Open with JSmol

A commensurately modulated structure of parabutlerite, FeIIISO4(OH).2H2O

Authors:

Plasil, Jakub; Petricek, Vaclav; Majzlan, Juraj

Journal:

Acta Crystallographica Section B 73 856-862 (2017)

DOI:

https://doi.org/10.1107/S2052520617007156

B-IncStrDB ID: 13292ElLLnf Entry date: 2017-09-29 Last revision: 2021-12-12

Download CIF
Open in JSmol

I

Chemical data

Structural Formula Sum: Fe1 H5 O7 S1 [ Help ]

Formula weight: 204.9 Da [ Help ]

Crystallographic data and experimental details

Crystal system: orthorhombic [ Help ]

Superspace group name: Pnma(0β0)s0s [ Help ]

Symmetry operations of the superspace group: [ Help ]

Operation code Operation in algebraic form
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

a: 20.0789(8) Å [ Help ]

b: 7.4024(7) Å [ Help ]

c: 7.2294(15) Å [ Help ]

α: 90 ° [ Help ]

β: 90 ° [ Help ]

γ: 90 ° [ Help ]

Volume: 1074.5(2) Å3 [ Help ]

Modulation dimension: 1 [ Help ]

Measured independent wave vectors: [ Help ]

Wave vector id q_x q_y q_z
1 0.000000 0.400000 0.000000

Z: 8 [ Help ]

Cell measurement temperature: 283 K [ Help ]

μ: 3.166 mm-1 [ Help ]

Absorption correction type: multi-scan [ Help ]

Minimum transmission factor: 0.901 [ Help ]

Maximum transmission factor: 1 [ Help ]

Refinement details

Matrix type used for the least-squares: full [ Help ]

Total nb. of reflections: 11937 [ Help ]

Nb. of observed reflections: 5550 [ Help ]

Intense reflections threshold: I>3σ(I) [ Help ]

Refinement based on: F [ Help ]

R(obs): 0.0531 [ Help ]

wR(obs): 0.0622 [ Help ]

R(all): 0.1185 [ Help ]

wR(all): 0.0754 [ Help ]

S(all): 1.75 [ Help ]

S(obs): 2.14 [ Help ]

Nb. of reflections: 11937 [ Help ]

Nb. of parameters: 280 [ Help ]

Number of restraints: 8 [ Help ]

Number of constraints: 6 [ Help ]

Weighting scheme: sigma [ Help ]

Weighting scheme remarks: w=1/(σ2(F)+0.0001F2) [ Help ]

Refinement of hydrogen atoms: refall [ Help ]

Δ/σ(max): 0.0471 [ Help ]

Δ/σ(mean): 0.0072 [ Help ]

Δρ(max): 1.19 e_Å-3 [ Help ]

Δρ(min): -1.69 e_Å-3 [ Help ]

Extinction method: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) [ Help ]

Extinction coefficient: 240(90) [ Help ]

Structural Information

Average Structure: [ Help ]

Atom site label Atom symbol x y z ADP type Uiso/equiv Symmetry multiplicity Occupancy Coords from (d)iffraction or (c)alculated Coords restraints or constraints Disordered cluster Disordered group
Fe1 Fe 0.375062(12) -0.00005(3) 0.21143(4) Uani 0.01047(9) 8 1 d ? ? ?
S1 S 0.37768(3) 0.25 0.57746(9) Uani 0.01163(18) 4 1 d ? ? ?
S2 S 0.37334(3) -0.25 -0.15860(9) Uani 0.01083(18) 4 1 d ? ? ?
O1 O 0.33547(9) 0.25 0.7387(2) Uani 0.0195(6) 4 1 d ? ? ?
O2 O 0.30588(9) -0.25 -0.2170(3) Uani 0.0274(7) 4 1 d ? ? ?
O3 O 0.47584(7) 0.01074(16) 0.2304(2) Uani 0.0283(5) 8 1 d ? ? ?
O4 O 0.41800(9) -0.25 -0.3120(3) Uani 0.0210(6) 4 1 d ? ? ?
O5 O 0.44696(9) 0.25 0.6243(3) Uani 0.0282(7) 4 1 d ? ? ?
O6 O 0.27525(7) -0.01426(16) 0.1790(2) Uani 0.0272(5) 8 1 d ? ? ?
O7 O 0.37696(8) -0.25 0.3040(2) Uani 0.0137(5) 4 1 d ? ? ?
O8 O 0.36230(6) 0.08811(16) 0.46558(18) Uani 0.0172(4) 8 1 d ? ? ?
O9 O 0.38552(6) -0.08887(16) -0.04695(18) Uani 0.0203(4) 8 1 d ? ? ?
O10 O 0.37494(9) 0.25 0.1178(2) Uani 0.0154(5) 4 1 d ? ? ?
H1 H 0.2482(6) -0.1067(13) 0.195(3) Uiso 0.0326 8 1 d ? ? ?
H2 H 0.2505(6) 0.0837(13) 0.205(3) Uiso 0.0326 8 1 d ? ? ?
H3 H 0.4994(7) -0.0871(13) 0.270(3) Uiso 0.034 8 1 d ? ? ?
H4 H 0.4995(7) 0.1063(13) 0.268(3) Uiso 0.034 8 1 d ? ? ?
H5 H 0.3765(12) -0.25 0.4299(8) Uiso 0.0165 4 1 d ? ? ?
H6 H 0.3672(12) 0.25 -0.0063(10) Uiso 0.0185 4 1 d ? ? ?

ADP components: [ Help ]

Atom site label Atom site symbol U11 U22 U33 U12 U13 U23
Fe1 Fe 0.01311(16) 0.00660(15) 0.01170(16) -0.00007(9) 0.00002(10) -0.00089(10)
S1 S 0.0147(3) 0.0098(3) 0.0104(3) 0 -0.0019(2) 0
S2 S 0.0123(3) 0.0091(3) 0.0111(3) 0 -0.0005(2) 0
O1 O 0.0317(11) 0.0174(10) 0.0093(10) 0 0.0056(8) 0
O2 O 0.0208(11) 0.0241(11) 0.0374(15) 0 -0.0120(10) 0
O3 O 0.0159(7) 0.0219(8) 0.0471(10) -0.0012(6) -0.0056(7) 0.0051(8)
O4 O 0.0289(11) 0.0189(10) 0.0151(11) 0 0.0073(9) 0
O5 O 0.0187(10) 0.0268(11) 0.0390(14) 0 -0.0105(9) 0
O6 O 0.0125(7) 0.0210(7) 0.0481(10) 0.0003(5) -0.0018(7) -0.0078(8)
O7 O 0.0256(10) 0.0074(8) 0.0081(9) 0 0.0013(8) 0
O8 O 0.0299(8) 0.0105(6) 0.0111(7) -0.0027(5) 0.0004(5) -0.0015(6)
O9 O 0.0387(9) 0.0105(6) 0.0118(7) -0.0014(6) 0.0028(6) -0.0030(6)
O10 O 0.0290(11) 0.0083(8) 0.0089(9) 0 -0.0014(8) 0

Fourier Wave Vectors (explicit: q_x,q_y,q_z or coefficients: q_1,q_2,...): [ Help ]

Wave vector code q_1
1 1
2 2

Definition of the displacive (translational) Fourier series: [ Help ]

Modulation code Atom site label Displacement axis Wave vector code
Fe1x1 Fe1 x 1
Fe1y1 Fe1 y 1
Fe1z1 Fe1 z 1
Fe1x2 Fe1 x 2
Fe1y2 Fe1 y 2
fE1z2 Fe1 z 2
S1x1 S1 x 1
S1y1 S1 y 1
S1z1 S1 z 1
S1x2 S1 x 2
S1y2 S1 y 2
S1z2 S1 z 2
S2x1 S2 x 1
S2y1 S2 y 1
S2z1 S2 z 1
S2x2 S2 x 2
S2y2 S2 y 2
S2z2 S2 z 2
O1x1 O1 x 1
O1y1 O1 y 1
O1z1 O1 z 1
O1x2 O1 x 2
O1y2 O1 y 2
O1z2 O1 z 2
O2x1 O2 x 1
O2y1 O2 y 1
O2z1 O2 z 1
O2x2 O2 x 2
O2y2 O2 y 2
O2z2 O2 z 2
O3x1 O3 x 1
O3y1 O3 y 1
O3z1 O3 z 1
O3x2 O3 x 2
O3y2 O3 y 2
O3z2 O3 z 2
O4x1 O4 x 1
O4y1 O4 y 1
O4z1 O4 z 1
O4x2 O4 x 2
O4y2 O4 y 2
O4z2 O4 z 2
O5x1 O5 x 1
O5y1 O5 y 1
O5z1 O5 z 1
O5x2 O5 x 2
O5y2 O5 y 2
O5z2 O5 z 2
O6x1 O6 x 1
O6y1 O6 y 1
O6z1 O6 z 1
O6x2 O6 x 2
O6y2 O6 y 2
O6z2 O6 z 2
O7x1 O7 x 1
O7y1 O7 y 1
O7z1 O7 z 1
O7x2 O7 x 2
O7y2 O7 y 2
O7z2 O7 z 2
O8x1 O8 x 1
O8y1 O8 y 1
O8z1 O8 z 1
O8x2 O8 x 2
O8y2 O8 y 2
O8z2 O8 z 2
O9x1 O9 x 1
O9y1 O9 y 1
O9z1 O9 z 1
O9x2 O9 x 2
O9y2 O9 y 2
O9z2 O9 z 2
O10x1 O10 x 1
O10y1 O10 y 1
O10z1 O10 z 1
O10x2 O10 x 2
O10y2 O10 y 2
O10z2 O10 z 2
H1x1 H1 x 1
H1y1 H1 y 1
H1z1 H1 z 1
H1x2 H1 x 2
H1y2 H1 y 2
H1z2 H1 z 2
H2x1 H2 x 1
H2y1 H2 y 1
H2z1 H2 z 1
H2x2 H2 x 2
H2y2 H2 y 2
H2z2 H2 z 2
H3x1 H3 x 1
H3y1 H3 y 1
H3z1 H3 z 1
H3x2 H3 x 2
H3y2 H3 y 2
H3z2 H3 z 2
H4x1 H4 x 1
H4y1 H4 y 1
H4z1 H4 z 1
H4x2 H4 x 2
H4y2 H4 y 2
H4z2 H4 z 2
H5x1 H5 x 1
H5y1 H5 y 1
H5z1 H5 z 1
H5x2 H5 x 2
H5y2 H5 y 2
H5z2 H5 z 2
H6x1 H6 x 1
H6y1 H6 y 1
H6z1 H6 z 1
H6x2 H6 x 2
H6y2 H6 y 2
H6z2 H6 z 2

Displacive (translational) Fourier coefficients: [ Help ]

Modulation code Cosine coefficient Sine coefficient
Fe1x1 -0.002614(16) 0.005712(15)
Fe1y1 -0.00040(4) -0.00183(4)
Fe1z1 -0.00593(5) -0.00004(5)
Fe1x2 -0.00061(2) 0.002375(18)
Fe1y2 -0.00094(6) 0.00045(5)
fE1z2 0.00159(7) -0.00091(7)
S1x1 -0.00240(4) 0
S1y1 0 -0.01466(11)
S1z1 0.00371(12) 0
S1x2 -0.00314(5) 0
S1y2 0 0.00223(15)
S1z2 0.00143(17) 0
S2x1 0.00015(4) 0
S2y1 0 0.00809(10)
S2z1 0.00016(12) 0
S2x2 0.00207(5) 0
S2y2 0 0.00064(14)
S2z2 -0.00179(16) 0
O1x1 -0.01131(12) 0
O1y1 0 -0.0080(3)
O1z1 -0.0129(3) 0
O1x2 -0.00403(15) 0
O1y2 0 0.0069(4)
O1z2 -0.0026(4) 0
O2x1 -0.00640(12) 0
O2y1 0 0.0462(4)
O2z1 0.0471(4) 0
O2x2 0.00523(15) 0
O2y2 0 0.0137(4)
O2z2 -0.0280(5) 0
O3x1 -0.00193(8) 0.00435(8)
O3y1 0.0309(3) -0.0087(3)
O3z1 -0.0099(3) 0.0276(3)
O3x2 -0.00093(10) 0.00252(10)
O3y2 -0.0012(3) -0.0030(3)
O3z2 0.0059(3) -0.0025(3)
O4x1 -0.01092(12) 0
O4y1 0 -0.0029(3)
O4z1 -0.0259(3) 0
O4x2 0.00732(15) 0
O4y2 0 -0.0039(4)
O4z2 0.0126(4) 0
O5x1 -0.00567(12) 0
O5y1 0 -0.0463(3)
O5z1 0.0367(4) 0
O5x2 -0.00363(15) 0
O5y2 0 0.0065(4)
O5z2 0.0037(5) 0
O6x1 -0.00209(8) 0.00624(8)
O6y1 -0.0300(2) -0.0090(2)
O6z1 -0.0002(3) -0.0357(3)
O6x2 -0.00115(10) 0.00192(10)
O6y2 0.0006(3) 0.0009(3)
O6z2 0.0095(3) 0.0026(4)
O7x1 0.00775(11) 0
O7y1 0 -0.0047(3)
O7z1 -0.0048(3) 0
O7x2 0.00198(14) 0
O7y2 0 0.0002(4)
O7z2 -0.0010(4) 0
O8x1 -0.00063(8) -0.01051(8)
O8y1 -0.00124(19) -0.00197(20)
O8z1 -0.0041(2) -0.0083(2)
O8x2 -0.00124(10) 0.00232(11)
O8y2 -0.0011(3) 0.0005(3)
O8z2 0.0036(3) 0.0007(3)
O9x1 0.00367(9) 0.01390(9)
O9y1 0.00052(20) -0.0040(2)
O9z1 -0.0052(2) 0.0052(2)
O9x2 -0.00365(11) 0.00028(11)
O9y2 0.0023(3) -0.0006(3)
O9z2 -0.0010(3) -0.0006(3)
O10x1 -0.01678(13) 0
O10y1 0 -0.0008(3)
O10z1 -0.0058(3) 0
O10x2 -0.00260(15) 0
O10y2 0 -0.0027(4)
O10z2 0.0039(4) 0
H1x1 -0.0005(8) 0.0074(8)
H1y1 -0.0218(18) 0.0006(16)
H1z1 0.023(3) -0.026(3)
H1x2 -0.0017(9) -0.0031(9)
H1y2 0.0078(18) 0.0155(18)
H1z2 0.021(3) 0.008(3)
H2x1 -0.0014(8) 0.0083(8)
H2y1 -0.0197(17) -0.0131(16)
H2z1 -0.007(3) -0.033(3)
H2x2 -0.0055(9) 0.0068(9)
H2y2 -0.0086(18) 0.0144(18)
H2z2 0.0151(19) -0.002(2)
H3x1 -0.0017(7) 0.0049(8)
H3y1 0.0243(17) -0.0129(16)
H3z1 -0.0087(19) 0.0348(19)
H3x2 0.0033(8) 0.0041(9)
H3y2 0.0041(19) 0.000(2)
H3z2 0.0100(17) -0.0036(17)
H4x1 -0.0053(9) 0.0060(9)
H4y1 0.0278(17) 0.0007(17)
H4z1 0.006(3) 0.014(3)
H4x2 0.0001(11) -0.0003(11)
H4y2 0.001(2) 0.006(2)
H4z2 -0.008(4) -0.007(4)
H5x1 0.0079(15) 0
H5y1 0 -0.001(4)
H5z1 -0.0047(11) 0
H5x2 -0.0010(18) 0
H5y2 0 0.008(5)
H5z2 -0.0011(12) 0
H6x1 -0.0134(15) 0
H6y1 0 0.001(4)
H6z1 -0.0069(13) 0
H6x2 0.0012(18) 0
H6y2 0 -0.001(5)
H6z2 0.0029(15) 0