The structures and phase transitions in 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2]
Authors:Bednarchuk, Tamara J.; Hornfeck, Wolfgang; Kinzhybalo, Vasyl; Zhou, Zhengyang; Dusek, Michal ; Pietraszko, Adam
Journal:Acta Crystallographica Section B 75 1144-1151 (2019)
DOI:https://doi.org/10.1107/S2052520619013155
B-IncStrDB ID: 15592EoXXcr Entry date: 2021-12-11 Last revision: 2021-12-12
PhaseII
Chemical data
Structural Formula Sum: Fe S2 O12 N2 C5 H15 [ Help ]
Formula weight: 415.1 Da [ Help ]
Crystallographic data and experimental details
Crystal system: monoclinic [ Help ]
Superspace group name: X2/c(α0γ)0s [ Help ]
Symmetry operations of the superspace group: (Show/hide table) [ Help ]
| Operation code | Operation in algebraic form |
|---|---|
| 1 | x1,x2,x3,x4 |
| 2 | -x1,x2,-x3+1/2,-x4+1/2 |
| 3 | -x1,-x2,-x3,-x4 |
| 4 | x1,-x2,x3+1/2,x4+1/2 |
| 5 | x1+1/2,x2+1/2,x3,x4+1/2 |
| 6 | -x1+1/2,x2+1/2,-x3+1/2,-x4 |
| 7 | -x1+1/2,-x2+1/2,-x3,-x4+1/2 |
| 8 | x1+1/2,-x2+1/2,x3+1/2,x4 |
a: 12.1601(3) Å [ Help ]
b: 17.2511(3) Å [ Help ]
c: 6.7758(2) Å [ Help ]
α: 90 ° [ Help ]
β: 100.715(2) ° [ Help ]
γ: 90 ° [ Help ]
Volume: 1396.61(6) Å3 [ Help ]
Modulation dimension: 1 [ Help ]
Measured independent wave vectors: (Show/hide table) [ Help ]
| Wave vector id | q_x | q_y | q_z |
|---|---|---|---|
| 1 | 0.294300 | 0.000000 | 0.564000 |
Z: 4 [ Help ]
Cell determination reflection Nb.: 6734 [ Help ]
θ(min) for cell determination: 3.4 ° [ Help ]
θ(max) for cell determination: 29.33 ° [ Help ]
Cell measurement temperature: 244.9(2) K [ Help ]
μ: 1.45 mm-1 [ Help ]
Absorption correction type: analytical [ Help ]
Absorption correction remarks: CrysAlisPro 1.171.39.12b (Rigaku Oxford Diffraction, 2015) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. [ Help ]
Minimum transmission factor: 0.586 [ Help ]
Maximum transmission factor: 0.751 [ Help ]
Refinement details
Total nb. of reflections: 5303 [ Help ]
Nb. of observed reflections: 2856 [ Help ]
Intense reflections threshold: I>3σ(I) [ Help ]
Refinement based on: Fsqd [ Help ]
R(obs): 0.0328 [ Help ]
wR(obs): 0.0790 [ Help ]
R(all): 0.0604 [ Help ]
wR(all): 0.0887 [ Help ]
S(all): 1.34 [ Help ]
S(obs): 1.68 [ Help ]
Nb. of reflections: 5303 [ Help ]
Nb. of parameters: 384 [ Help ]
Number of constraints: 41 [ Help ]
Weighting scheme: sigma [ Help ]
Weighting scheme remarks: w=1/(σ2(I)+0.0004I2) [ Help ]
Refinement of hydrogen atoms: mixed [ Help ]
Δ/σ(max): 3.8037 [ Help ]
Δ/σ(mean): 0.1426 [ Help ]
Δρ(max): 1.24 e_Å-3 [ Help ]
Δρ(min): -0.61 e_Å-3 [ Help ]
Extinction method: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) [ Help ]
Extinction coefficient: 5408.21 [ Help ]
Refinement remarks: WARNING: Unrealiable negative Uiso for atoms H1o5w1, H2o5w1, H1o5w2 and H2o5w2. [ Help ]
Structural Information
Average Structure: (Show/hide table) [ 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 | 0.5 | 0.356897(15) | 0.25 | Uani | 0.01310(9) | 4 | 1 | d | ? | ? | ? |
| S1 | S | 0.33286(3) | 0.351013(19) | -0.19593(5) | Uani | 0.01402(11) | 8 | 1 | d | ? | ? | ? |
| O2s | O | 0.22908(8) | 0.34282(6) | -0.11998(17) | Uani | 0.0264(4) | 8 | 1 | d | ? | ? | ? |
| O4s | O | 0.33393(13) | 0.42245(6) | -0.3114(2) | Uani | 0.0277(4) | 8 | 1 | d | ? | ? | ? |
| O3s | O | 0.35027(13) | 0.28467(7) | -0.3189(2) | Uani | 0.0258(7) | 8 | 1 | d | ? | ? | ? |
| O6w | O | 0.6044(2) | 0.27668(14) | 0.1791(4) | Uani | 0.0317(9) | 8 | 1 | d | ? | ? | ? |
| O5w1 | O | 0.5921(7) | 0.4411(3) | 0.1541(10) | Uani | 0.0516(12) | 8 | 0.5 | d | ? | ? | ? |
| O5w2 | O | 0.6067(6) | 0.4360(3) | 0.1756(8) | Uani | 0.0213(10) | 8 | 0.5 | d | ? | ? | ? |
| N1 | N | 0.5 | 0.08806(12) | 0.25 | Uani | 0.0280(8) | 4 | 1 | d | ? | ? | ? |
| O1b1 | O | 0.4271(5) | 0.3484(4) | -0.0265(8) | Uani | 0.0204(8) | 8 | 0.5 | d | ? | ? | ? |
| O1b2 | O | 0.4281(5) | 0.3630(5) | -0.0241(8) | Uani | 0.045(2) | 8 | 0.5 | d | ? | ? | ? |
| N2 | N | 0.5 | -0.14851(10) | 0.25 | Uani | 0.0282(7) | 4 | 1 | d | ? | ? | ? |
| C1 | C | 0.5 | 0.01091(12) | 0.25 | Uani | 0.0200(6) | 4 | 1 | d | ? | ? | ? |
| C2 | C | 0.39963(12) | -0.03151(9) | 0.2237(2) | Uani | 0.0267(5) | 8 | 1 | d | ? | ? | ? |
| C3 | C | 0.40199(13) | -0.11030(9) | 0.2261(2) | Uani | 0.0294(5) | 8 | 1 | d | ? | ? | ? |
| H1c2 | H | 0.329214 | -0.00477 | 0.204043 | Uiso | 0.032 | 8 | 1 | d | ? | ? | ? |
| H1c3 | H | 0.333185 | -0.138886 | 0.21059 | Uiso | 0.0352 | 8 | 1 | d | ? | ? | ? |
| H1n1 | H | 0.544(5) | 0.108(3) | 0.293(7) | Uiso | 0.033620(2) | 8 | 0.5 | d | ? | ? | ? |
| H2n1 | H | 0.559(5) | 0.113(3) | 0.242(7) | Uiso | 0.033620(2) | 8 | 0.5 | d | ? | ? | ? |
| H1n2 | H | 0.5 | -0.198938 | 0.25 | Uiso | 0.0338 | 4 | 1 | d | ? | ? | ? |
| H1o6w | H | 0.6228(18) | 0.2806(12) | 0.069(4) | Uiso | 0.016(9) | 8 | 1 | d | ? | ? | ? |
| H2o6w | H | 0.642(3) | 0.2512(15) | 0.243(5) | Uiso | 0.000(8) | 8 | 1 | d | ? | ? | ? |
| H1o5w1 | H | 0.605(3) | 0.436(2) | 0.094(6) | Uiso | -0.030(6) | 8 | 0.5 | d | ? | ? | ? |
| H2o5w1 | H | 0.629(3) | 0.508(3) | 0.239(6) | Uiso | -0.010(8) | 8 | 0.5 | d | ? | ? | ? |
| H1o5w2 | H | 0.631(2) | 0.437(2) | 0.123(7) | Uiso | -0.012(7) | 8 | 0.5 | d | ? | ? | ? |
| H2o5w2 | H | 0.630(3) | 0.515(3) | 0.239(5) | Uiso | -0.001(8) | 8 | 0.5 | d | ? | ? | ? |
ADP components: (Show/hide table) [ Help ]
| Atom site label | Atom site symbol | U11 | U22 | U33 | U12 | U13 | U23 |
|---|---|---|---|---|---|---|---|
| Fe1 | Fe | 0.01362(15) | 0.01408(15) | 0.01110(16) | 0 | 0.00098(12) | 0 |
| S1 | S | 0.01275(17) | 0.01712(18) | 0.01179(19) | 0.00005(12) | 0.00129(14) | 0.00043(12) |
| O2s | O | 0.0172(5) | 0.0314(6) | 0.0327(7) | -0.0009(4) | 0.0106(5) | 0.0004(5) |
| O4s | O | 0.0431(7) | 0.0153(5) | 0.0270(7) | -0.0005(5) | 0.0128(6) | 0.0016(5) |
| O3s | O | 0.0422(12) | 0.0150(9) | 0.0232(15) | 0.0015(8) | 0.0137(10) | -0.0003(10) |
| O6w | O | 0.0359(15) | 0.0348(15) | 0.0279(15) | 0.0201(10) | 0.0147(12) | 0.0082(9) |
| O5w1 | O | 0.094(2) | 0.0295(19) | 0.0460(15) | -0.0328(19) | 0.0502(16) | -0.0181(14) |
| O5w2 | O | 0.0245(19) | 0.0222(14) | 0.0176(18) | -0.0090(12) | 0.0046(13) | -0.0011(11) |
| N1 | N | 0.0214(12) | 0.0180(10) | 0.0435(15) | 0 | 0.0032(11) | 0 |
| O1b1 | O | 0.0235(9) | 0.019(2) | 0.0152(9) | 0.0029(16) | -0.0046(7) | -0.0039(15) |
| O1b2 | O | 0.019(2) | 0.101(6) | 0.0140(15) | 0.001(3) | -0.0031(12) | 0.005(2) |
| N2 | N | 0.0348(11) | 0.0140(9) | 0.0336(12) | 0 | 0.0009(10) | 0 |
| C1 | C | 0.0206(10) | 0.0192(10) | 0.0204(11) | 0 | 0.0040(9) | 0 |
| C2 | C | 0.0171(7) | 0.0241(8) | 0.0379(10) | 0.0008(6) | 0.0026(7) | -0.0008(7) |
| C3 | C | 0.0232(8) | 0.0260(8) | 0.0378(10) | -0.0061(7) | 0.0027(7) | -0.0011(7) |
Fourier Wave Vectors (explicit: q_x,q_y,q_z or coefficients: q_1,q_2,...): (Show/hide table) [ Help ]
| Wave vector code | q_1 |
|---|---|
| 1 | 1 |
| 2 | 2 |
Occupation crenel coefficients: (Show/hide table) [ Help ]
| Atom site label | Center (x0) | Width |
|---|---|---|
| O3s | 0.2381 | 1 |
| O6w | 0.5946 | 1 |
| O5w1 | 0.3268 | 0.5 |
| O5w2 | 0.8439 | 0.5 |
| O1b1 | 0.1754(5) | 0.5 |
| O1b2 | 0.6771(8) | 0.5 |
| H1o6w | 0.5412 | 1 |
| H2o6w | 0.6447 | 1 |
| H1o5w1 | 0.2722 | 0.5 |
| H2o5w1 | 0.3709 | 0.5 |
| H1o5w2 | 0.7835 | 0.5 |
| H2o5w2 | 0.9003 | 0.5 |
Definition of the displacive (translational) Fourier series: (Show/hide table) [ Help ]
| Modulation code | Atom site label | Displacement axis | Wave vector code |
|---|---|---|---|
| Fe1x1 | Fe1 | x | 1 |
| Fe1y1 | Fe1 | y | 1 |
| Fe1z1 | Fe1 | z | 1 |
| S1x1 | S1 | x | 1 |
| S1y1 | S1 | y | 1 |
| S1z1 | S1 | z | 1 |
| O2sx1 | O2s | x | 1 |
| O2sy1 | O2s | y | 1 |
| O2sz1 | O2s | z | 1 |
| O4sx1 | O4s | x | 1 |
| O4sy1 | O4s | y | 1 |
| O4sz1 | O4s | z | 1 |
| N1x1 | N1 | x | 1 |
| N1y1 | N1 | y | 1 |
| N1z1 | N1 | z | 1 |
| N2x1 | N2 | x | 1 |
| N2y1 | N2 | y | 1 |
| N2z1 | N2 | z | 1 |
| C1x1 | C1 | x | 1 |
| C1y1 | C1 | y | 1 |
| C1z1 | C1 | z | 1 |
| C2x1 | C2 | x | 1 |
| C2y1 | C2 | y | 1 |
| C2z1 | C2 | z | 1 |
| C3x1 | C3 | x | 1 |
| C3y1 | C3 | y | 1 |
| C3z1 | C3 | z | 1 |
| H1c2x1 | H1c2 | x | 1 |
| H1c2y1 | H1c2 | y | 1 |
| H1c2z1 | H1c2 | z | 1 |
| H1c3x1 | H1c3 | x | 1 |
| H1c3y1 | H1c3 | y | 1 |
| H1c3z1 | H1c3 | z | 1 |
| H1n1x1 | H1n1 | x | 1 |
| H1n1y1 | H1n1 | y | 1 |
| H1n1z1 | H1n1 | z | 1 |
| H2n1x1 | H2n1 | x | 1 |
| H2n1y1 | H2n1 | y | 1 |
| H2n1z1 | H2n1 | z | 1 |
| H1n2x1 | H1n2 | x | 1 |
| H1n2y1 | H1n2 | y | 1 |
| H1n2z1 | H1n2 | z | 1 |
Displacive (translational) Fourier coefficients: (Show/hide table) [ Help ]
| Modulation code | Cosine coefficient | Sine coefficient |
|---|---|---|
| Fe1x1 | 0.00246(3) | 0 |
| Fe1y1 | 0 | 0.001805(19) |
| Fe1z1 | 0.00233(5) | 0 |
| S1x1 | -0.00085(3) | -0.00136(3) |
| S1y1 | -0.00173(3) | -0.00459(3) |
| S1z1 | -0.00082(7) | -0.00365(7) |
| O2sx1 | -0.00140(9) | -0.00303(9) |
| O2sy1 | -0.00020(7) | -0.00069(7) |
| O2sz1 | -0.00237(19) | -0.00742(20) |
| O4sx1 | 0.00566(16) | 0.00926(16) |
| O4sy1 | -0.00216(8) | -0.00013(9) |
| O4sz1 | 0.0066(3) | 0.0159(3) |
| N1x1 | -0.00344(17) | 0 |
| N1y1 | 0 | 0.00094(12) |
| N1z1 | -0.0011(3) | 0 |
| N2x1 | -0.00002(18) | 0 |
| N2y1 | 0 | 0.00101(12) |
| N2z1 | -0.0042(3) | 0 |
| C1x1 | -0.0023(2) | 0 |
| C1y1 | 0 | 0.00088(15) |
| C1z1 | -0.0022(4) | 0 |
| C2x1 | -0.00180(15) | 0.00037(15) |
| C2y1 | -0.00050(11) | 0.00109(11) |
| C2z1 | -0.0030(3) | -0.0010(3) |
| C3x1 | -0.00056(16) | 0.00006(16) |
| C3y1 | -0.00046(11) | 0.00117(11) |
| C3z1 | -0.0039(3) | -0.0003(3) |
| H1c2x1 | -0.0021 | 0.0009 |
| H1c2y1 | -0.0007 | 0.0014 |
| H1c2z1 | -0.0034 | -0.0018 |
| H1c3x1 | -0.0001 | 0 |
| H1c3y1 | -0.0007 | 0.0015 |
| H1c3z1 | -0.0045 | -0.0001 |
| H1n1x1 | -0.00344(17) | 0 |
| H1n1y1 | 0 | 0.00094(12) |
| H1n1z1 | -0.0011(3) | 0 |
| H2n1x1 | -0.00344(17) | 0 |
| H2n1y1 | 0 | 0.00094(12) |
| H2n1z1 | -0.0011(3) | 0 |
| H1n2x1 | 0.0007 | 0 |
| H1n2y1 | 0 | 0.001 |
| H1n2z1 | -0.005 | 0 |
Displacive (translational) Legendre coefficients: (Show/hide table) [ Help ]
| Atom site label | Displacement axis | Polynomial order | Polynomial coeff. |
|---|---|---|---|
| O5w1 | x | 1 | -0.0078(16) |
| O5w1 | y | 1 | -0.0014(9) |
| O5w1 | z | 1 | -0.013(2) |
| O5w1 | x | 2 | 0.001(6) |
| O5w1 | y | 2 | -0.004(2) |
| O5w1 | z | 2 | -0.006(8) |
| O5w2 | x | 1 | 0.0278(14) |
| O5w2 | y | 1 | -0.0081(9) |
| O5w2 | z | 1 | 0.039(2) |
| O5w2 | x | 2 | -0.0211(12) |
| O5w2 | y | 2 | 0.0066(10) |
| O5w2 | z | 2 | -0.0257(19) |
| H1o5w1 | x | 1 | -0.041(6) |
| H1o5w1 | y | 1 | 0.009(4) |
| H1o5w1 | z | 1 | -0.063(15) |
| H1o5w1 | x | 2 | -0.030(7) |
| H1o5w1 | y | 2 | 0.002(6) |
| H1o5w1 | z | 2 | 0.149(13) |
| H2o5w1 | x | 1 | 0.029(7) |
| H2o5w1 | y | 1 | 0.060(6) |
| H2o5w1 | z | 1 | 0.050(12) |
| H2o5w1 | x | 2 | 0.047(10) |
| H2o5w1 | y | 2 | 0.043(7) |
| H2o5w1 | z | 2 | 0.081(17) |
| H1o5w2 | x | 1 | 0.011(5) |
| H1o5w2 | y | 1 | 0.006(4) |
| H1o5w2 | z | 1 | -0.022(16) |
| H1o5w2 | x | 2 | 0.024(7) |
| H1o5w2 | y | 2 | 0.018(6) |
| H1o5w2 | z | 2 | 0.202(15) |
| H2o5w2 | x | 1 | 0.036(7) |
| H2o5w2 | y | 1 | 0.068(6) |
| H2o5w2 | z | 1 | 0.080(12) |
| H2o5w2 | x | 2 | 0.023(10) |
| H2o5w2 | y | 2 | 0.051(8) |
| H2o5w2 | z | 2 | 0.033(18) |
Displacive (translational) XHarm coefficients: (Show/hide table) [ Help ]
| Atom site label | Displacement axis | XHarm order | XHarm coefficient |
|---|---|---|---|
| O3s | x | 1 | 0.0067(8) |
| O3s | y | 1 | 0.0003(6) |
| O3s | z | 1 | 0.0159(12) |
| O3s | x | 2 | -0.01056(14) |
| O3s | y | 2 | -0.00082(7) |
| O3s | z | 2 | -0.0215(3) |
| O3s | x | 3 | 0.0011(11) |
| O3s | y | 3 | 0.0035(8) |
| O3s | z | 3 | -0.0059(16) |
| O3s | x | 4 | -0.0047(15) |
| O3s | y | 4 | -0.0001(12) |
| O3s | z | 4 | -0.003(3) |
| O6w | x | 1 | -0.0090(7) |
| O6w | y | 1 | -0.0037(6) |
| O6w | z | 1 | -0.0145(15) |
| O6w | x | 2 | 0.0086(2) |
| O6w | y | 2 | 0.00234(13) |
| O6w | z | 2 | 0.0173(3) |
| O6w | x | 3 | 0.0021(10) |
| O6w | y | 3 | -0.0016(7) |
| O6w | z | 3 | 0.000(2) |
| O6w | x | 4 | 0.0038(18) |
| O6w | y | 4 | 0.0036(13) |
| O6w | z | 4 | 0.008(3) |
| O1b1 | x | 1 | -0.0017(5) |
| O1b1 | y | 1 | -0.0282(5) |
| O1b1 | z | 1 | -0.0002(10) |
| O1b1 | x | 2 | 0.0001(5) |
| O1b1 | y | 2 | -0.0077(4) |
| O1b1 | z | 2 | -0.0006(9) |
| O1b2 | x | 1 | -0.0005(6) |
| O1b2 | y | 1 | 0.0075(6) |
| O1b2 | z | 1 | 0.0039(11) |
| O1b2 | x | 2 | 0.006(2) |
| O1b2 | y | 2 | -0.007(2) |
| O1b2 | z | 2 | -0.006(4) |
| H1o6w | x | 1 | 0.000(6) |
| H1o6w | y | 1 | 0.001(5) |
| H1o6w | z | 1 | -0.004(13) |
| H1o6w | x | 2 | 0.011(2) |
| H1o6w | y | 2 | 0.0013(15) |
| H1o6w | z | 2 | 0.015(4) |
| H1o6w | x | 3 | -0.006(7) |
| H1o6w | y | 3 | -0.003(5) |
| H1o6w | z | 3 | -0.010(13) |
| H1o6w | x | 4 | -0.002(4) |
| H1o6w | y | 4 | -0.002(3) |
| H1o6w | z | 4 | 0.067(6) |
| H2o6w | x | 1 | -0.008(3) |
| H2o6w | y | 1 | -0.003(2) |
| H2o6w | z | 1 | -0.019(5) |
| H2o6w | x | 2 | 0.0045(16) |
| H2o6w | y | 2 | 0.0018(11) |
| H2o6w | z | 2 | 0.013(3) |
| H2o6w | x | 3 | 0.004(4) |
| H2o6w | y | 3 | -0.004(3) |
| H2o6w | z | 3 | 0.008(7) |
| H2o6w | x | 4 | 0.030(5) |
| H2o6w | y | 4 | -0.016(3) |
| H2o6w | z | 4 | 0.058(9) |
Definition of the ADP Fourier series: (Show/hide table) [ Help ]
| Modulation code | Atom site label | Tensor element | Wave vector code |
|---|---|---|---|
| Fe1U111 | Fe1 | U11 | 1 |
| Fe1U221 | Fe1 | U22 | 1 |
| Fe1U331 | Fe1 | U33 | 1 |
| Fe1U121 | Fe1 | U12 | 1 |
| Fe1U131 | Fe1 | U13 | 1 |
| Fe1U231 | Fe1 | U23 | 1 |
| S1U111 | S1 | U11 | 1 |
| S1U221 | S1 | U22 | 1 |
| S1U331 | S1 | U33 | 1 |
| S1U121 | S1 | U12 | 1 |
| S1U131 | S1 | U13 | 1 |
| S1U231 | S1 | U23 | 1 |
| O4sU111 | O4s | U11 | 1 |
| O4sU221 | O4s | U22 | 1 |
| O4sU331 | O4s | U33 | 1 |
| O4sU121 | O4s | U12 | 1 |
| O4sU131 | O4s | U13 | 1 |
| O4sU231 | O4s | U23 | 1 |
| N1U111 | N1 | U11 | 1 |
| N1U221 | N1 | U22 | 1 |
| N1U331 | N1 | U33 | 1 |
| N1U121 | N1 | U12 | 1 |
| N1U131 | N1 | U13 | 1 |
| N1U231 | N1 | U23 | 1 |
| N2U111 | N2 | U11 | 1 |
| N2U221 | N2 | U22 | 1 |
| N2U331 | N2 | U33 | 1 |
| N2U121 | N2 | U12 | 1 |
| N2U131 | N2 | U13 | 1 |
| N2U231 | N2 | U23 | 1 |
| C1U111 | C1 | U11 | 1 |
| C1U221 | C1 | U22 | 1 |
| C1U331 | C1 | U33 | 1 |
| C1U121 | C1 | U12 | 1 |
| C1U131 | C1 | U13 | 1 |
| C1U231 | C1 | U23 | 1 |
| C2U111 | C2 | U11 | 1 |
| C2U221 | C2 | U22 | 1 |
| C2U331 | C2 | U33 | 1 |
| C2U121 | C2 | U12 | 1 |
| C2U131 | C2 | U13 | 1 |
| C2U231 | C2 | U23 | 1 |
| C3U111 | C3 | U11 | 1 |
| C3U221 | C3 | U22 | 1 |
| C3U331 | C3 | U33 | 1 |
| C3U121 | C3 | U12 | 1 |
| C3U131 | C3 | U13 | 1 |
| C3U231 | C3 | U23 | 1 |
ADP Fourier coefficients: (Show/hide table) [ Help ]
| Modulation code | Cosine coefficient | Sine coefficient |
|---|---|---|
| Fe1U111 | 0 | -0.00016(17) |
| Fe1U221 | 0 | -0.00027(19) |
| Fe1U331 | 0 | -0.00015(20) |
| Fe1U121 | -0.00025(15) | 0 |
| Fe1U131 | 0 | 0.00014(16) |
| Fe1U231 | -0.00047(15) | 0 |
| S1U111 | 0.0005(2) | 0.0006(2) |
| S1U221 | 0.0002(2) | 0.0009(2) |
| S1U331 | 0.0002(2) | -0.0005(2) |
| S1U121 | 0.00023(18) | 0.00010(19) |
| S1U131 | 0.00006(19) | -0.00021(20) |
| S1U231 | 0.00002(18) | -0.00051(18) |
| O4sU111 | 0.0141(9) | 0.0063(10) |
| O4sU221 | -0.0027(7) | 0.0002(7) |
| O4sU331 | 0.0061(9) | 0.0045(9) |
| O4sU121 | -0.0018(7) | -0.0038(7) |
| O4sU131 | 0.0088(7) | 0.0047(8) |
| O4sU231 | -0.0005(6) | -0.0020(7) |
| N1U111 | 0 | 0.0004(12) |
| N1U221 | 0 | -0.0003(12) |
| N1U331 | 0 | -0.0021(15) |
| N1U121 | 0.0008(11) | 0 |
| N1U131 | 0 | 0.0006(11) |
| N1U231 | -0.0011(11) | 0 |
| N2U111 | 0 | 0.0002(14) |
| N2U221 | 0 | 0.0001(12) |
| N2U331 | 0 | -0.0014(15) |
| N2U121 | -0.0002(11) | 0 |
| N2U131 | 0 | -0.0011(12) |
| N2U231 | -0.0004(10) | 0 |
| C1U111 | 0 | 0.0007(14) |
| C1U221 | 0 | -0.0016(14) |
| C1U331 | 0 | 0.0015(15) |
| C1U121 | -0.0006(12) | 0 |
| C1U131 | 0 | 0.0011(12) |
| C1U231 | 0.0003(12) | 0 |
| C2U111 | 0.0008(10) | 0.0006(10) |
| C2U221 | 0.0003(11) | -0.0012(11) |
| C2U331 | 0.0000(13) | -0.0031(13) |
| C2U121 | -0.0003(9) | 0.0004(9) |
| C2U131 | 0.0013(9) | -0.0014(10) |
| C2U231 | 0.0003(10) | -0.0004(9) |
| C3U111 | 0.0009(11) | 0.0008(10) |
| C3U221 | -0.0005(12) | -0.0005(12) |
| C3U331 | -0.0002(13) | -0.0023(14) |
| C3U121 | 0.0000(9) | 0.0001(9) |
| C3U131 | 0.0008(10) | -0.0003(10) |
| C3U231 | 0.0006(10) | 0.0010(10) |
ADP XHarm coefficients: (Show/hide table) [ Help ]
| Atom site label | Tensor element | XHarm order | XHarm coefficient |
|---|---|---|---|
| O3s | U11 | 1 | -0.0106(17) |
| O3s | U22 | 1 | 0.0005(18) |
| O3s | U33 | 1 | -0.0068(15) |
| O3s | U12 | 1 | -0.0003(13) |
| O3s | U13 | 1 | -0.0070(12) |
| O3s | U23 | 1 | 0.0002(12) |
| O3s | U11 | 2 | -0.007(3) |
| O3s | U22 | 2 | 0.0020(11) |
| O3s | U33 | 2 | -0.001(4) |
| O3s | U12 | 2 | -0.0058(18) |
| O3s | U13 | 2 | -0.006(2) |
| O3s | U23 | 2 | -0.004(2) |
| O6w | U11 | 1 | -0.0099(14) |
| O6w | U22 | 1 | -0.013(2) |
| O6w | U33 | 1 | -0.0069(16) |
| O6w | U12 | 1 | -0.0091(12) |
| O6w | U13 | 1 | -0.0085(12) |
| O6w | U23 | 1 | -0.0068(13) |
| O6w | U11 | 2 | 0.002(4) |
| O6w | U22 | 2 | 0.001(2) |
| O6w | U33 | 2 | -0.005(4) |
| O6w | U12 | 2 | 0.001(3) |
| O6w | U13 | 2 | -0.003(3) |
| O6w | U23 | 2 | -0.003(2) |
PhaseIII
Chemical data
Structural Formula Sum: C5 N2 O12 S2 Fe H15 [ Help ]
Formula weight: 415.1 Da [ Help ]
Crystallographic data and experimental details
Crystal system: monoclinic [ Help ]
Superspace group name: X2/c(α0γ)0s [ Help ]
Symmetry operations of the superspace group: (Show/hide table) [ Help ]
| Operation code | Operation in algebraic form |
|---|---|
| 1 | x1,x2,x3,x4 |
| 2 | -x1,x2,-x3+1/2,-x4+1/2 |
| 3 | -x1,-x2,-x3,-x4 |
| 4 | x1,-x2,x3+1/2,x4+1/2 |
| 5 | x1+1/2,x2+1/2,x3,x4+1/2 |
| 6 | -x1+1/2,x2+1/2,-x3+1/2,-x4 |
| 7 | -x1+1/2,-x2+1/2,-x3,-x4+1/2 |
| 8 | x1+1/2,-x2+1/2,x3+1/2,x4 |
a: 12.175(11) Å [ Help ]
b: 17.217(5) Å [ Help ]
c: 6.769(2) Å [ Help ]
α: 90 ° [ Help ]
β: 100.87(4) ° [ Help ]
γ: 90 ° [ Help ]
Volume: 1393.4(14) Å3 [ Help ]
Modulation dimension: 1 [ Help ]
Measured independent wave vectors: (Show/hide table) [ Help ]
| Wave vector id | q_x | q_y | q_z |
|---|---|---|---|
| 1 | 0.336600 | 0.000000 | 0.554400 |
Z: 4 [ Help ]
Cell determination reflection Nb.: 7559 [ Help ]
θ(min) for cell determination: 3.41 ° [ Help ]
θ(max) for cell determination: 29.33 ° [ Help ]
Cell measurement temperature: 194.9(2) K [ Help ]
μ: 1.45 mm-1 [ Help ]
Absorption correction type: gaussian [ Help ]
Absorption correction remarks: Jana2006 [ Help ]
Minimum transmission factor: 0.5826 [ Help ]
Maximum transmission factor: 0.7523 [ Help ]
Refinement details
Total nb. of reflections: 5282 [ Help ]
Nb. of observed reflections: 3721 [ Help ]
Intense reflections threshold: I>3σ(I) [ Help ]
Refinement based on: Fsqd [ Help ]
R(obs): 0.0307 [ Help ]
wR(obs): 0.0700 [ Help ]
R(all): 0.0475 [ Help ]
wR(all): 0.0747 [ Help ]
S(all): 2.01 [ Help ]
S(obs): 2.28 [ Help ]
Nb. of reflections: 5282 [ Help ]
Nb. of parameters: 343 [ Help ]
Number of restraints: 7 [ Help ]
Number of constraints: 105 [ Help ]
Weighting scheme: sigma [ Help ]
Weighting scheme remarks: w=1/(σ2(I)+0.0004I2) [ Help ]
Refinement of hydrogen atoms: mixed [ Help ]
Δ/σ(max): 0.0471 [ Help ]
Δ/σ(mean): 0.0036 [ Help ]
Δρ(max): 0.76 e_Å-3 [ Help ]
Δρ(min): -0.45 e_Å-3 [ Help ]
Extinction method: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) [ Help ]
Extinction coefficient: 5320(160) [ Help ]
Structural Information
Average Structure: (Show/hide table) [ 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 | 1 | 0.643241(12) | 0.25 | Uani | 0.01092(8) | 4 | 1 | d | ? | ? | ? |
| S1 | S | 0.83288(2) | 0.649134(15) | -0.19644(4) | Uani | 0.01169(9) | 8 | 1 | d | ? | ? | ? |
| O1b1 | O | 0.92703(17) | 0.66428(13) | -0.0272(3) | Uani | 0.0292(5) | 8 | 0.5 | d | ? | ? | ? |
| O1b2 | O | 0.92889(17) | 0.62694(10) | -0.0238(3) | Uani | 0.0236(4) | 8 | 0.5 | d | ? | ? | ? |
| O2s | O | 0.72909(7) | 0.65734(5) | -0.11977(13) | Uani | 0.0213(3) | 8 | 1 | d | ? | ? | ? |
| O3s | O | 0.85049(7) | 0.71561(5) | -0.31897(12) | Uani | 0.0227(3) | 8 | 1 | d | ? | ? | ? |
| O5w1 | O | 1.08154(17) | 0.55665(9) | 0.1413(2) | Uani | 0.0317(5) | 8 | 0.5 | d | ? | ? | ? |
| O5w2 | O | 1.11916(17) | 0.56749(8) | 0.1928(2) | Uani | 0.0214(4) | 8 | 0.5 | d | ? | ? | ? |
| O6w | O | 1.10435(9) | 0.72361(6) | 0.17929(15) | Uani | 0.0239(3) | 8 | 1 | d | ? | ? | ? |
| O4s | O | 0.83380(9) | 0.57748(5) | -0.31196(16) | Uani | 0.0209(6) | 8 | 1 | d | ? | ? | ? |
| N1 | N | 0.5 | 0.41157(8) | 0.25 | Uani | 0.0222(5) | 4 | 1 | d | ? | ? | ? |
| N2 | N | 0.5 | 0.64870(8) | 0.25 | Uani | 0.0229(5) | 4 | 1 | d | ? | ? | ? |
| C1 | C | 0.5 | 0.48873(9) | 0.25 | Uani | 0.0170(5) | 4 | 1 | d | ? | ? | ? |
| C2 | C | 0.39927(10) | 0.53146(7) | 0.22442(19) | Uani | 0.0222(4) | 8 | 1 | d | ? | ? | ? |
| C3 | C | 0.40184(10) | 0.61031(7) | 0.22710(19) | Uani | 0.0245(4) | 8 | 1 | d | ? | ? | ? |
| H1c2 | H | 0.328874 | 0.504717 | 0.205097 | Uiso | 0.0266 | 8 | 1 | d | ? | ? | ? |
| H1c3 | H | 0.333164 | 0.638985 | 0.212572 | Uiso | 0.0294 | 8 | 1 | d | ? | ? | ? |
| H1n1 | H | 0.5581(16) | 0.3871(16) | 0.224(4) | Uiso | 0.0267(4) | 8 | 0.5 | d | ? | ? | ? |
| H2n1 | H | 0.4409(15) | 0.3878(16) | 0.186(4) | Uiso | 0.0267(4) | 8 | 0.5 | d | ? | ? | ? |
| H1n2 | H | 0.5 | 0.699228 | 0.25 | Uiso | 0.0275 | 4 | 1 | d | ? | ? | ? |
| H1o6w | H | 1.1217(12) | 0.7187(8) | 0.0715(13) | Uiso | 0.0287(13) | 8 | 1 | d | ? | ? | ? |
| H1o5w1 | H | 1.1032(17) | 0.5621(11) | 0.0374(18) | Uiso | 0.038033(2) | 8 | 0.5 | d | ? | ? | ? |
| H2o5w1 | H | 1.1076(15) | 0.5181(7) | 0.198(3) | Uiso | 0.038033(2) | 8 | 0.5 | d | ? | ? | ? |
| H2o6w | H | 1.1446(10) | 0.7517(7) | 0.2552(16) | Uiso | 0.0287(16) | 8 | 1 | d | ? | ? | ? |
| H1o5w2 | H | 1.1302(16) | 0.5700(10) | 0.0799(14) | Uiso | 0.0256(14) | 8 | 0.5 | d | ? | ? | ? |
| H2o5w2 | H | 1.1252(15) | 0.5231(5) | 0.228(3) | Uiso | 0.0256(3) | 8 | 0.5 | d | ? | ? | ? |
ADP components: (Show/hide table) [ Help ]
| Atom site label | Atom site symbol | U11 | U22 | U33 | U12 | U13 | U23 |
|---|---|---|---|---|---|---|---|
| Fe1 | Fe | 0.01136(12) | 0.01141(13) | 0.00961(14) | 0 | 0.00097(9) | 0 |
| S1 | S | 0.01085(14) | 0.01380(15) | 0.01008(16) | -0.00005(10) | 0.00111(11) | -0.00030(10) |
| O1b1 | O | 0.0172(7) | 0.0541(9) | 0.0137(7) | -0.0033(8) | -0.0038(5) | 0.0035(8) |
| O1b2 | O | 0.0168(6) | 0.0384(8) | 0.0130(7) | 0.0050(7) | -0.0036(5) | -0.0052(7) |
| O2s | O | 0.0145(4) | 0.0261(5) | 0.0250(5) | 0.0003(3) | 0.0079(4) | -0.0006(4) |
| O3s | O | 0.0343(5) | 0.0140(4) | 0.0222(5) | -0.0001(4) | 0.0118(4) | 0.0018(3) |
| O5w1 | O | 0.0564(11) | 0.0190(7) | 0.0272(8) | 0.0183(7) | 0.0270(8) | 0.0088(6) |
| O5w2 | O | 0.0288(8) | 0.0179(7) | 0.0201(7) | 0.0101(6) | 0.0113(6) | 0.0058(5) |
| O6w | O | 0.0289(5) | 0.0275(5) | 0.0174(5) | -0.0162(4) | 0.0099(4) | -0.0063(4) |
| O4s | O | 0.0318(11) | 0.0132(7) | 0.0190(12) | 0.0003(7) | 0.0080(8) | -0.0010(7) |
| N1 | N | 0.0172(7) | 0.0149(7) | 0.0334(9) | 0 | 0.0018(7) | 0 |
| N2 | N | 0.0279(8) | 0.0120(7) | 0.0272(9) | 0 | 0.0009(7) | 0 |
| C1 | C | 0.0172(8) | 0.0168(8) | 0.0167(8) | 0 | 0.0028(7) | 0 |
| C2 | C | 0.0144(5) | 0.0201(6) | 0.0311(7) | -0.0006(5) | 0.0023(5) | -0.0001(5) |
| C3 | C | 0.0201(6) | 0.0218(6) | 0.0304(7) | 0.0049(5) | 0.0020(6) | 0.0007(5) |
Fourier Wave Vectors (explicit: q_x,q_y,q_z or coefficients: q_1,q_2,...): (Show/hide table) [ Help ]
| Wave vector code | q_1 |
|---|---|
| 1 | 1 |
| 2 | 2 |
Occupation crenel coefficients: (Show/hide table) [ Help ]
| Atom site label | Center (x0) | Width |
|---|---|---|
| O1b1 | 0.32177(18) | 0.5 |
| O1b2 | 0.8243(3) | 0.5 |
| O5w1 | 0.4672(3) | 0.5 |
| O5w2 | 1.0084(3) | 0.5 |
| O6w | 0.7459(3) | 1 |
| O4s | 0.3825(4) | 1 |
| H1o6w | 0.6920(9) | 1 |
| H1o5w1 | 0.4169(12) | 0.5 |
| H2o5w1 | 0.5074(16) | 0.5 |
| H2o6w | 0.8015(10) | 1 |
| H1o5w2 | 0.9495(10) | 0.5 |
| H2o5w2 | 1.0302(16) | 0.5 |
Definition of the displacive (translational) Fourier series: (Show/hide table) [ Help ]
| Modulation code | Atom site label | Displacement axis | Wave vector code |
|---|---|---|---|
| Fe1x1 | Fe1 | x | 1 |
| Fe1y1 | Fe1 | y | 1 |
| Fe1z1 | Fe1 | z | 1 |
| S1x1 | S1 | x | 1 |
| S1y1 | S1 | y | 1 |
| S1z1 | S1 | z | 1 |
| O2sx1 | O2s | x | 1 |
| O2sy1 | O2s | y | 1 |
| O2sz1 | O2s | z | 1 |
| O3sx1 | O3s | x | 1 |
| O3sy1 | O3s | y | 1 |
| O3sz1 | O3s | z | 1 |
| N1x1 | N1 | x | 1 |
| N1y1 | N1 | y | 1 |
| N1z1 | N1 | z | 1 |
| N2x1 | N2 | x | 1 |
| N2y1 | N2 | y | 1 |
| N2z1 | N2 | z | 1 |
| C1x1 | C1 | x | 1 |
| C1y1 | C1 | y | 1 |
| C1z1 | C1 | z | 1 |
| C2x1 | C2 | x | 1 |
| C2y1 | C2 | y | 1 |
| C2z1 | C2 | z | 1 |
| C3x1 | C3 | x | 1 |
| C3y1 | C3 | y | 1 |
| C3z1 | C3 | z | 1 |
| H1c2x1 | H1c2 | x | 1 |
| H1c2y1 | H1c2 | y | 1 |
| H1c2z1 | H1c2 | z | 1 |
| H1c3x1 | H1c3 | x | 1 |
| H1c3y1 | H1c3 | y | 1 |
| H1c3z1 | H1c3 | z | 1 |
| H1n1x1 | H1n1 | x | 1 |
| H1n1y1 | H1n1 | y | 1 |
| H1n1z1 | H1n1 | z | 1 |
| H2n1x1 | H2n1 | x | 1 |
| H2n1y1 | H2n1 | y | 1 |
| H2n1z1 | H2n1 | z | 1 |
| H1n2x1 | H1n2 | x | 1 |
| H1n2y1 | H1n2 | y | 1 |
| H1n2z1 | H1n2 | z | 1 |
Displacive (translational) Fourier coefficients: (Show/hide table) [ Help ]
| Modulation code | Cosine coefficient | Sine coefficient |
|---|---|---|
| Fe1x1 | 0.00248(2) | 0 |
| Fe1y1 | 0 | -0.002004(15) |
| Fe1z1 | 0.00281(4) | 0 |
| S1x1 | -0.00076(3) | -0.00172(3) |
| S1y1 | 0.00225(2) | 0.00586(2) |
| S1z1 | -0.00096(5) | -0.00406(5) |
| O2sx1 | -0.00146(7) | -0.00343(7) |
| O2sy1 | 0.00023(6) | 0.00114(6) |
| O2sz1 | -0.00256(15) | -0.00777(15) |
| O3sx1 | -0.00867(9) | -0.01257(9) |
| O3sy1 | 0.00285(6) | 0.00110(6) |
| O3sz1 | -0.01343(16) | -0.02490(16) |
| N1x1 | 0.00255(6) | 0 |
| N1y1 | 0 | 0.00147(6) |
| N1z1 | -0.00058(19) | 0 |
| N2x1 | -0.00045(14) | 0 |
| N2y1 | 0 | 0.00098(10) |
| N2z1 | 0.0050(3) | 0 |
| C1x1 | 0.00245(16) | 0 |
| C1y1 | 0 | 0.00110(11) |
| C1z1 | 0.0021(3) | 0 |
| C2x1 | 0.00154(12) | -0.00026(12) |
| C2y1 | -0.00066(9) | 0.00119(8) |
| C2z1 | 0.0034(2) | 0.0013(2) |
| C3x1 | 0.00017(13) | 0.00005(12) |
| C3y1 | -0.00065(9) | 0.00117(9) |
| C3z1 | 0.0044(2) | 0.0005(2) |
| H1c2x1 | 0.0019 | -0.0008 |
| H1c2y1 | -0.001 | 0.0016 |
| H1c2z1 | 0.0042 | 0.0024 |
| H1c3x1 | -0.0003 | 0.0003 |
| H1c3y1 | -0.001 | 0.0015 |
| H1c3z1 | 0.005 | 0.0003 |
| H1n1x1 | 0.00255(6) | 0 |
| H1n1y1 | 0 | 0.00147(6) |
| H1n1z1 | -0.00058(19) | 0 |
| H2n1x1 | 0.00255(6) | 0 |
| H2n1y1 | 0 | 0.00147(6) |
| H2n1z1 | -0.00058(19) | 0 |
| H1n2x1 | -0.0014 | 0 |
| H1n2y1 | 0 | 0.001 |
| H1n2z1 | 0.0063 | 0 |
Displacive (translational) Legendre coefficients: (Show/hide table) [ Help ]
| Atom site label | Displacement axis | Polynomial order | Polynomial coeff. |
|---|---|---|---|
| O5w1 | x | 1 | 0.0040(2) |
| O5w1 | y | 1 | 0.00354(13) |
| O5w1 | z | 1 | 0.0018(3) |
| O5w1 | x | 2 | 0.0008(10) |
| O5w1 | y | 2 | -0.0029(5) |
| O5w1 | z | 2 | 0.0077(11) |
| O5w2 | x | 1 | 0.00108(19) |
| O5w2 | y | 1 | -0.00224(11) |
| O5w2 | z | 1 | 0.0009(3) |
| O5w2 | x | 2 | 0.0054(12) |
| O5w2 | y | 2 | 0.0028(3) |
| O5w2 | z | 2 | 0.0056(10) |
| H1o5w1 | x | 1 | 0.0040(2) |
| H1o5w1 | y | 1 | 0.00354(13) |
| H1o5w1 | z | 1 | 0.0018(3) |
| H1o5w1 | x | 2 | 0.0008(10) |
| H1o5w1 | y | 2 | -0.0029(5) |
| H1o5w1 | z | 2 | 0.0077(11) |
| H2o5w1 | x | 1 | 0.0040(2) |
| H2o5w1 | y | 1 | 0.00354(13) |
| H2o5w1 | z | 1 | 0.0018(3) |
| H2o5w1 | x | 2 | 0.0008(10) |
| H2o5w1 | y | 2 | -0.0029(5) |
| H2o5w1 | z | 2 | 0.0077(11) |
| H1o5w2 | x | 1 | 0.00108(19) |
| H1o5w2 | y | 1 | -0.00224(11) |
| H1o5w2 | z | 1 | 0.0009(3) |
| H1o5w2 | x | 2 | 0.0054(12) |
| H1o5w2 | y | 2 | 0.0028(3) |
| H1o5w2 | z | 2 | 0.0056(10) |
| H2o5w2 | x | 1 | 0.00108(19) |
| H2o5w2 | y | 1 | -0.00224(11) |
| H2o5w2 | z | 1 | 0.0009(3) |
| H2o5w2 | x | 2 | 0.0054(12) |
| H2o5w2 | y | 2 | 0.0028(3) |
| H2o5w2 | z | 2 | 0.0056(10) |
Displacive (translational) XHarm coefficients: (Show/hide table) [ Help ]
| Atom site label | Displacement axis | XHarm order | XHarm coefficient |
|---|---|---|---|
| O1b1 | x | 1 | 0.00097(19) |
| O1b1 | y | 1 | 0.00152(14) |
| O1b1 | z | 1 | -0.0022(4) |
| O1b1 | x | 2 | -0.0024(8) |
| O1b1 | y | 2 | -0.0005(5) |
| O1b1 | z | 2 | -0.0011(14) |
| O1b2 | x | 1 | -0.00114(18) |
| O1b2 | y | 1 | -0.00498(12) |
| O1b2 | z | 1 | 0.0001(3) |
| O1b2 | x | 2 | -0.0013(7) |
| O1b2 | y | 2 | -0.0012(4) |
| O1b2 | z | 2 | 0.0016(13) |
| O6w | x | 1 | -0.01402(16) |
| O6w | y | 1 | 0.00602(12) |
| O6w | z | 1 | -0.02735(14) |
| O6w | x | 2 | 0.00064(8) |
| O6w | y | 2 | 0.00204(6) |
| O6w | z | 2 | 0.00154(8) |
| O6w | x | 3 | -0.0041(2) |
| O6w | y | 3 | 0.0015(2) |
| O6w | z | 3 | -0.0060(2) |
| O6w | x | 4 | 0.0005(4) |
| O6w | y | 4 | 0.0000(3) |
| O6w | z | 4 | 0.0014(4) |
| O4s | x | 1 | -0.0115(8) |
| O4s | y | 1 | -0.0005(7) |
| O4s | z | 1 | -0.0191(15) |
| O4s | x | 2 | 0.00143(11) |
| O4s | y | 2 | -0.00195(6) |
| O4s | z | 2 | 0.00569(18) |
| O4s | x | 3 | -0.0058(11) |
| O4s | y | 3 | -0.0025(9) |
| O4s | z | 3 | -0.008(2) |
| O4s | x | 4 | -0.0028(13) |
| O4s | y | 4 | 0.0003(11) |
| O4s | z | 4 | -0.005(2) |
| H1o6w | x | 1 | -0.01402(16) |
| H1o6w | y | 1 | 0.00602(12) |
| H1o6w | z | 1 | -0.02735(14) |
| H1o6w | x | 2 | 0.00064(8) |
| H1o6w | y | 2 | 0.00204(6) |
| H1o6w | z | 2 | 0.00154(8) |
| H1o6w | x | 3 | -0.0041(2) |
| H1o6w | y | 3 | 0.0015(2) |
| H1o6w | z | 3 | -0.0060(2) |
| H1o6w | x | 4 | 0.0005(4) |
| H1o6w | y | 4 | 0.0000(3) |
| H1o6w | z | 4 | 0.0014(4) |
| H2o6w | x | 1 | -0.01402(16) |
| H2o6w | y | 1 | 0.00602(12) |
| H2o6w | z | 1 | -0.02735(14) |
| H2o6w | x | 2 | 0.00064(8) |
| H2o6w | y | 2 | 0.00204(6) |
| H2o6w | z | 2 | 0.00154(8) |
| H2o6w | x | 3 | -0.0041(2) |
| H2o6w | y | 3 | 0.0015(2) |
| H2o6w | z | 3 | -0.0060(2) |
| H2o6w | x | 4 | 0.0005(4) |
| H2o6w | y | 4 | 0.0000(3) |
| H2o6w | z | 4 | 0.0014(4) |
Definition of the ADP Fourier series: (Show/hide table) [ Help ]
| Modulation code | Atom site label | Tensor element | Wave vector code |
|---|---|---|---|
| Fe1U111 | Fe1 | U11 | 1 |
| Fe1U221 | Fe1 | U22 | 1 |
| Fe1U331 | Fe1 | U33 | 1 |
| Fe1U121 | Fe1 | U12 | 1 |
| Fe1U131 | Fe1 | U13 | 1 |
| Fe1U231 | Fe1 | U23 | 1 |
| S1U111 | S1 | U11 | 1 |
| S1U221 | S1 | U22 | 1 |
| S1U331 | S1 | U33 | 1 |
| S1U121 | S1 | U12 | 1 |
| S1U131 | S1 | U13 | 1 |
| S1U231 | S1 | U23 | 1 |
| O2sU111 | O2s | U11 | 1 |
| O2sU221 | O2s | U22 | 1 |
| O2sU331 | O2s | U33 | 1 |
| O2sU121 | O2s | U12 | 1 |
| O2sU131 | O2s | U13 | 1 |
| O2sU231 | O2s | U23 | 1 |
| O3sU111 | O3s | U11 | 1 |
| O3sU221 | O3s | U22 | 1 |
| O3sU331 | O3s | U33 | 1 |
| O3sU121 | O3s | U12 | 1 |
| O3sU131 | O3s | U13 | 1 |
| O3sU231 | O3s | U23 | 1 |
| N1U111 | N1 | U11 | 1 |
| N1U221 | N1 | U22 | 1 |
| N1U331 | N1 | U33 | 1 |
| N1U121 | N1 | U12 | 1 |
| N1U131 | N1 | U13 | 1 |
| N1U231 | N1 | U23 | 1 |
| N2U111 | N2 | U11 | 1 |
| N2U221 | N2 | U22 | 1 |
| N2U331 | N2 | U33 | 1 |
| N2U121 | N2 | U12 | 1 |
| N2U131 | N2 | U13 | 1 |
| N2U231 | N2 | U23 | 1 |
| C1U111 | C1 | U11 | 1 |
| C1U221 | C1 | U22 | 1 |
| C1U331 | C1 | U33 | 1 |
| C1U121 | C1 | U12 | 1 |
| C1U131 | C1 | U13 | 1 |
| C1U231 | C1 | U23 | 1 |
| C2U111 | C2 | U11 | 1 |
| C2U221 | C2 | U22 | 1 |
| C2U331 | C2 | U33 | 1 |
| C2U121 | C2 | U12 | 1 |
| C2U131 | C2 | U13 | 1 |
| C2U231 | C2 | U23 | 1 |
| C3U111 | C3 | U11 | 1 |
| C3U221 | C3 | U22 | 1 |
| C3U331 | C3 | U33 | 1 |
| C3U121 | C3 | U12 | 1 |
| C3U131 | C3 | U13 | 1 |
| C3U231 | C3 | U23 | 1 |
ADP Fourier coefficients: (Show/hide table) [ Help ]
| Modulation code | Cosine coefficient | Sine coefficient |
|---|---|---|
| Fe1U111 | 0 | -0.00005(14) |
| Fe1U221 | 0 | -0.00021(15) |
| Fe1U331 | 0 | -0.00007(16) |
| Fe1U121 | 0.00031(11) | 0 |
| Fe1U131 | 0 | 0.00027(13) |
| Fe1U231 | 0.00046(11) | 0 |
| S1U111 | 0.00044(17) | 0.00066(17) |
| S1U221 | 0.00072(19) | 0.00120(19) |
| S1U331 | 0.00018(19) | -0.0005(2) |
| S1U121 | -0.00052(14) | 0.00004(14) |
| S1U131 | 0.00050(16) | 0.00004(16) |
| S1U231 | -0.00005(14) | 0.00060(14) |
| O2sU111 | 0.0001(5) | 0.0005(5) |
| O2sU221 | 0.0009(6) | 0.0013(6) |
| O2sU331 | 0.0013(7) | 0.0014(7) |
| O2sU121 | 0.0000(5) | -0.0018(5) |
| O2sU131 | 0.0001(5) | 0.0001(5) |
| O2sU231 | 0.0008(5) | -0.0014(5) |
| O3sU111 | 0.0024(7) | -0.0036(7) |
| O3sU221 | 0.0009(6) | 0.0019(6) |
| O3sU331 | -0.0033(7) | -0.0088(7) |
| O3sU121 | 0.0002(5) | 0.0038(5) |
| O3sU131 | -0.0009(6) | -0.0066(6) |
| O3sU231 | -0.0005(5) | 0.0017(5) |
| N1U111 | 0 | -0.0012(9) |
| N1U221 | 0 | 0.0012(9) |
| N1U331 | 0 | 0.0020(11) |
| N1U121 | -0.0001(8) | 0 |
| N1U131 | 0 | 0.0006(8) |
| N1U231 | 0.0002(8) | 0 |
| N2U111 | 0 | -0.0006(10) |
| N2U221 | 0 | 0.0007(9) |
| N2U331 | 0 | 0.0028(12) |
| N2U121 | 0.0005(8) | 0 |
| N2U131 | 0 | 0.0020(10) |
| N2U231 | 0.0002(8) | 0 |
| C1U111 | 0 | -0.0001(10) |
| C1U221 | 0 | 0.0005(11) |
| C1U331 | 0 | 0.0003(12) |
| C1U121 | -0.0011(9) | 0 |
| C1U131 | 0 | -0.0013(9) |
| C1U231 | 0.0002(9) | 0 |
| C2U111 | 0.0003(7) | -0.0012(7) |
| C2U221 | 0.0002(8) | 0.0006(8) |
| C2U331 | -0.0009(10) | 0.0024(10) |
| C2U121 | 0.0002(7) | 0.0007(7) |
| C2U131 | -0.0009(7) | 0.0006(7) |
| C2U231 | 0.0008(7) | 0.0007(7) |
| C3U111 | -0.0001(8) | -0.0001(8) |
| C3U221 | 0.0002(9) | -0.0007(9) |
| C3U331 | -0.0003(10) | 0.0042(10) |
| C3U121 | 0.0003(7) | -0.0006(7) |
| C3U131 | 0.0002(7) | 0.0013(8) |
| C3U231 | 0.0007(7) | 0.0006(7) |
ADP XHarm coefficients: (Show/hide table) [ Help ]
| Atom site label | Tensor element | XHarm order | XHarm coefficient |
|---|---|---|---|
| O6w | U11 | 1 | 0.0007(8) |
| O6w | U22 | 1 | -0.0079(8) |
| O6w | U33 | 1 | 0.0027(6) |
| O6w | U12 | 1 | 0.0044(6) |
| O6w | U13 | 1 | 0.0014(5) |
| O6w | U23 | 1 | 0.0007(6) |
| O6w | U11 | 2 | 0.0090(11) |
| O6w | U22 | 2 | 0.0044(9) |
| O6w | U33 | 2 | 0.0120(9) |
| O6w | U12 | 2 | -0.0060(9) |
| O6w | U13 | 2 | 0.0102(9) |
| O6w | U23 | 2 | -0.0071(9) |
| O4s | U11 | 1 | -0.011(2) |
| O4s | U22 | 1 | -0.0004(17) |
| O4s | U33 | 1 | -0.0035(19) |
| O4s | U12 | 1 | -0.0045(16) |
| O4s | U13 | 1 | -0.0054(14) |
| O4s | U23 | 1 | -0.0020(14) |
| O4s | U11 | 2 | -0.001(3) |
| O4s | U22 | 2 | 0.0010(11) |
| O4s | U33 | 2 | 0.004(3) |
| O4s | U12 | 2 | -0.0013(17) |
| O4s | U13 | 2 | 0.002(2) |
| O4s | U23 | 2 | -0.0025(18) |
PhaseIV
Chemical data
Structural Formula Sum: C5 H15 Fe N2 O12 S2 [ Help ]
Formula weight: 415.16 Da [ Help ]
Crystallographic data and experimental details
Crystal system: triclinic [ Help ]
Space group nb.: 2 [ Help ]
Space group name (H-M): P -1 [ Help ]
Space group name (Hall): -P 1 [ Help ]
Symmetry operations of the space group: (Show/hide table) [ Help ]
| Operation code | Operation in algebraic form |
|---|---|
| 1 | x, y, z |
| 2 | -x, -y, -z |
a: 10.516(4) Å [ Help ]
b: 11.873(4) Å [ Help ]
c: 13.099(4) Å [ Help ]
α: 65.34(3) ° [ Help ]
β: 77.51(3) ° [ Help ]
γ: 68.73(3) ° [ Help ]
Volume: 1381.0(9) Å3 [ Help ]
Z: 4 [ Help ]
Cell measurement temperature: 80(2) K [ Help ]
Cell determination reflection Nb.: 2322 [ Help ]
θ(min) for cell determination: 2.4010 ° [ Help ]
θ(max) for cell determination: 29.2810 ° [ Help ]
μ: 1.463 mm-1 [ Help ]
Absorption correction type: analytical [ Help ]
Minimum transmission factor: 0.592 [ Help ]
Maximum transmission factor: 0.764 [ Help ]
Absorption correction remarks: CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. [ Help ]
Refinement details
Total nb. of reflections: 7895 [ Help ]
Nb. of observed reflections: 5963 [ Help ]
Intense reflections threshold: I > 2σ(I) [ Help ]
Proportion of Friedel related intensities: 0.000 [ Help ]
Reflection handling remarks: _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would bepossible theoretically, ignoring centric projections andsystematic absences. [ Help ]
Refinement remarks: Refined as a 2-component twin. [ Help ]
Refinement based on: Fsqd [ Help ]
Matrix type used for the least-squares: full [ Help ]
Weighting scheme: calc [ Help ]
Weighting scheme remarks: w=1/[σ2(Fo2)+(0.0453P)2] where P=(Fo2+2Fc2)/3 [ Help ]
Refinement of hydrogen atoms: mixed [ Help ]
Extinction method: none [ Help ]
Nb. of reflections: 7895 [ Help ]
Nb. of parameters: 446 [ Help ]
Number of restraints: 28 [ Help ]
R(all): 0.0371 [ Help ]
R(obs): 0.0268 [ Help ]
wR(all): 0.0772 [ Help ]
wR(obs): 0.0746 [ Help ]
S(all): 0.984 [ Help ]
Restrained S(all): 0.986 [ Help ]
Δ/σ(max): 0.000 [ Help ]
Δ/σ(mean): 0.000 [ Help ]
Δρ(max): 0.363 e_Å-3 [ Help ]
Δρ(min): -0.598 e_Å-3 [ Help ]
Δρ(rms): 0.088 e_Å-3 [ Help ]
Structural Information
Average Structure: (Show/hide table) [ Help ]
| Atom site label | Atom symbol | x | y | z | Uiso/equiv | ADP type | Occupancy | _atom_site_site_symmetry_order | Coords from (d)iffraction or (c)alculated | Coords restraints or constraints | ADPs constraints or restraints | Disordered cluster | Disordered group |
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | Fe | 0.85489(5) | 0.80465(5) | 0.05110(4) | 0.00606(9) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O11W | O | 0.8995(2) | 0.7303(2) | -0.06833(19) | 0.0149(5) | Uani | 1 | 1 | d | D | ? | ? | ? |
| H11A | H | 0.895(3) | 0.659(2) | -0.062(2) | 0.022 | Uiso | 1 | 1 | d | D | U | ? | ? |
| H11B | H | 0.917(3) | 0.785(2) | -0.1299(18) | 0.022 | Uiso | 1 | 1 | d | D | U | ? | ? |
| O12W | O | 1.0244(2) | 0.8607(2) | -0.00306(17) | 0.0180(5) | Uani | 1 | 1 | d | D | ? | ? | ? |
| H12A | H | 1.090(2) | 0.848(2) | 0.032(2) | 0.027 | Uiso | 1 | 1 | d | D | U | ? | ? |
| H12B | H | 1.035(3) | 0.899(2) | -0.0698(16) | 0.027 | Uiso | 1 | 1 | d | D | U | ? | ? |
| O13W | O | 0.81186(18) | 0.87453(18) | 0.17633(15) | 0.0121(4) | Uani | 1 | 1 | d | D | ? | ? | ? |
| H13A | H | 0.797(2) | 0.821(2) | 0.2440(16) | 0.018 | Uiso | 1 | 1 | d | D | U | ? | ? |
| H13B | H | 0.855(3) | 0.909(2) | 0.196(2) | 0.018 | Uiso | 1 | 1 | d | D | U | ? | ? |
| O14W | O | 0.6785(2) | 0.7595(2) | 0.10258(19) | 0.0129(5) | Uani | 1 | 1 | d | D | ? | ? | ? |
| H14A | H | 0.600(2) | 0.812(2) | 0.078(2) | 0.019 | Uiso | 1 | 1 | d | D | U | ? | ? |
| H14B | H | 0.659(3) | 0.716(2) | 0.1693(16) | 0.019 | Uiso | 1 | 1 | d | D | U | ? | ? |
| S11 | S | 1.02552(8) | 0.49807(7) | 0.19250(6) | 0.00594(17) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O11 | O | 0.94714(15) | 0.63949(14) | 0.16268(12) | 0.0119(3) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O12 | O | 1.1177(2) | 0.4786(2) | 0.09617(18) | 0.0117(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O13 | O | 1.1034(2) | 0.4622(2) | 0.28774(19) | 0.0105(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O14 | O | 0.9275(2) | 0.4234(2) | 0.2238(2) | 0.0120(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| S12 | S | 0.67609(8) | 1.10656(8) | -0.09414(6) | 0.00639(18) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O15 | O | 0.75980(15) | 0.96622(14) | -0.06330(12) | 0.0140(3) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O16 | O | 0.7677(2) | 1.1834(2) | -0.10813(19) | 0.0129(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O17 | O | 0.6192(2) | 1.14596(19) | -0.19994(18) | 0.0115(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O18 | O | 0.5663(2) | 1.1188(2) | -0.00516(19) | 0.0106(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| Fe2 | Fe | 0.14147(5) | 0.69703(5) | 0.44620(4) | 0.00613(9) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O21W | O | 0.12655(18) | 0.67397(18) | 0.30560(15) | 0.0138(4) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H21A | H | 0.160(2) | 0.717(2) | 0.2402(16) | 0.021 | Uiso | 1 | 1 | d | ? | U | ? | ? |
| H21B | H | 0.126(3) | 0.607(2) | 0.299(2) | 0.021 | Uiso | 1 | 1 | d | ? | U | ? | ? |
| O22W | O | 0.3376(2) | 0.69092(19) | 0.39982(19) | 0.0136(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H22A | H | 0.406(2) | 0.656(2) | 0.433(2) | 0.020 | Uiso | 1 | 1 | d | ? | U | ? | ? |
| H22B | H | 0.359(3) | 0.750(2) | 0.3361(18) | 0.020 | Uiso | 1 | 1 | d | ? | U | ? | ? |
| O23W | O | 0.1403(2) | 0.73612(19) | 0.58166(18) | 0.0106(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H23A | H | 0.129(3) | 0.8129(19) | 0.576(2) | 0.016 | Uiso | 1 | 1 | d | ? | U | ? | ? |
| H23B | H | 0.106(3) | 0.690(2) | 0.6342(18) | 0.016 | Uiso | 1 | 1 | d | ? | U | ? | ? |
| O24W | O | -0.05504(19) | 0.69447(17) | 0.49652(16) | 0.0105(4) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H24A | H | -0.062(3) | 0.645(2) | 0.5571(17) | 0.016 | Uiso | 1 | 1 | d | ? | U | ? | ? |
| H24B | H | -0.108(2) | 0.697(2) | 0.4532(19) | 0.016 | Uiso | 1 | 1 | d | ? | U | ? | ? |
| S21 | S | 0.30787(8) | 0.39157(8) | 0.58710(7) | 0.00705(17) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O21 | O | 0.19184(14) | 0.51098(14) | 0.53521(12) | 0.0121(3) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O22 | O | 0.4257(2) | 0.3861(2) | 0.50322(18) | 0.0105(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O23 | O | 0.34297(19) | 0.39600(19) | 0.68592(18) | 0.0114(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O24 | O | 0.2543(2) | 0.2805(2) | 0.61826(19) | 0.0101(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| S22 | S | -0.01189(8) | 1.01117(7) | 0.31362(6) | 0.00706(19) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O25 | O | 0.09707(15) | 0.88340(14) | 0.35703(13) | 0.0125(3) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O26 | O | 0.0580(2) | 1.11249(19) | 0.27131(19) | 0.0102(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O27 | O | -0.0733(2) | 1.0135(2) | 0.22243(18) | 0.0126(5) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| O28 | O | -0.1149(2) | 1.0298(2) | 0.40460(19) | 0.0125(6) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| N11 | N | 0.6558(3) | 0.4454(3) | 0.1977(3) | 0.0104(4) | Uani | 1 | 1 | d | ? | U | ? | ? |
| H11 | H | 0.7086 | 0.4706 | 0.2218 | 0.013 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| C12 | C | 0.7124(4) | 0.3670(4) | 0.1404(3) | 0.0134(9) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H12 | H | 0.8092 | 0.3391 | 0.1273 | 0.016 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| C13 | C | 0.6372(4) | 0.3262(4) | 0.1007(3) | 0.0114(8) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H13 | H | 0.6801 | 0.2693 | 0.0609 | 0.014 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| C14 | C | 0.4888(5) | 0.3704(5) | 0.1195(4) | 0.0103(4) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| N14 | N | 0.4103(3) | 0.3316(3) | 0.0820(3) | 0.0122(4) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H14C | H | 0.3208 | 0.3574 | 0.0954 | 0.015 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| H14D | H | 0.4480 | 0.2800 | 0.0439 | 0.015 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| C15 | C | 0.4343(4) | 0.4506(4) | 0.1793(3) | 0.0124(9) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H15 | H | 0.3378 | 0.4813 | 0.1930 | 0.015 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| C16 | C | 0.5167(4) | 0.4877(4) | 0.2198(3) | 0.0127(8) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H16 | H | 0.4778 | 0.5418 | 0.2624 | 0.015 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| N21 | N | 0.3527(3) | 0.0502(3) | 0.2988(3) | 0.0124(4) | Uani | 1 | 1 | d | ? | U | ? | ? |
| H21 | H | 0.3015 | 0.0243 | 0.2737 | 0.015 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| C22 | C | 0.4918(4) | 0.0105(4) | 0.2774(3) | 0.0126(9) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H22 | H | 0.5327 | -0.0428 | 0.2342 | 0.015 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| C23 | C | 0.5721(4) | 0.0488(4) | 0.3193(3) | 0.0119(9) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H23 | H | 0.6688 | 0.0197 | 0.3060 | 0.014 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| C24 | C | 0.5145(4) | 0.1282(5) | 0.3797(4) | 0.0097(4) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| N24 | N | 0.5907(3) | 0.1685(3) | 0.4186(3) | 0.0128(4) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H24C | H | 0.6803 | 0.1441 | 0.4055 | 0.015 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| H24D | H | 0.5513 | 0.2194 | 0.4571 | 0.015 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| C25 | C | 0.3660(4) | 0.1699(4) | 0.3980(3) | 0.0131(9) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H25 | H | 0.3211 | 0.2261 | 0.4382 | 0.016 | Uiso | 1 | 1 | calc | R | U | ? | ? |
| C26 | C | 0.2936(4) | 0.1276(4) | 0.3572(3) | 0.0142(9) | Uani | 1 | 1 | d | ? | ? | ? | ? |
| H26 | H | 0.1968 | 0.1536 | 0.3702 | 0.017 | Uiso | 1 | 1 | calc | R | U | ? | ? |
ADP components: (Show/hide table) [ Help ]
| Atom site label | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 0.0051(3) | 0.0058(2) | 0.0068(3) | -0.00176(16) | -0.00046(19) | -0.00186(18) |
| O11W | 0.0279(12) | 0.0102(11) | 0.0083(9) | -0.0045(8) | 0.0026(8) | -0.0088(9) |
| O12W | 0.0152(10) | 0.0302(13) | 0.0087(9) | 0.0016(9) | -0.0027(8) | -0.0165(9) |
| O13W | 0.0186(10) | 0.0124(10) | 0.0086(9) | -0.0046(8) | 0.0010(8) | -0.0088(8) |
| O14W | 0.0106(9) | 0.0195(12) | 0.0090(9) | -0.0025(9) | -0.0008(7) | -0.0082(9) |
| S11 | 0.0060(3) | 0.0058(4) | 0.0063(3) | -0.0021(3) | -0.0004(3) | -0.0023(3) |
| O11 | 0.0138(8) | 0.0065(8) | 0.0111(8) | -0.0022(6) | -0.0020(6) | 0.0009(7) |
| O12 | 0.0113(12) | 0.0139(13) | 0.0082(11) | -0.0051(9) | 0.0018(9) | -0.0022(10) |
| O13 | 0.0099(10) | 0.0111(10) | 0.0116(9) | -0.0050(7) | -0.0009(7) | -0.0034(8) |
| O14 | 0.0089(9) | 0.0158(11) | 0.0122(9) | -0.0034(8) | -0.0021(7) | -0.0061(8) |
| S12 | 0.0060(3) | 0.0064(4) | 0.0065(3) | -0.0024(3) | -0.0009(3) | -0.0013(3) |
| O15 | 0.0139(8) | 0.0106(9) | 0.0131(8) | -0.0035(7) | -0.0020(6) | 0.0007(7) |
| O16 | 0.0130(10) | 0.0173(12) | 0.0103(10) | -0.0033(9) | -0.0020(8) | -0.0083(9) |
| O17 | 0.0149(10) | 0.0099(11) | 0.0090(9) | -0.0011(8) | -0.0015(7) | -0.0055(8) |
| O18 | 0.0083(12) | 0.0158(13) | 0.0115(11) | -0.0093(10) | 0.0015(9) | -0.0041(10) |
| Fe2 | 0.0050(3) | 0.0061(2) | 0.0068(3) | -0.00165(16) | -0.00057(19) | -0.00194(18) |
| O21W | 0.0234(11) | 0.0149(11) | 0.0083(9) | -0.0043(8) | -0.0003(8) | -0.0122(9) |
| O22W | 0.0071(9) | 0.0140(12) | 0.0114(10) | 0.0024(9) | -0.0025(7) | -0.0015(9) |
| O23W | 0.0172(11) | 0.0073(11) | 0.0079(9) | -0.0026(8) | 0.0011(8) | -0.0056(8) |
| O24W | 0.0090(9) | 0.0132(10) | 0.0092(9) | -0.0018(8) | -0.0016(7) | -0.0056(8) |
| S21 | 0.0063(3) | 0.0061(4) | 0.0079(3) | -0.0027(3) | 0.0002(3) | -0.0013(3) |
| O21 | 0.0097(8) | 0.0109(8) | 0.0142(8) | -0.0029(6) | -0.0013(6) | -0.0036(7) |
| O22 | 0.0089(12) | 0.0144(13) | 0.0100(11) | -0.0069(9) | 0.0007(9) | -0.0035(10) |
| O23 | 0.0112(10) | 0.0145(12) | 0.0092(9) | -0.0031(8) | -0.0023(8) | -0.0054(8) |
| O24 | 0.0137(10) | 0.0080(11) | 0.0092(9) | -0.0016(8) | -0.0019(7) | -0.0054(8) |
| S22 | 0.0074(3) | 0.0061(4) | 0.0064(3) | -0.0013(3) | -0.0002(3) | -0.0019(3) |
| O25 | 0.0109(8) | 0.0082(8) | 0.0138(8) | -0.0021(7) | -0.0011(6) | 0.0000(7) |
| O26 | 0.0150(10) | 0.0089(11) | 0.0109(9) | -0.0041(8) | -0.0014(7) | -0.0077(8) |
| O27 | 0.0159(11) | 0.0164(11) | 0.0092(10) | -0.0034(8) | -0.0031(8) | -0.0093(9) |
| O28 | 0.0110(13) | 0.0125(12) | 0.0097(11) | -0.0036(9) | 0.0011(9) | -0.0006(10) |
| N11 | 0.0072(12) | 0.0110(11) | 0.0127(11) | -0.0020(8) | -0.0049(9) | -0.0029(9) |
| C12 | 0.0095(18) | 0.014(2) | 0.016(2) | -0.0040(16) | -0.0030(15) | -0.0037(15) |
| C13 | 0.0061(18) | 0.0085(19) | 0.0155(19) | -0.0043(16) | 0.0007(15) | 0.0012(15) |
| C14 | 0.007(2) | 0.0102(15) | 0.0089(16) | 0.0020(10) | -0.0019(12) | -0.0030(11) |
| N14 | 0.0075(17) | 0.0146(13) | 0.0202(15) | -0.0120(9) | 0.0026(11) | -0.0051(10) |
| C15 | 0.0080(18) | 0.016(2) | 0.0160(19) | -0.0067(17) | -0.0004(15) | -0.0055(16) |
| C16 | 0.0101(18) | 0.011(2) | 0.0132(19) | -0.0028(16) | -0.0009(14) | -0.0013(14) |
| N21 | 0.0093(13) | 0.0135(11) | 0.0148(11) | -0.0029(8) | -0.0046(9) | -0.0047(9) |
| C22 | 0.0099(18) | 0.013(2) | 0.0130(19) | -0.0053(16) | 0.0014(14) | -0.0015(15) |
| C23 | 0.0072(17) | 0.015(2) | 0.0160(19) | -0.0064(17) | 0.0009(15) | -0.0062(15) |
| C24 | 0.0048(19) | 0.0103(16) | 0.0084(16) | 0.0019(10) | -0.0017(11) | -0.0019(11) |
| N24 | 0.0084(17) | 0.0144(13) | 0.0210(15) | -0.0117(9) | 0.0022(11) | -0.0053(10) |
| C25 | 0.0065(18) | 0.013(2) | 0.018(2) | -0.0079(17) | 0.0014(16) | 0.0000(15) |
| C26 | 0.0088(18) | 0.019(2) | 0.016(2) | -0.0079(17) | -0.0002(15) | -0.0043(16) |