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Parabutlerite, orthorhombic FeIIISO4(OH)·2H2O, has been reinvestigated using single-crystal X-ray diffraction. The structure of parabutlerite is commensurately modulated, with a = 20.0789 (8), b = 7.4024 (7), c = 7.2294 (15) Å and q = 0.4b*. The superstructure has been determined, using a superspace approach, as having the superspace group Pnma(0β0)s0s and t0 = 1/20, and refined to R = 0.0295 for 2392 main reflections with I > 3σ(I). The structure consists of infinite chains of Fe octahedra that are linked via vertices (OH groups); these chains are encased from both sides by SO4 tetrahedra. The displacive modulation of atoms in parabutlerite is connected with a tilt of the chains around the b axis towards the adjacent chains due to the accommodation of an energetically more favorable hydrogen-bond geometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520617007156/eb5063sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520617007156/eb5063Isup2.hkl
Contains datablock I

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052520617007156/eb5063sup3.pdf
Supplementary material

B-IncStrDB reference: 13292E1LLnf

CCDC reference: 1549984

Computing details top

(I) top
Crystal data top
FeH5O7SZ = 8
Mr = 204.9F(000) = 824
Orthorhombic, Pnma(0β0)s0sDx = 2.534 Mg m3
q = 0.400000b*Mo Kα radiation, λ = 0.71073 Å
a = 20.0789 (8) ŵ = 3.17 mm1
b = 7.4024 (7) ÅT = 283 K
c = 7.2294 (15) ÅTabular, orange
V = 1074.5 (2) Å30.13 × 0.04 × 0.03 mm
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x1+1/2, −x2, x3+1/2, −x4+1/2; (3) −x1, x2+1/2, −x3, x4; (4) x1+1/2, −x2+1/2, −x3+1/2, −x4+1/2; (5) −x1, −x2, −x3, −x4; (6) x1+1/2, x2, −x3+1/2, x4+1/2; (7) x1, −x2+1/2, x3, −x4; (8) −x1+1/2, x2+1/2, x3+1/2, x4+1/2.

Data collection top
Oxford Diffraction CCD
diffractometer
11937 independent reflections
Radiation source: X-ray tube5550 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.027
ω scansθmax = 28.0°, θmin = 3.2°
Absorption correction: multi-scanh = 2626
Tmin = 0.901, Tmax = 1k = 59
31672 measured reflectionsl = 99
Refinement top
Refinement on FSecondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.053All H-atom parameters refined
wR(F2) = 0.075Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2)
S = 1.75(Δ/σ)max = 0.047
11937 reflectionsΔρmax = 1.19 e Å3
280 parametersΔρmin = 1.69 e Å3
8 restraintsExtinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)
6 constraintsExtinction coefficient: 240 (90)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.375062 (12)0.00005 (3)0.21143 (4)0.01047 (9)
S10.37768 (3)0.250.57746 (9)0.01163 (18)
S20.37334 (3)0.250.15860 (9)0.01083 (18)
O10.33547 (9)0.250.7387 (2)0.0195 (6)
O20.30588 (9)0.250.2170 (3)0.0274 (7)
O30.47584 (7)0.01074 (16)0.2304 (2)0.0283 (5)
O40.41800 (9)0.250.3120 (3)0.0210 (6)
O50.44696 (9)0.250.6243 (3)0.0282 (7)
O60.27525 (7)0.01426 (16)0.1790 (2)0.0272 (5)
O70.37696 (8)0.250.3040 (2)0.0137 (5)
O80.36230 (6)0.08811 (16)0.46558 (18)0.0172 (4)
O90.38552 (6)0.08887 (16)0.04695 (18)0.0203 (4)
O100.37494 (9)0.250.1178 (2)0.0154 (5)
H10.2482 (6)0.1067 (13)0.195 (3)0.0326*
H20.2505 (6)0.0837 (13)0.205 (3)0.0326*
H30.4994 (7)0.0871 (13)0.270 (3)0.034*
H40.4995 (7)0.1063 (13)0.268 (3)0.034*
H50.3765 (12)0.250.4299 (8)0.0165*
H60.3672 (12)0.250.0063 (10)0.0185*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.01311 (16)0.00660 (15)0.01170 (16)0.00007 (9)0.00002 (10)0.00089 (10)
S10.0147 (3)0.0098 (3)0.0104 (3)00.0019 (2)0
S20.0123 (3)0.0091 (3)0.0111 (3)00.0005 (2)0
O10.0317 (11)0.0174 (10)0.0093 (10)00.0056 (8)0
O20.0208 (11)0.0241 (11)0.0374 (15)00.0120 (10)0
O30.0159 (7)0.0219 (8)0.0471 (10)0.0012 (6)0.0056 (7)0.0051 (8)
O40.0289 (11)0.0189 (10)0.0151 (11)00.0073 (9)0
O50.0187 (10)0.0268 (11)0.0390 (14)00.0105 (9)0
O60.0125 (7)0.0210 (7)0.0481 (10)0.0003 (5)0.0018 (7)0.0078 (8)
O70.0256 (10)0.0074 (8)0.0081 (9)00.0013 (8)0
O80.0299 (8)0.0105 (6)0.0111 (7)0.0027 (5)0.0004 (5)0.0015 (6)
O90.0387 (9)0.0105 (6)0.0118 (7)0.0014 (6)0.0028 (6)0.0030 (6)
O100.0290 (11)0.0083 (8)0.0089 (9)00.0014 (8)0
Bond lengths (Å) top
AverageMinimumMaximum
Fe1—O32.042 (4)2.016 (4)2.072 (4)
Fe1—O62.036 (4)2.003 (4)2.063 (4)
Fe1—O71.972 (3)1.959 (4)1.985 (4)
Fe1—O81.980 (4)1.976 (4)1.987 (4)
Fe1—O91.997 (4)1.991 (4)2.004 (4)
Fe1—O101.978 (3)1.967 (4)1.984 (4)
S1—O11.450 (4)1.434 (5)1.457 (5)
S1—O51.452 (4)1.443 (5)1.462 (5)
S1—O81.490 (4)1.482 (4)1.509 (4)
S1—O81i1.490 (4)1.478 (4)1.501 (4)
S2—O21.464 (4)1.420 (5)1.495 (5)
S2—O41.446 (4)1.429 (5)1.463 (5)
S2—O91.479 (4)1.459 (4)1.507 (4)
S2—O91ii1.479 (4)1.462 (4)1.497 (4)
O3—H30.92 (3)0.91 (3)0.92 (3)
O3—H40.91 (4)0.90 (4)0.93 (4)
O6—H10.91 (3)0.87 (4)0.93 (4)
O6—H20.92 (3)0.89 (3)0.94 (3)
O7—H50.912 (12)0.911 (16)0.914 (16)
O7—Fe11ii1.972 (3)1.955 (4)1.986 (4)
O10—H60.914 (15)0.91 (2)0.92 (2)
O10—Fe11i1.978 (3)1.971 (4)1.987 (4)
Fe11—O312.042 (4)2.017 (4)2.070 (4)
Fe11—O612.036 (4)2.001 (4)2.059 (4)
Fe11—O811.980 (4)1.974 (4)1.985 (4)
Fe11—O911.997 (4)1.988 (4)2.002 (4)
O31—H310.92 (3)0.90 (3)0.93 (3)
O31—H410.91 (4)0.89 (4)0.92 (4)
O61—H110.91 (3)0.89 (4)0.92 (4)
O61—H210.92 (3)0.90 (3)0.93 (3)
Symmetry codes: (i) x1, x2+1/2, x3, x4; (ii) x1, x21/2, x3, x4.
 

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