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The structure of cronstedtite-1M was refined using a crystal from Eisleben (Saxony-Anhalt, Germany). The space group is Cm, a = 5.5033 (3), b = 9.5289 (6), c = 7.3328 (5) Å, β = 104.493 (7)°, composition (Fe2+2.461Fe3+0.539)(Si1.461Fe3+0.539)O5(OH)4, Z = 2. Despite diffusely streaked characteristic polytype reflections, the refinement converged to Robs = 0.0242 for 1117 independent reflections. Separate Robs values of 0.0183 and 0.0553 were obtained for 415 subfamily and 702 characteristic reflections, respectively. The structure is built of one edge-sharing octahedral (Oc) and one corner-sharing tetrahedral (Tet) sheet forming the 1:1 layer by sharing apical corners of the Tet sheet. Consecutive layers are shifted by a/3 of the hexagonal cell, the polytype belongs to the subfamily (Bailey's group) A. There are two octahedral sites M1 (at m), M2 (in a general position) both fully occupied by Fe. Since the M2 octahedron is larger than M1, the Oc sheet is meso-octahedral. The Tet sheet contains one tetrahedral position, T1, occupied by Si and Fe in the ratio 0.731:0.269 (9). The ring of tetrahedra is strongly ditrigonalized, α = +12.7°; Franzini type A. Of three H atoms localized, two are involved in hydrogen bonds, linking OH groups of the Oc sheet with basal O atoms of the Tet sheet. The basal O atoms (acceptors) of the Tet sheet are rotated close to OH groups (donors) of the Oc sheet of an adjacent layer in order to achieve reasonable lengths and geometries of hydrogen bonds. The structure is interpreted as an example of the order–disorder (OD) structure of more than one kind of layer with a very low degree of desymmetrization.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614020897/wf5112sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614020897/wf5112Isup2.hkl
Contains datablock I

CCDC reference: 1024945

Experimental top

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1.

Results and discussion top

Computing details top

Data collection: CrysAlis PRO, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05); cell refinement: CrysAlis PRO, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05); data reduction: CrysAlis PRO, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
(I) top
Crystal data top
Fe3.539H4O9Si1.461F(000) = 377
Mr = 386.7Dx = 3.448 Mg m3
Monoclinic, CmMo Kα radiation, λ = 0.71073 Å
Hall symbol: C -2yCell parameters from 1042 reflections
a = 5.5033 (3) Åθ = 4.2–30.3°
b = 9.5289 (5) ŵ = 7.04 mm1
c = 7.3328 (5) ÅT = 293 K
β = 104.493 (6)°Plate, black
V = 372.30 (4) Å30.25 × 0.15 × 0.10 mm
Z = 2
Data collection top
Xcalibur, Atlas, Gemini ultra
diffractometer
1117 independent reflections
Radiation source: X-ray tube999 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.020
Detector resolution: 10.3784 pixels mm-1θmax = 30.9°, θmin = 2.9°
ω scansh = 77
Absorption correction: multi-scan
CrysAlis PRO, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 1213
Tmin = 0.554, Tmax = 1l = 1010
2993 measured reflections
Refinement top
Refinement on F14 constraints
R[F2 > 2σ(F2)] = 0.024All H-atom parameters refined
wR(F2) = 0.035Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2)
S = 1.64(Δ/σ)max = 0.019
1117 reflectionsΔρmax = 0.62 e Å3
77 parametersΔρmin = 0.37 e Å3
3 restraintsAbsolute structure: 533 of Friedel pairs used in the refinement
Crystal data top
Fe3.539H4O9Si1.461V = 372.30 (4) Å3
Mr = 386.7Z = 2
Monoclinic, CmMo Kα radiation
a = 5.5033 (3) ŵ = 7.04 mm1
b = 9.5289 (5) ÅT = 293 K
c = 7.3328 (5) Å0.25 × 0.15 × 0.10 mm
β = 104.493 (6)°
Data collection top
Xcalibur, Atlas, Gemini ultra
diffractometer
1117 independent reflections
Absorption correction: multi-scan
CrysAlis PRO, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
999 reflections with I > 3σ(I)
Tmin = 0.554, Tmax = 1Rint = 0.020
2993 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0243 restraints
wR(F2) = 0.035All H-atom parameters refined
S = 1.64Δρmax = 0.62 e Å3
1117 reflectionsΔρmin = 0.37 e Å3
77 parametersAbsolute structure: 533 of Friedel pairs used in the refinement
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Fem10.250.50.60.0116 (3)
Fem20.2516 (2)0.16754 (7)0.59589 (16)0.01178 (17)
Sit10.4519 (2)0.16619 (8)0.19842 (17)0.0091 (3)0.731 (9)
Fet10.4519 (2)0.16619 (8)0.19842 (17)0.0091 (3)0.269 (9)
O10.0109 (11)0.50.1200 (7)0.0302 (19)
O20.1426 (8)0.2172 (4)0.1208 (5)0.0310 (13)
O40.5371 (7)0.1633 (3)0.4448 (5)0.0164 (11)
Oh10.5279 (10)0.50.4467 (7)0.0163 (16)
Oh20.0335 (11)0.50.7365 (7)0.0146 (17)
Oh30.4631 (8)0.3357 (3)0.7374 (5)0.0145 (11)
H10.493 (14)0.50.319 (3)0.0195*
H20.005 (14)0.50.863 (3)0.0175*
H30.507 (10)0.334 (5)0.863 (3)0.0174*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fem10.0093 (4)0.0093 (4)0.0174 (5)00.0053 (4)0
Fem20.0091 (3)0.0085 (3)0.0187 (3)0.0001 (3)0.0053 (2)0.0001 (3)
Sit10.0090 (4)0.0102 (4)0.0081 (5)0.0005 (11)0.0023 (3)0.0008 (9)
Fet10.0090 (4)0.0102 (4)0.0081 (5)0.0005 (11)0.0023 (3)0.0008 (9)
O10.033 (3)0.035 (3)0.023 (3)00.006 (2)0
O20.030 (2)0.036 (2)0.027 (2)0.0011 (19)0.0070 (18)0.0003 (18)
O40.0156 (17)0.0170 (19)0.0171 (17)0.0008 (14)0.0046 (16)0.0008 (13)
Oh10.016 (2)0.017 (3)0.016 (2)00.004 (2)0
Oh20.015 (2)0.014 (2)0.015 (3)00.006 (3)0
Oh30.0137 (17)0.0137 (18)0.016 (2)0.0013 (16)0.0034 (17)0.0003 (13)
Geometric parameters (Å, º) top
Fem1—O4i2.103 (3)Fem2—Oh32.096 (3)
Fem1—O4ii2.103 (3)Fem2—Oh3ii2.103 (5)
Fem1—Oh12.112 (6)Sit1—O1v1.714 (2)
Fem1—Oh22.054 (6)Sit1—O21.724 (4)
Fem1—Oh32.061 (3)Sit1—O2vi1.721 (5)
Fem1—Oh3iii2.061 (3)Sit1—O41.750 (4)
Fem2—O42.137 (4)Oh1—H10.91 (2)
Fem2—O4ii2.136 (3)Oh2—H20.90 (2)
Fem2—Oh1iv2.142 (3)Oh3—H30.89 (2)
Fem2—Oh2v2.098 (3)
O4i—Fem1—O4ii95.47 (12)O4—Fem2—Oh383.22 (15)
O4i—Fem1—Oh195.26 (14)O4—Fem2—Oh3ii177.50 (13)
O4i—Fem1—Oh282.84 (14)O4ii—Fem2—Oh1iv97.19 (13)
O4i—Fem1—Oh3176.58 (15)O4ii—Fem2—Oh2v178.1 (2)
O4i—Fem1—Oh3iii82.78 (13)O4ii—Fem2—Oh381.15 (13)
O4ii—Fem1—Oh195.26 (14)O4ii—Fem2—Oh3ii83.08 (15)
O4ii—Fem1—Oh282.84 (14)Oh1iv—Fem2—Oh2v82.24 (14)
O4ii—Fem1—Oh382.78 (13)Oh1iv—Fem2—Oh3178.33 (14)
O4ii—Fem1—Oh3iii176.58 (15)Oh1iv—Fem2—Oh3ii80.35 (18)
Oh1—Fem1—Oh2177.16 (17)Oh2v—Fem2—Oh399.42 (14)
Oh1—Fem1—Oh382.01 (14)Oh2v—Fem2—Oh3ii98.5 (2)
Oh1—Fem1—Oh3iii82.01 (14)Oh3—Fem2—Oh3ii99.28 (16)
Oh2—Fem1—Oh399.81 (15)O1v—Sit1—O2109.9 (2)
Oh2—Fem1—Oh3iii99.81 (15)O1v—Sit1—O2vi110.6 (3)
Oh3—Fem1—Oh3iii98.81 (13)O1v—Sit1—O4107.9 (2)
O4—Fem2—O4ii97.36 (15)O2—Sit1—O2vi110.0 (2)
O4—Fem2—Oh1iv97.15 (18)O2—Sit1—O4109.4 (2)
O4—Fem2—Oh2v80.98 (19)O2vi—Sit1—O4108.90 (18)
Symmetry codes: (i) x1/2, y+1/2, z; (ii) x1/2, y+1/2, z; (iii) x, y+1, z; (iv) x1/2, y1/2, z; (v) x+1/2, y1/2, z; (vi) x+1/2, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
Oh2—H2···O1vii0.90 (2)1.91 (3)2.784 (7)164 (7)
Oh3—H3···O2viii0.89 (2)1.91 (2)2.782 (5)165 (5)
Symmetry codes: (vii) x, y, z+1; (viii) x+1/2, y+1/2, z+1.

Experimental details

Crystal data
Chemical formulaFe3.539H4O9Si1.461
Mr386.7
Crystal system, space groupMonoclinic, Cm
Temperature (K)293
a, b, c (Å)5.5033 (3), 9.5289 (5), 7.3328 (5)
β (°) 104.493 (6)
V3)372.30 (4)
Z2
Radiation typeMo Kα
µ (mm1)7.04
Crystal size (mm)0.25 × 0.15 × 0.10
Data collection
DiffractometerXcalibur, Atlas, Gemini ultra
diffractometer
Absorption correctionMulti-scan
CrysAlis PRO, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
Tmin, Tmax0.554, 1
No. of measured, independent and
observed [I > 3σ(I)] reflections
2993, 1117, 999
Rint0.020
(sin θ/λ)max1)0.723
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.035, 1.64
No. of reflections1117
No. of parameters77
No. of restraints3
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)0.62, 0.37
Absolute structure533 of Friedel pairs used in the refinement

Computer programs: CrysAlis PRO, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05).

 

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