (1)0.008 (1)0.000 (1)
C20.021 (1)0.026 (1)0.027 (1)0.003 (1)0.004 (1)0.002 (1)
C30.023 (1)0.026 (1)0.021 (1)0.004 (1)0.003 (1)0.001 (1)
C40.023 (1)0.024 (1)0.020 (1)0.003 (1)0.004 (1)0.001 (1)
Geometric parameters (Å, º) top
Fe1—O12.094 (1)N4—C41.483 (3)
Fe1—O1i2.094 (1)C1—C21.494 (3)
Fe1—O51.983 (1)C3—C41.513 (3)
Fe1—O5i1.983 (1)O9—H9o0.84 (1)
Fe1—O91.951 (1)O1w—H1w10.84 (1)
Fe1—O9i1.951 (1)O1w—H1w20.84 (1)
Fe2—O22.044 (1)N1—H1n10.85 (1)
Fe2—O2ii2.044 (1)N1—H1n20.85 (1)
Fe2—O61.998 (1)N1—H1n30.86 (1)
Fe2—O6ii1.998 (1)N2—H2n10.86 (1)
Fe2—O91.962 (1)N2—H2n20.85 (1)
Fe2—O9ii1.962 (1)N2—H2n30.85 (1)
S1—O31.441 (2)N3—H3n10.85 (1)
S1—O41.458 (2)N3—H3n20.85 (1)
S1—O11.502 (1)N3—H3n30.85 (1)
S1—O21.509 (1)N4—H4n10.86 (1)
S2—O81.446 (2)N4—H4n20.86 (1)
S2—O71.459 (2)N4—H4n30.86 (1)
S2—O61.493 (1)C1—H1a0.95 (1)
S2—O51.496 (2)C1—H1b0.95 (1)
S3—O101.461 (2)C2—H2a0.95 (1)
S3—O111.475 (2)C2—H2b0.95 (1)
S3—O121.475 (2)C3—H3a0.94 (1)
S3—O131.477 (2)C3—H3b0.94 (1)
N1—C11.486 (3)C4—H4a0.94 (1)
N2—C21.482 (3)C4—H4b0.94 (1)
N3—C31.477 (3)
O1—Fe1—O1i180N4—C4—C3108.9 (2)
O1—Fe1—O587.99 (6)H1w1—O1w—H1w2102 (3)
O1—Fe1—O5i92.01 (6)C1—N1—H1n1110 (2)
O1—Fe1—O991.53 (6)C1—N1—H1n2108 (2)
O1—Fe1—O9i88.47 (6)H1n1—N1—H1n2104 (3)
O5—Fe1—O5i180C1—N1—H1n3114 (2)
O5—Fe1—O991.13 (6)H1n1—N1—H1n3110 (3)
O5—Fe1—O9i88.87 (6)H1n2—N1—H1n3111 (3)
O9i—Fe1—O9180C2—N2—H2n1113 (2)
O2—Fe2—O2ii180C2—N2—H2n2113 (2)
O2—Fe2—O690.99 (6)H2n1—N2—H2n2108 (3)
O2—Fe2—O6ii89.00 (6)C2—N2—H2n3108 (2)
O2—Fe2—O991.61 (6)H2n1—N2—H2n3106 (3)
O2—Fe2—O9ii88.39 (6)H2n2—N2—H2n3110 (3)
O6—Fe2—O6ii180C3—N3—H3n1109 (2)
O6—Fe2—O988.39 (6)C3—N3—H3n2110 (2)
O6—Fe2—O9ii91.61 (6)H3n1—N3—H3n2102 (3)
O9—Fe2—O9ii180C3—N3—H3n3121 (2)
O3—S1—O4112.8 (1)H3n1—N3—H3n3106 (3)
O3—S1—O1109.3 (1)H3n2—N3—H3n3106 (3)
O4—S1—O1110.2 (1)C4—N4—H4n1110 (2)
O3—S1—O2108.5 (1)C4—N4—H4n2112 (2)
O4—S1—O2108.3 (1)H4n1—N4—H4n2110 (3)
O1—S1—O2107.7 (1)C4—N4—H4n3113 (2)
O8—S2—O7112.1 (1)H4n1—N4—H4n3104 (3)
O8—S2—O6110.2 (1)H4n2—N4—H4n3107 (3)
O7—S2—O6108.7 (1)N1—C1—H1a107 (2)
O8—S2—O5109.7 (1)C2—C1—H1a103 (2)
O7—S2—O5107.0 (1)N1—C1—H1b108 (2)
O6—S2—O5108.9 (1)C2—C1—H1b112 (2)
O10—S3—O11111.3 (1)H1a—C1—H1b113 (2)
O10—S3—O12109.1 (1)N2—C2—H2a105 (2)
O11—S3—O12107.9 (1)C1—C2—H2a114 (2)
O10—S3—O13110.1 (1)N2—C2—H2b109 (2)
O11—S3—O13108.7 (1)C1—C2—H2b110 (2)
O12—S3—O13109.7 (1)H2a—C2—H2b106 (2)
S1—O1—Fe1136.20 (9)N3—C3—H3a103 (2)
S1—O2—Fe2132.86 (8)C4—C3—H3a113 (2)
S2—O5—Fe1134.20 (9)N3—C3—H3b104 (2)
S2—O6—Fe2137.17 (9)C4—C3—H3b112 (2)
Fe1—O9—Fe2131.52 (7)H3a—C3—H3b113 (2)
Fe1—O9—H9o117 (2)N4—C4—H4a111 (2)
Fe2—O9—H9o109 (2)C3—C4—H4a110 (2)
N1—C1—C2113.3 (2)N4—C4—H4b107 (2)
N2—C2—C1112.3 (2)C3—C4—H4b111 (2)
N3—C3—C4111.1 (2)H4a—C4—H4b109 (2)
O3—S1—O1—Fe1158.8 (1)O1—Fe1—O5—S295.0 (1)
O4—S1—O1—Fe176.8 (2)O1i—Fe1—O5—S285.0 (1)
O2—S1—O1—Fe141.1 (2)O8—S2—O6—Fe275.2 (2)
O9i—Fe1—O1—S1144.2 (1)O7—S2—O6—Fe2161.5 (1)
O9—Fe1—O1—S135.8 (1)O5—S2—O6—Fe245.3 (2)
O5i—Fe1—O1—S1124.7 (1)O9—Fe2—O6—S28.9 (1)
O5—Fe1—O1—S155.3 (1)O9ii—Fe2—O6—S2171.1 (1)
O3—S1—O2—Fe2168.0 (1)O2ii—Fe2—O6—S279.5 (1)
O4—S1—O2—Fe269.4 (1)O2—Fe2—O6—S2100.5 (1)
O1—S1—O2—Fe249.8 (1)O5i—Fe1—O9—Fe2132.2 (1)
O9—Fe2—O2—S149.7 (1)O5—Fe1—O9—Fe247.8 (1)
O9ii—Fe2—O2—S1130.3 (1)O1—Fe1—O9—Fe240.2 (1)
O6ii—Fe2—O2—S1141.3 (1)O1i—Fe1—O9—Fe2139.8 (1)
O6—Fe2—O2—S138.7 (1)O6ii—Fe2—O9—Fe1134.3 (1)
O8—S2—O5—Fe180.2 (1)O6—Fe2—O9—Fe145.7 (1)
O7—S2—O5—Fe1157.9 (1)O2ii—Fe2—O9—Fe1134.7 (1)
O6—S2—O5—Fe140.5 (2)O2—Fe2—O9—Fe145.3 (1)
O9i—Fe1—O5—S2176.5 (1)N1—C1—C2—N271.2 (3)
O9—Fe1—O5—S23.5 (1)N3—C3—C4—N4172.8 (2)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9o···O1w0.84 (1)1.94 (1)2.757 (2)164 (2)
O1w—H1w1···O4ii0.84 (1)2.18 (1)2.988 (2)163 (3)
O1w—H1w2···O7iii0.84 (1)1.99 (1)2.790 (2)159 (3)
N1—H1n1···O12i0.85 (1)2.14 (2)2.912 (3)151 (3)
N1—H1n2···O8iii0.85 (1)2.32 (3)2.966 (3)132 (3)
N1—H1n3···O7i0.86 (1)2.17 (2)2.967 (3)153 (3)
N1—H1n2···O1w0.85 (1)2.30 (3)2.923 (3)130 (3)
N2—H2n1···O4i0.86 (1)2.04 (1)2.847 (3)158 (3)
N2—H2n2···O13iv0.85 (1)2.05 (2)2.840 (3)155 (3)
N2—H2n3···O10v0.85 (1)1.88 (1)2.714 (3)165 (3)
N3—H3n1···O110.85 (1)2.02 (1)2.842 (3)161 (3)
N3—H3n2···O2vi0.85 (1)2.07 (1)2.912 (2)174 (3)
N3—H3n3···O10.85 (1)2.12 (1)2.964 (2)176 (3)
N4—H4n1···O11vii0.86 (1)1.97 (1)2.811 (3)168 (3)
N4—H4n2···O12viii0.86 (1)1.96 (1)2.807 (3)169 (3)
N4—H4n3···O13iii0.86 (1)1.99 (1)2.834 (3)165 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x, y1, z; (iv) x+2, y+1, z+1; (v) x, y1, z+1; (vi) x+1, y, z; (vii) x+2, y+1, z; (viii) x+1, y+1, z.
 

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