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The structure of the title compound, ammonium iron(II) hydrogen bis(sulfate) dihydrate, NH4FeH(SO4)2·2H2O, is isotypic with three similar kröhnkite-type structures of type E. The Fe2+ cation is surrounded by two water mol­ecules and four partially protonated sulfate anions. The structure is completed by ammonium ions. The Fe and the N atom are located on centres of inversion.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680401373X/wm6020sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680401373X/wm6020Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](S-O) = 0.001 Å
  • H-atom completeness 89%
  • R factor = 0.018
  • wR factor = 0.049
  • Data-to-parameter ratio = 10.7

checkCIF/PLATON results

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Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT354_ALERT_3_C Short O-H Bond (0.82A) O5 - H5A ... 0.71 Ang.
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:H9 Fe1 N1 O10 S2 Atom count from the _atom_site data: H8 Fe1 N1 O10 S2 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 1 From the CIF: _chemical_formula_sum Fe H9 N O10 S2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff Fe 1.00 1.00 0.00 H 9.00 8.00 1.00 N 1.00 1.00 0.00 O 10.00 10.00 0.00 S 2.00 2.00 0.00
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97.

; top
Crystal data top
FeH9NO10S2Z = 1
Mr = 303.05F(000) = 154
Triclinic, P1Dx = 2.347 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 4.5955 (9) ÅCell parameters from 6924 reflections
b = 5.8420 (12) Åθ = 3.6–27.4°
c = 8.3811 (16) ŵ = 2.29 mm1
α = 103.678 (15)°T = 100 K
β = 98.069 (16)°Needle, colourless
γ = 95.638 (16)°0.47 × 0.22 × 0.13 mm
V = 214.43 (8) Å3
Data collection top
STOE IPDS II two-circle
diffractometer
980 independent reflections
Radiation source: fine-focus sealed tube922 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
ω scansθmax = 27.6°, θmin = 3.9°
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
h = 55
Tmin = 0.405, Tmax = 0.740k = 77
3969 measured reflectionsl = 1010
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)] = 0.018H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.049 w = 1/[σ2(Fo2) + (0.0271P)2 + 0.0862P]
where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max < 0.001
980 reflectionsΔρmax = 0.44 e Å3
92 parametersΔρmin = 0.36 e Å3
4 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.148 (9)
Special details top

Experimental. ;

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)
Fe0.00000.00000.00000.01102 (12)
O50.1993 (3)0.2180 (2)0.14161 (14)0.0145 (2)
H5A0.111 (6)0.311 (4)0.160 (3)0.025 (6)*
H5B0.344 (6)0.270 (5)0.126 (3)0.029 (6)*
S0.60037 (7)0.31653 (6)0.23937 (4)0.01068 (12)
O10.4994 (3)0.3020 (2)0.40179 (13)0.0200 (3)
O20.3409 (2)0.28480 (19)0.10850 (13)0.0154 (2)
O30.7726 (2)0.54790 (19)0.26264 (13)0.0171 (2)
O40.7750 (2)0.11876 (19)0.20058 (13)0.0142 (2)
N10.00000.00000.50000.0170 (4)
H1A0.062 (10)0.145 (4)0.572 (5)0.026 (11)*0.50
H1B0.121 (10)0.113 (7)0.504 (8)0.038 (14)*0.50
H1C0.150 (7)0.068 (8)0.460 (5)0.025 (11)*0.50
H1D0.097 (10)0.030 (10)0.593 (4)0.031 (12)*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe0.01036 (17)0.01036 (16)0.01227 (16)0.00139 (10)0.00108 (10)0.00323 (10)
O50.0122 (5)0.0139 (5)0.0204 (5)0.0032 (4)0.0047 (4)0.0087 (4)
S0.01309 (19)0.00969 (18)0.00858 (18)0.00021 (12)0.00203 (12)0.00158 (12)
O10.0311 (6)0.0155 (5)0.0123 (5)0.0046 (4)0.0117 (4)0.0001 (4)
O20.0121 (5)0.0144 (5)0.0195 (5)0.0012 (4)0.0003 (4)0.0058 (4)
O30.0216 (6)0.0125 (5)0.0153 (5)0.0044 (4)0.0061 (4)0.0005 (4)
O40.0135 (5)0.0159 (5)0.0156 (5)0.0052 (4)0.0041 (4)0.0065 (4)
N10.0214 (9)0.0133 (8)0.0139 (8)0.0001 (7)0.0025 (7)0.0034 (7)
Geometric parameters (Å, º) top
Fe—O2i2.1029 (11)S—O21.4670 (11)
Fe—O22.1029 (11)S—O41.4704 (11)
Fe—O4ii2.1105 (11)S—O11.5164 (11)
Fe—O4iii2.1105 (11)O4—Feiv2.1105 (11)
Fe—O5i2.1231 (12)N1—H1A0.908 (10)
Fe—O52.1231 (12)N1—H1B0.905 (10)
O5—H5A0.70 (3)N1—H1C0.906 (10)
O5—H5B0.77 (3)N1—H1D0.908 (10)
S—O31.4538 (11)
O2i—Fe—O2180.0Fe—O5—H5B123.6 (18)
O2i—Fe—O4ii90.99 (4)H5A—O5—H5B104 (3)
O2—Fe—O4ii89.01 (4)O3—S—O2109.79 (7)
O2i—Fe—O4iii89.01 (4)O3—S—O4113.00 (6)
O2—Fe—O4iii90.99 (4)O2—S—O4110.38 (6)
O4ii—Fe—O4iii180.00 (4)O3—S—O1109.01 (6)
O2i—Fe—O5i88.35 (4)O2—S—O1109.67 (7)
O2—Fe—O5i91.66 (5)O4—S—O1104.86 (7)
O4ii—Fe—O5i86.93 (4)S—O2—Fe132.53 (7)
O4iii—Fe—O5i93.07 (4)S—O4—Feiv131.93 (6)
O2i—Fe—O591.65 (4)H1A—N1—H1B117 (4)
O2—Fe—O588.34 (4)H1A—N1—H1C74 (4)
O4ii—Fe—O593.07 (4)H1B—N1—H1C83 (4)
O4iii—Fe—O586.93 (4)H1A—N1—H1D75 (4)
O5i—Fe—O5180.0H1B—N1—H1D54 (4)
Fe—O5—H5A120 (2)H1C—N1—H1D102 (4)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z; (iii) x1, y, z; (iv) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5A···O3v0.70 (3)2.07 (3)2.7262 (16)155 (3)
O5—H5B···O2vi0.77 (3)2.57 (3)2.9967 (16)117 (2)
O5—H5B···O3vi0.77 (3)2.59 (3)3.2335 (17)143 (2)
N1—H1A···O3vii0.91 (1)2.00 (1)2.9007 (12)175 (5)
N1—H1C···O10.91 (1)2.19 (1)3.0790 (12)168 (4)
N1—H1D···O4viii0.91 (1)1.95 (1)2.8433 (12)168 (5)
Symmetry codes: (v) x1, y1, z; (vi) x, y1, z; (vii) x1, y1, z1; (viii) x1, y, z1.
 

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