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The continuous rotation electron diffraction (cRED) method has the capability of providing fast three-dimensional electron diffraction data collection on existing and future transmission electron microscopes; unknown structures could be potentially solved and refined using cRED data collected from nano- and submicrometre-sized crystals. However, structure refinements of cRED data using SHELXL often lead to relatively high R1 values when compared with those refined against single-crystal X-ray diffraction data. It is therefore necessary to analyse the quality of the structural models refined against cRED data. In this work, multiple cRED data sets collected from different crystals of an oxofluoride (FeSeO3F) and a zeolite (ZSM-5) with known structures are used to assess the data consistency and quality and, more importantly, the accuracy of the structural models refined against these data sets. An evaluation of the precision and consistency of the cRED data by examination of the statistics obtained from the data processing software DIALS is presented. It is shown that, despite the high R1 values caused by dynamical scattering and other factors, the refined atomic positions obtained from the cRED data collected for different crystals are consistent with those of the reference models refined against single-crystal X-ray diffraction data. The results serve as a reference for the quality of the cRED data and the achievable accuracy of the structural parameters.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600576718007604/kc5069sup1.cif
Contains datablocks dataset1, dataset2, dataset3, dataset4, dataset5, dataset6, dataset7, dataset8, dataset9, dataset10

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576718007604/kc5069dataset1sup2.hkl
Contains datablock dataset1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576718007604/kc5069dataset2sup3.hkl
Contains datablock dataset2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576718007604/kc5069dataset3sup4.hkl
Contains datablock dataset3

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576718007604/kc5069dataset4sup5.hkl
Contains datablock dataset4

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576718007604/kc5069dataset5sup6.hkl
Contains datablock dataset5

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576718007604/kc5069dataset6sup7.hkl
Contains datablock dataset6

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576718007604/kc5069dataset7sup8.hkl
Contains datablock dataset7

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576718007604/kc5069dataset8sup9.hkl
Contains datablock dataset8

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576718007604/kc5069dataset9sup10.hkl
Contains datablock dataset9

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600576718007604/kc5069dataset10sup11.hkl
Contains datablock dataset10

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S1600576718007604/kc5069sup12.pdf
Supplementary tables

CCDC references: 1844586; 1844587; 1844588; 1844589; 1844590; 1844591; 1844592; 1844593; 1844594; 1844595

Computing details top

Program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2014) for dataset1, dataset2, dataset3, dataset4, dataset5, dataset6; SHELXL2018/3 (Sheldrick, 2018) for dataset7, dataset8, dataset9, dataset10.

(dataset1) top
Crystal data top
FFeO3SeZ = 4
Mr = 201.80F(000) = 88
Monoclinic, P21/nDx = 4.359 Mg m3
a = 4.956 (1) ÅCell parameters from 640 reflections
b = 5.202 (1) Åθ = 0.1–0.9°
c = 12.040 (2) ŵ = 0.000 mm1
β = 97.87 (3)°T = 293 K
V = 307.48 (11) Å3Plate, white
Data collection top
JEOL JEM-2100
diffractometer
θmax = 0.9°, θmin = 0.1°
1257 measured reflectionsh = 66
462 independent reflectionsk = 55
317 reflections with I > 2σ(I)l = 1515
Rint = 0.210
Refinement top
Refinement on F20 restraints
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.1102P)2]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.152(Δ/σ)max = 0.060
wR(F2) = 0.368Δρmax = 0.35 e Å3
S = 1.25Δρmin = 0.36 e Å3
462 reflectionsExtinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
26 parametersExtinction coefficient: 4725 (71)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Se10.5168 (9)0.3609 (11)0.3332 (3)0.0052 (13)*
Fe10.4583 (10)0.2562 (13)0.0724 (4)0.0052 (14)*
O10.337 (3)0.628 (4)0.3507 (11)0.013 (3)*
O20.806 (3)0.440 (3)0.4234 (10)0.007 (3)*
O30.623 (3)0.426 (3)0.2093 (9)0.006 (3)*
F10.270 (3)0.570 (3)0.0114 (10)0.009 (3)*
Geometric parameters (Å, º) top
Se1—O11.680 (18)Fe1—O2iii2.014 (16)
Se1—O31.682 (12)Fe1—O2iv2.111 (15)
Se1—O21.727 (14)O1—Fe1v1.952 (16)
Fe1—O31.947 (15)O2—Fe1vi2.014 (16)
Fe1—O1i1.952 (16)O2—Fe1vii2.111 (15)
Fe1—F11.970 (16)F1—Fe1ii2.006 (14)
Fe1—F1ii2.006 (14)
O1—Se1—O3100.4 (7)F1ii—Fe1—O2iii87.4 (6)
O1—Se1—O297.8 (8)O3—Fe1—O2iv176.0 (6)
O3—Se1—O2100.2 (7)O1i—Fe1—O2iv92.0 (7)
O3—Fe1—O1i90.4 (6)F1—Fe1—O2iv89.3 (6)
O3—Fe1—F193.6 (6)F1ii—Fe1—O2iv88.6 (5)
O1i—Fe1—F196.5 (7)O2iii—Fe1—O2iv76.4 (6)
O3—Fe1—F1ii89.4 (6)Se1—O1—Fe1v142.0 (10)
O1i—Fe1—F1ii172.3 (8)Se1—O2—Fe1vi129.7 (8)
F1—Fe1—F1ii75.8 (6)Se1—O2—Fe1vii126.1 (8)
O3—Fe1—O2iii100.1 (6)Fe1vi—O2—Fe1vii103.6 (6)
O1i—Fe1—O2iii100.2 (7)Se1—O3—Fe1120.9 (9)
F1—Fe1—O2iii158.2 (5)Fe1—F1—Fe1ii104.2 (6)
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x+1, y+1, z; (iii) x+3/2, y1/2, z+1/2; (iv) x1/2, y+1/2, z1/2; (v) x+1/2, y+1/2, z+1/2; (vi) x+3/2, y+1/2, z+1/2; (vii) x+1/2, y+1/2, z+1/2.
(dataset2) top
Crystal data top
FFeO3SeZ = 4
Mr = 201.80F(000) = 88
Monoclinic, P21/nDx = 4.359 Mg m3
a = 4.956 (1) ÅCell parameters from 714 reflections
b = 5.202 (1) Åθ = 0.2–0.9°
c = 12.040 (2) ŵ = 0.000 mm1
β = 97.87 (3)°T = 293 K
V = 307.48 (11) Å3Plate, white
Data collection top
JEOL JEM-2100
diffractometer
θmax = 0.9°, θmin = 0.2°
1319 measured reflectionsh = 66
487 independent reflectionsk = 66
418 reflections with I > 2σ(I)l = 1313
Rint = 0.210
Refinement top
Refinement on F20 restraints
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.1804P)2 + 1.974P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.189(Δ/σ)max = 0.693
wR(F2) = 0.471Δρmax = 0.39 e Å3
S = 1.24Δρmin = 0.38 e Å3
487 reflectionsExtinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
26 parametersExtinction coefficient: 11626 (99)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Se10.5181 (11)0.3574 (13)0.3345 (6)0.0010 (17)*
Fe10.4575 (12)0.2581 (14)0.0722 (6)0.0020 (17)*
O10.329 (4)0.624 (4)0.3470 (19)0.011 (4)*
O20.807 (3)0.434 (4)0.4238 (18)0.009 (4)*
O30.616 (3)0.425 (4)0.2070 (17)0.006 (4)*
F10.271 (3)0.573 (4)0.0107 (17)0.006 (3)*
Geometric parameters (Å, º) top
Se1—O11.69 (2)Fe1—O2iii2.05 (2)
Se1—O31.71 (2)Fe1—O2iv2.09 (2)
Se1—O21.72 (2)O1—Fe1v1.96 (2)
Fe1—O31.91 (2)O2—Fe1vi2.05 (2)
Fe1—O1i1.96 (2)O2—Fe1vii2.09 (2)
Fe1—F11.976 (19)F1—Fe1ii1.986 (19)
Fe1—F1ii1.986 (19)
O1—Se1—O398.1 (11)F1ii—Fe1—O2iii87.2 (8)
O1—Se1—O2100.2 (10)O3—Fe1—O2iv176.5 (8)
O3—Se1—O2101.5 (9)O1i—Fe1—O2iv93.2 (9)
O3—Fe1—O1i88.9 (9)F1—Fe1—O2iv89.0 (9)
O3—Fe1—F193.4 (9)F1ii—Fe1—O2iv88.2 (8)
O1i—Fe1—F198.5 (8)O2iii—Fe1—O2iv76.2 (9)
O3—Fe1—F1ii89.9 (8)Se1—O1—Fe1v141.7 (13)
O1i—Fe1—F1ii174.4 (9)Se1—O2—Fe1vi129.1 (12)
F1—Fe1—F1ii76.1 (8)Se1—O2—Fe1vii126.4 (12)
O3—Fe1—O2iii100.8 (9)Fe1vi—O2—Fe1vii103.8 (9)
O1i—Fe1—O2iii98.4 (9)Se1—O3—Fe1122.4 (11)
F1—Fe1—O2iii158.1 (10)Fe1—F1—Fe1ii103.9 (8)
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x+1, y+1, z; (iii) x+3/2, y1/2, z+1/2; (iv) x1/2, y+1/2, z1/2; (v) x+1/2, y+1/2, z+1/2; (vi) x+3/2, y+1/2, z+1/2; (vii) x+1/2, y+1/2, z+1/2.
(dataset3) top
Crystal data top
FFeO3SeZ = 4
Mr = 201.80F(000) = 88
Monoclinic, P21/nDx = 4.359 Mg m3
a = 4.956 (1) ÅCell parameters from 725 reflections
b = 5.202 (1) Åθ = 0.2–0.9°
c = 12.040 (2) ŵ = 0.000 mm1
β = 97.87 (3)°T = 293 K
V = 307.48 (11) Å3Plate, white
Data collection top
JEOL JEM-2100
diffractometer
θmax = 0.9°, θmin = 0.2°
1497 measured reflectionsh = 66
495 independent reflectionsk = 66
400 reflections with I > 2σ(I)l = 1212
Rint = 0.205
Refinement top
Refinement on F20 restraints
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.1243P)2 + 1.3153P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.170(Δ/σ)max = 0.195
wR(F2) = 0.393Δρmax = 0.36 e Å3
S = 1.19Δρmin = 0.40 e Å3
495 reflectionsExtinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
26 parametersExtinction coefficient: 6855 (79)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Se10.5172 (10)0.3574 (9)0.3342 (6)0.0027 (13)*
Fe10.4566 (11)0.2557 (10)0.0721 (6)0.0072 (14)*
O10.327 (3)0.621 (3)0.3474 (19)0.015 (3)*
O20.809 (3)0.432 (2)0.4234 (18)0.010 (3)*
O30.620 (3)0.419 (2)0.2088 (17)0.008 (3)*
F10.268 (3)0.573 (2)0.0091 (17)0.011 (3)*
Geometric parameters (Å, º) top
Se1—O11.686 (16)Fe1—O2iii2.042 (14)
Se1—O31.69 (2)Fe1—O2iv2.08 (2)
Se1—O21.722 (17)O1—Fe1v1.94 (2)
Fe1—O31.929 (19)O2—Fe1vi2.042 (14)
Fe1—O1i1.94 (2)O2—Fe1vii2.08 (2)
Fe1—F1ii1.994 (17)F1—Fe1ii1.994 (17)
Fe1—F11.994 (15)
O1—Se1—O399.8 (9)F1—Fe1—O2iii158.0 (9)
O1—Se1—O2100.9 (8)O3—Fe1—O2iv175.8 (7)
O3—Se1—O2100.7 (9)O1i—Fe1—O2iv93.8 (8)
O3—Fe1—O1i88.9 (8)F1ii—Fe1—O2iv88.4 (7)
O3—Fe1—F1ii89.2 (7)F1—Fe1—O2iv88.3 (7)
O1i—Fe1—F1ii174.4 (6)O2iii—Fe1—O2iv76.6 (8)
O3—Fe1—F194.5 (7)Se1—O1—Fe1v142.4 (12)
O1i—Fe1—F198.9 (7)Se1—O2—Fe1vi129.0 (10)
F1ii—Fe1—F176.1 (7)Se1—O2—Fe1vii126.6 (8)
O3—Fe1—O2iii99.8 (7)Fe1vi—O2—Fe1vii103.4 (8)
O1i—Fe1—O2iii98.0 (7)Se1—O3—Fe1122.4 (8)
F1ii—Fe1—O2iii87.5 (6)Fe1ii—F1—Fe1103.9 (7)
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x+1, y+1, z; (iii) x+3/2, y1/2, z+1/2; (iv) x1/2, y+1/2, z1/2; (v) x+1/2, y+1/2, z+1/2; (vi) x+3/2, y+1/2, z+1/2; (vii) x+1/2, y+1/2, z+1/2.
(dataset4) top
Crystal data top
FFeO3SeZ = 4
Mr = 201.80F(000) = 88
Monoclinic, P21/nDx = 4.359 Mg m3
a = 4.956 (1) ÅCell parameters from 643 reflections
b = 5.202 (1) Åθ = 0.2–0.9°
c = 12.040 (2) ŵ = 0.000 mm1
β = 97.87 (3)°T = 293 K
V = 307.48 (11) Å3Plate, white
Data collection top
JEOL JEM-2100
diffractometer
θmax = 0.9°, θmin = 0.2°
1198 measured reflectionsh = 66
460 independent reflectionsk = 66
394 reflections with I > 2σ(I)l = 1213
Rint = 0.196
Refinement top
Refinement on F20 restraints
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.1535P)2 + 1.6983P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.195(Δ/σ)max = 0.688
wR(F2) = 0.447Δρmax = 0.40 e Å3
S = 1.22Δρmin = 0.49 e Å3
460 reflectionsExtinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
26 parametersExtinction coefficient: 10316 (98)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Se10.5189 (10)0.3569 (13)0.3344 (6)0.0010 (16)*
Fe10.4581 (12)0.2558 (13)0.0726 (7)0.0031 (17)*
O10.329 (3)0.620 (4)0.3480 (18)0.007 (4)*
O20.810 (3)0.438 (4)0.427 (2)0.011 (4)*
O30.620 (3)0.424 (4)0.2102 (17)0.004 (4)*
F10.269 (3)0.568 (4)0.0159 (18)0.011 (4)*
Geometric parameters (Å, º) top
Se1—O31.68 (2)Fe1—F1iii2.05 (2)
Se1—O11.682 (19)Fe1—O2iv2.06 (2)
Se1—O21.75 (2)O1—Fe1v1.951 (19)
Fe1—O31.95 (2)O2—Fe1vi2.02 (2)
Fe1—F11.95 (2)O2—Fe1vii2.06 (2)
Fe1—O1i1.951 (19)F1—Fe1iii2.05 (2)
Fe1—O2ii2.02 (2)
O3—Se1—O199.0 (10)O2ii—Fe1—F1iii87.1 (8)
O3—Se1—O2101.5 (9)O3—Fe1—O2iv176.2 (8)
O1—Se1—O299.5 (10)F1—Fe1—O2iv90.6 (9)
O3—Fe1—F192.6 (9)O1i—Fe1—O2iv92.2 (8)
O3—Fe1—O1i89.4 (8)O2ii—Fe1—O2iv74.7 (9)
F1—Fe1—O1i97.3 (8)F1iii—Fe1—O2iv87.8 (8)
O3—Fe1—O2ii101.6 (8)Se1—O1—Fe1v142.9 (12)
F1—Fe1—O2ii158.4 (10)Se1—O2—Fe1vi128.1 (13)
O1i—Fe1—O2ii99.1 (8)Se1—O2—Fe1vii126.3 (12)
O3—Fe1—F1iii90.9 (8)Fe1vi—O2—Fe1vii105.3 (9)
F1—Fe1—F1iii76.3 (8)Se1—O3—Fe1121.6 (10)
O1i—Fe1—F1iii173.6 (8)Fe1—F1—Fe1iii103.7 (8)
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x+3/2, y1/2, z+1/2; (iii) x+1, y+1, z; (iv) x1/2, y+1/2, z1/2; (v) x+1/2, y+1/2, z+1/2; (vi) x+3/2, y+1/2, z+1/2; (vii) x+1/2, y+1/2, z+1/2.
(dataset5) top
Crystal data top
FFeO3SeZ = 4
Mr = 201.80F(000) = 88
Monoclinic, P21/nDx = 4.359 Mg m3
a = 4.956 (1) ÅCell parameters from 769 reflections
b = 5.202 (1) Åθ = 0.1–0.9°
c = 12.040 (2) ŵ = 0.000 mm1
β = 97.87 (3)°T = 293 K
V = 307.48 (11) Å3Plate, white
Data collection top
JEOL JEM-2100
diffractometer
θmax = 0.9°, θmin = 0.1°
1459 measured reflectionsh = 66
582 independent reflectionsk = 66
394 reflections with I > 2σ(I)l = 1515
Rint = 0.308
Refinement top
Refinement on F24 restraints
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.2P)2]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.223(Δ/σ)max = 2.478
wR(F2) = 0.532Δρmax = 0.51 e Å3
S = 1.41Δρmin = 0.56 e Å3
582 reflectionsExtinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
26 parametersExtinction coefficient: 9729 (77)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Se10.5186 (14)0.3578 (10)0.3342 (4)0.0010 (17)*
Fe10.4581 (14)0.2575 (10)0.0731 (5)0.0010 (17)*
O10.324 (4)0.625 (3)0.3455 (13)0.002 (2)*
O20.796 (4)0.431 (3)0.4195 (13)0.002 (2)*
O30.620 (4)0.424 (3)0.2096 (13)0.002 (2)*
F10.271 (4)0.571 (3)0.0105 (13)0.003 (2)*
Geometric parameters (Å, º) top
Se1—O21.644 (17)Fe1—O2iii2.085 (17)
Se1—O31.681 (18)Fe1—O2iv2.149 (16)
Se1—O11.710 (16)O1—Fe1v1.94 (2)
Fe1—O31.932 (17)O2—Fe1vi2.085 (17)
Fe1—O1i1.94 (2)O2—Fe1vii2.149 (16)
Fe1—F11.975 (16)F1—Fe1ii1.993 (17)
Fe1—F1ii1.993 (18)
O2—Se1—O3100.6 (10)F1ii—Fe1—O2iii87.5 (7)
O2—Se1—O1101.2 (8)O3—Fe1—O2iv177.4 (8)
O3—Se1—O198.4 (8)O1i—Fe1—O2iv93.6 (7)
O3—Fe1—O1i88.4 (7)F1—Fe1—O2iv87.0 (6)
O3—Fe1—F194.2 (7)F1ii—Fe1—O2iv88.1 (7)
O1i—Fe1—F198.9 (7)O2iii—Fe1—O2iv79.2 (7)
O3—Fe1—F1ii90.0 (7)Se1—O1—Fe1v141.6 (9)
O1i—Fe1—F1ii174.1 (7)Se1—O2—Fe1vi130.5 (9)
F1—Fe1—F1ii75.5 (8)Se1—O2—Fe1vii127.9 (9)
O3—Fe1—O2iii99.0 (7)Fe1vi—O2—Fe1vii100.8 (7)
O1i—Fe1—O2iii98.4 (7)Se1—O3—Fe1121.9 (10)
F1—Fe1—O2iii158.5 (8)Fe1—F1—Fe1ii104.5 (8)
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x+1, y+1, z; (iii) x+3/2, y1/2, z+1/2; (iv) x1/2, y+1/2, z1/2; (v) x+1/2, y+1/2, z+1/2; (vi) x+3/2, y+1/2, z+1/2; (vii) x+1/2, y+1/2, z+1/2.
(dataset6) top
Crystal data top
FFeO3SeZ = 4
Mr = 201.80F(000) = 88
Monoclinic, P21/nDx = 4.359 Mg m3
a = 4.956 (1) ÅCell parameters from 590 reflections
b = 5.202 (1) Åθ = 0.2–0.9°
c = 12.040 (2) ŵ = 0.000 mm1
β = 97.87 (3)°T = 293 K
V = 307.48 (11) Å3Plate, white
Data collection top
JEOL JEM-2100
diffractometer
θmax = 0.9°, θmin = 0.2°
1173 measured reflectionsh = 66
498 independent reflectionsk = 66
400 reflections with I > 2σ(I)l = 1213
Rint = 0.158
Refinement top
Refinement on F20 restraints
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.1251P)2 + 0.6919P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.144(Δ/σ)max = 0.078
wR(F2) = 0.386Δρmax = 0.33 e Å3
S = 1.18Δρmin = 0.36 e Å3
498 reflectionsExtinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
26 parametersExtinction coefficient: 4973 (63)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Se10.5180 (8)0.3599 (7)0.3345 (5)0.0049 (12)*
Fe10.4595 (9)0.2557 (8)0.0717 (5)0.0091 (13)*
O10.332 (3)0.621 (2)0.3468 (16)0.017 (3)*
O20.809 (3)0.439 (2)0.4254 (15)0.013 (3)*
O30.617 (2)0.422 (2)0.2083 (14)0.010 (2)*
F10.268 (2)0.5717 (19)0.0096 (13)0.012 (2)*
Geometric parameters (Å, º) top
Se1—O11.660 (13)Fe1—O2iii2.007 (12)
Se1—O31.690 (16)Fe1—O2iv2.079 (17)
Se1—O21.735 (15)O1—Fe1v1.983 (16)
Fe1—O31.928 (16)O2—Fe1vi2.007 (12)
Fe1—O1i1.983 (16)O2—Fe1vii2.079 (17)
Fe1—F1ii1.986 (13)F1—Fe1ii1.986 (13)
Fe1—F11.991 (13)
O1—Se1—O399.0 (8)F1—Fe1—O2iii157.9 (7)
O1—Se1—O2100.0 (7)O3—Fe1—O2iv176.7 (5)
O3—Se1—O2101.8 (7)O1i—Fe1—O2iv92.6 (6)
O3—Fe1—O1i88.5 (7)F1ii—Fe1—O2iv89.6 (6)
O3—Fe1—F1ii89.7 (6)F1—Fe1—O2iv89.2 (6)
O1i—Fe1—F1ii173.6 (5)O2iii—Fe1—O2iv75.7 (7)
O3—Fe1—F193.7 (6)Se1—O1—Fe1v141.7 (9)
O1i—Fe1—F197.8 (6)Se1—O2—Fe1vi129.0 (8)
F1ii—Fe1—F176.2 (5)Se1—O2—Fe1vii126.2 (7)
O3—Fe1—O2iii101.0 (6)Fe1vi—O2—Fe1vii104.3 (7)
O1i—Fe1—O2iii99.0 (5)Se1—O3—Fe1123.2 (7)
F1ii—Fe1—O2iii87.4 (5)Fe1ii—F1—Fe1103.8 (5)
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x+1, y+1, z; (iii) x+3/2, y1/2, z+1/2; (iv) x1/2, y+1/2, z1/2; (v) x+1/2, y+1/2, z+1/2; (vi) x+3/2, y+1/2, z+1/2; (vii) x+1/2, y+1/2, z+1/2.
(dataset7) top
Crystal data top
O24Si12F(000) = 939
Mr = 721.01Dx = 1.796 Mg m3
Orthorhombic, PnmaCell parameters from 8815 reflections
a = 20.022 (4) Åθ = 0.1–0.8°
b = 19.899 (4) ŵ = 0.000 mm1
c = 13.383 (3) ÅT = 293 K
V = 5332.0 (19) Å3Plate, white
Z = 8
Data collection top
JEOL JEM-2100
diffractometer
θmax = 0.8°, θmin = 0.1°
16752 measured reflectionsh = 2323
3330 independent reflectionsk = 2020
1743 reflections with I > 2σ(I)l = 1313
Rint = 0.232
Refinement top
Refinement on F248 restraints
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.2111P)2 + 2.380P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.195(Δ/σ)max = 0.003
wR(F2) = 0.508Δρmax = 0.35 e Å3
S = 1.13Δρmin = 0.19 e Å3
3330 reflectionsExtinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
150 parametersExtinction coefficient: 704 (88)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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*/Ueq
Si010.4231 (2)0.0571 (3)0.3341 (5)0.0143 (16)*
Si020.3093 (2)0.0296 (4)0.1864 (6)0.0184 (17)*
Si030.2794 (2)0.0616 (3)0.0361 (5)0.0164 (17)*
Si040.1223 (2)0.0637 (3)0.0309 (5)0.0149 (16)*
Si050.0723 (2)0.0284 (3)0.1822 (5)0.0110 (16)*
Si060.1883 (2)0.0597 (3)0.3238 (6)0.0155 (16)*
Si070.4231 (2)0.1720 (3)0.3231 (5)0.0141 (16)*
Si080.3093 (2)0.1300 (4)0.1804 (6)0.0174 (17)*
Si090.2743 (2)0.1724 (3)0.0341 (5)0.0153 (17)*
Si100.1194 (3)0.1726 (4)0.0308 (6)0.0193 (17)*
Si110.0695 (2)0.1304 (3)0.1813 (5)0.0124 (16)*
Si120.1879 (3)0.1725 (4)0.3144 (6)0.0226 (18)*
O010.3743 (5)0.0552 (6)0.2407 (9)0.041 (3)*
O020.3081 (5)0.0586 (7)0.0747 (10)0.038 (3)*
O030.2008 (3)0.0578 (7)0.0292 (12)0.042 (3)*
O040.0951 (6)0.0627 (7)0.0807 (9)0.049 (3)*
O050.1164 (5)0.0550 (6)0.2712 (10)0.035 (3)*
O060.2455 (5)0.0556 (7)0.2433 (11)0.049 (3)*
O070.3753 (5)0.1570 (7)0.2303 (10)0.040 (3)*
O080.3093 (5)0.1554 (7)0.0690 (9)0.038 (3)*
O090.1966 (4)0.1542 (6)0.0242 (10)0.029 (3)*
O100.0863 (6)0.1634 (9)0.0769 (10)0.063 (4)*
O110.1179 (5)0.1591 (7)0.2645 (11)0.041 (3)*
O120.2441 (5)0.1542 (7)0.2363 (10)0.051 (4)*
O130.3072 (7)0.0509 (8)0.1751 (18)0.075 (5)*
O140.0788 (6)0.0512 (6)0.1717 (12)0.047 (3)*
O150.4160 (5)0.1276 (5)0.3879 (9)0.035 (3)*
O160.4083 (6)0.0019 (7)0.4109 (12)0.053 (4)*
O170.4009 (5)0.1323 (6)0.4196 (10)0.039 (3)*
O180.1915 (4)0.1301 (6)0.3790 (10)0.034 (3)*
O190.1926 (5)0.0024 (6)0.4060 (11)0.047 (3)*
O200.1977 (5)0.1304 (7)0.4129 (11)0.047 (3)*
O210.0030 (4)0.0489 (6)0.2077 (10)0.032 (3)*
O220.0038 (4)0.1516 (6)0.2109 (10)0.039 (3)*
O230.4236 (8)0.2500000.3504 (17)0.046 (5)*
O240.1911 (6)0.2500000.3473 (15)0.036 (4)*
O250.2853 (7)0.2500000.0599 (14)0.032 (4)*
O260.1104 (6)0.2500000.0615 (14)0.030 (4)*
Geometric parameters (Å, º) top
Si01—O151.582 (10)Si07—O171.578 (13)
Si01—O011.587 (10)Si07—O22i1.585 (9)
Si01—O161.588 (14)Si07—O231.593 (8)
Si01—O21i1.591 (10)Si07—O071.597 (13)
Si02—O061.574 (12)Si08—O081.574 (14)
Si02—O011.575 (11)Si08—O071.575 (11)
Si02—O021.602 (14)Si08—O131.577 (16)
Si02—O131.609 (16)Si08—O121.580 (9)
Si03—O031.577 (7)Si09—O081.584 (13)
Si03—O021.592 (14)Si09—O18ii1.592 (12)
Si03—O19ii1.592 (8)Si09—O251.598 (8)
Si03—O20ii1.597 (13)Si09—O091.601 (9)
Si04—O031.577 (7)Si10—O15ii1.578 (10)
Si04—O16ii1.579 (14)Si10—O091.592 (9)
Si04—O17ii1.587 (13)Si10—O101.597 (13)
Si04—O041.590 (13)Si10—O261.604 (8)
Si05—O051.574 (12)Si11—O221.577 (9)
Si05—O041.587 (11)Si11—O101.580 (12)
Si05—O141.597 (13)Si11—O111.583 (12)
Si05—O211.598 (10)Si11—O141.593 (13)
Si06—O061.575 (13)Si12—O111.574 (11)
Si06—O181.584 (13)Si12—O201.575 (14)
Si06—O191.587 (10)Si12—O121.579 (10)
Si06—O051.605 (10)Si12—O241.605 (9)
O15—Si01—O01109.0 (7)O08—Si09—O25109.5 (9)
O15—Si01—O16110.1 (9)O18ii—Si09—O25107.1 (9)
O01—Si01—O16112.2 (8)O08—Si09—O09108.0 (7)
O15—Si01—O21i109.5 (6)O18ii—Si09—O09111.0 (7)
O01—Si01—O21i107.1 (7)O25—Si09—O09111.8 (7)
O16—Si01—O21i109.0 (7)O15ii—Si10—O09110.1 (7)
O06—Si02—O01109.9 (9)O15ii—Si10—O10111.8 (8)
O06—Si02—O02108.8 (8)O09—Si10—O10109.0 (8)
O01—Si02—O02109.0 (7)O15ii—Si10—O26108.6 (8)
O06—Si02—O13110.6 (9)O09—Si10—O26110.2 (7)
O01—Si02—O13112.7 (8)O10—Si10—O26107.1 (9)
O02—Si02—O13105.7 (11)O22—Si11—O10108.0 (8)
O03—Si03—O02107.7 (8)O22—Si11—O11107.3 (7)
O03—Si03—O19ii110.0 (7)O10—Si11—O11109.9 (8)
O02—Si03—O19ii107.2 (8)O22—Si11—O14113.2 (7)
O03—Si03—O20ii110.7 (7)O10—Si11—O14108.3 (10)
O02—Si03—O20ii109.1 (8)O11—Si11—O14110.0 (8)
O19ii—Si03—O20ii112.1 (9)O11—Si12—O20112.1 (8)
O03—Si04—O16ii109.6 (8)O11—Si12—O12108.3 (8)
O03—Si04—O17ii111.2 (7)O20—Si12—O12110.0 (8)
O16ii—Si04—O17ii110.5 (9)O11—Si12—O24108.3 (8)
O03—Si04—O04109.1 (8)O20—Si12—O24106.1 (10)
O16ii—Si04—O04108.7 (8)O12—Si12—O24112.1 (9)
O17ii—Si04—O04107.6 (8)Si02—O01—Si01151.6 (10)
O05—Si05—O04110.0 (8)Si03—O02—Si02152.6 (9)
O05—Si05—O14110.7 (8)Si03—O03—Si04171.9 (11)
O04—Si05—O14109.1 (9)Si05—O04—Si04155.2 (11)
O05—Si05—O21106.4 (7)Si05—O05—Si06148.8 (9)
O04—Si05—O21110.2 (7)Si02—O06—Si06159.8 (11)
O14—Si05—O21110.4 (7)Si08—O07—Si07153.8 (10)
O06—Si06—O18109.6 (7)Si08—O08—Si09153.3 (7)
O06—Si06—O19113.4 (8)Si10—O09—Si09152.4 (9)
O18—Si06—O19108.1 (9)Si11—O10—Si10159.1 (12)
O06—Si06—O05110.4 (8)Si12—O11—Si11154.8 (10)
O18—Si06—O05107.0 (6)Si12—O12—Si08166.6 (11)
O19—Si06—O05108.1 (7)Si08—O13—Si02171.5 (17)
O17—Si07—O22i111.5 (7)Si11—O14—Si05164.9 (10)
O17—Si07—O23107.6 (10)Si10iii—O15—Si01149.0 (9)
O22i—Si07—O23108.1 (8)Si04iii—O16—Si01165.3 (10)
O17—Si07—O07111.9 (7)Si07—O17—Si04iii148.8 (10)
O22i—Si07—O07106.3 (7)Si06—O18—Si09iii145.7 (9)
O23—Si07—O07111.3 (9)Si06—O19—Si03iii158.6 (9)
O08—Si08—O07107.0 (7)Si12—O20—Si03iii148.2 (12)
O08—Si08—O13106.1 (11)Si01iv—O21—Si05145.9 (10)
O07—Si08—O13112.5 (8)Si11—O22—Si07iv148.7 (10)
O08—Si08—O12110.5 (8)Si07—O23—Si07v153.5 (16)
O07—Si08—O12112.9 (9)Si12v—O24—Si12147.8 (15)
O13—Si08—O12107.7 (9)Si09—O25—Si09v150.2 (13)
O08—Si09—O18ii109.4 (7)Si10v—O26—Si10147.6 (13)
Symmetry codes: (i) x+1/2, y, z1/2; (ii) x+1/2, y, z+1/2; (iii) x+1/2, y, z1/2; (iv) x1/2, y, z1/2; (v) x, y1/2, z.
(dataset8) top
Crystal data top
O24Si12F(000) = 939
Mr = 721.01Dx = 1.796 Mg m3
Orthorhombic, PnmaCell parameters from 9808 reflections
a = 20.022 (4) Åθ = 0.1–0.8°
b = 19.899 (4) ŵ = 0.000 mm1
c = 13.383 (3) ÅT = 293 K
V = 5332.0 (19) Å3Plate, white
Z = 8
Data collection top
JEOL JEM-2100
diffractometer
θmax = 0.8°, θmin = 0.1°
17564 measured reflectionsh = 2323
3390 independent reflectionsk = 2020
2082 reflections with I > 2σ(I)l = 1313
Rint = 0.191
Refinement top
Refinement on F248 restraints
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.1964P)2 + 4.9252P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.197(Δ/σ)max < 0.001
wR(F2) = 0.508Δρmax = 0.24 e Å3
S = 1.13Δρmin = 0.16 e Å3
3390 reflectionsExtinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
150 parametersExtinction coefficient: 874 (100)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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*/Ueq
Si010.4231 (3)0.0574 (3)0.3355 (5)0.0222 (17)*
Si020.3088 (3)0.0294 (4)0.1883 (6)0.0274 (19)*
Si030.2797 (3)0.0616 (3)0.0353 (6)0.0246 (18)*
Si040.1226 (2)0.0639 (3)0.0287 (6)0.0219 (17)*
Si050.0725 (3)0.0285 (3)0.1836 (5)0.0188 (17)*
Si060.1875 (3)0.0598 (3)0.3265 (6)0.0216 (17)*
Si070.4228 (2)0.1718 (3)0.3245 (5)0.0211 (17)*
Si080.3085 (3)0.1299 (4)0.1834 (6)0.0265 (18)*
Si090.2746 (3)0.1724 (3)0.0319 (5)0.0231 (18)*
Si100.1198 (3)0.1723 (4)0.0300 (6)0.0266 (18)*
Si110.0692 (2)0.1301 (3)0.1819 (5)0.0210 (17)*
Si120.1871 (3)0.1729 (4)0.3167 (6)0.0294 (19)*
O010.3738 (5)0.0543 (7)0.2432 (10)0.050 (3)*
O020.3080 (5)0.0598 (7)0.0762 (10)0.047 (3)*
O030.2011 (3)0.0574 (7)0.0316 (13)0.048 (3)*
O040.0960 (6)0.0617 (7)0.0822 (10)0.058 (4)*
O050.1163 (5)0.0555 (6)0.2733 (10)0.043 (3)*
O060.2451 (5)0.0559 (7)0.2457 (10)0.057 (4)*
O070.3746 (5)0.1572 (7)0.2330 (11)0.053 (3)*
O080.3094 (5)0.1550 (7)0.0715 (10)0.046 (3)*
O090.1971 (4)0.1546 (7)0.0263 (11)0.042 (3)*
O100.0868 (7)0.1647 (9)0.0789 (11)0.080 (5)*
O110.1175 (5)0.1580 (7)0.2663 (10)0.051 (3)*
O120.2429 (5)0.1529 (7)0.2391 (10)0.056 (4)*
O130.3078 (7)0.0508 (8)0.1803 (18)0.082 (5)*
O140.0787 (6)0.0510 (6)0.1716 (13)0.058 (4)*
O150.4163 (5)0.1279 (6)0.3890 (10)0.045 (3)*
O160.4082 (6)0.0023 (8)0.4117 (13)0.064 (4)*
O170.4014 (5)0.1319 (6)0.4222 (9)0.047 (3)*
O180.1902 (5)0.1304 (7)0.3809 (11)0.045 (3)*
O190.1918 (5)0.0026 (6)0.4079 (12)0.056 (4)*
O200.1973 (6)0.1295 (7)0.4152 (11)0.057 (4)*
O210.0027 (5)0.0495 (6)0.2060 (10)0.040 (3)*
O220.0044 (4)0.1523 (6)0.2096 (11)0.047 (3)*
O230.4250 (8)0.2500000.3529 (17)0.053 (5)*
O240.1908 (7)0.2500000.3482 (17)0.050 (5)*
O250.2851 (7)0.2500000.0579 (14)0.039 (4)*
O260.1101 (7)0.2500000.0600 (15)0.044 (4)*
Geometric parameters (Å, º) top
Si01—O011.582 (11)Si07—O22i1.577 (9)
Si01—O151.583 (13)Si07—O071.586 (13)
Si01—O21i1.593 (11)Si07—O171.588 (11)
Si01—O161.594 (15)Si07—O231.602 (8)
Si02—O011.575 (11)Si08—O131.575 (16)
Si02—O061.579 (10)Si08—O071.576 (12)
Si02—O131.599 (16)Si08—O121.577 (9)
Si02—O021.618 (15)Si08—O081.580 (14)
Si03—O20ii1.574 (13)Si09—O081.587 (13)
Si03—O031.577 (7)Si09—O091.594 (10)
Si03—O19ii1.593 (9)Si09—O251.596 (8)
Si03—O021.596 (14)Si09—O18ii1.599 (13)
Si04—O041.577 (13)Si10—O15ii1.574 (13)
Si04—O031.578 (7)Si10—O091.588 (10)
Si04—O17ii1.580 (12)Si10—O101.608 (14)
Si04—O16ii1.587 (14)Si10—O261.608 (9)
Si05—O051.581 (13)Si11—O101.581 (12)
Si05—O041.581 (11)Si11—O221.582 (9)
Si05—O211.591 (10)Si11—O111.587 (10)
Si05—O141.594 (14)Si11—O141.592 (14)
Si06—O191.577 (12)Si12—O111.577 (9)
Si06—O061.582 (10)Si12—O121.578 (10)
Si06—O181.582 (13)Si12—O201.589 (11)
Si06—O051.597 (11)Si12—O241.592 (9)
O01—Si01—O15109.5 (7)O08—Si09—O25110.1 (9)
O01—Si01—O21i107.9 (8)O09—Si09—O25110.7 (8)
O15—Si01—O21i109.0 (7)O08—Si09—O18ii109.2 (8)
O01—Si01—O16110.7 (8)O09—Si09—O18ii110.2 (7)
O15—Si01—O16110.8 (10)O25—Si09—O18ii106.8 (9)
O21i—Si01—O16108.9 (7)O15ii—Si10—O09110.2 (8)
O01—Si02—O06109.6 (9)O15ii—Si10—O10112.5 (9)
O01—Si02—O13110.8 (9)O09—Si10—O10110.6 (8)
O06—Si02—O13110.9 (9)O15ii—Si10—O26108.2 (9)
O01—Si02—O02108.8 (7)O09—Si10—O26109.8 (8)
O06—Si02—O02108.5 (8)O10—Si10—O26105.5 (10)
O13—Si02—O02108.1 (11)O10—Si11—O22106.8 (8)
O20ii—Si03—O03110.5 (8)O10—Si11—O11109.4 (9)
O20ii—Si03—O19ii112.6 (9)O22—Si11—O11107.6 (8)
O03—Si03—O19ii109.2 (7)O10—Si11—O14109.2 (10)
O20ii—Si03—O02108.1 (8)O22—Si11—O14114.1 (7)
O03—Si03—O02108.9 (8)O11—Si11—O14109.6 (8)
O19ii—Si03—O02107.5 (8)O11—Si12—O12107.3 (8)
O04—Si04—O03111.0 (9)O11—Si12—O20111.5 (8)
O04—Si04—O17ii108.2 (8)O12—Si12—O20108.5 (8)
O03—Si04—O17ii111.3 (7)O11—Si12—O24109.6 (8)
O04—Si04—O16ii108.7 (9)O12—Si12—O24112.6 (9)
O03—Si04—O16ii108.2 (8)O20—Si12—O24107.3 (11)
O17ii—Si04—O16ii109.5 (9)Si02—O01—Si01153.2 (10)
O05—Si05—O04110.1 (8)Si03—O02—Si02151.5 (9)
O05—Si05—O21107.0 (7)Si03—O03—Si04172.2 (10)
O04—Si05—O21109.5 (8)Si04—O04—Si05156.8 (11)
O05—Si05—O14111.8 (8)Si05—O05—Si06148.5 (9)
O04—Si05—O14107.8 (9)Si02—O06—Si06159.5 (11)
O21—Si05—O14110.7 (7)Si08—O07—Si07153.9 (11)
O19—Si06—O06113.4 (8)Si08—O08—Si09153.0 (8)
O19—Si06—O18108.7 (10)Si10—O09—Si09153.9 (10)
O06—Si06—O18109.5 (7)Si11—O10—Si10157.4 (13)
O19—Si06—O05108.5 (7)Si12—O11—Si11155.3 (10)
O06—Si06—O05110.0 (8)Si08—O12—Si12167.0 (11)
O18—Si06—O05106.4 (7)Si08—O13—Si02174.5 (18)
O22i—Si07—O07107.1 (8)Si11—O14—Si05164.4 (11)
O22i—Si07—O17111.4 (7)Si10iii—O15—Si01148.2 (9)
O07—Si07—O17112.3 (8)Si04iii—O16—Si01165.9 (11)
O22i—Si07—O23106.4 (8)Si04iii—O17—Si07148.5 (10)
O07—Si07—O23112.3 (9)Si06—O18—Si09iii144.6 (9)
O17—Si07—O23107.3 (10)Si06—O19—Si03iii158.1 (10)
O13—Si08—O07111.2 (9)Si03iii—O20—Si12148.6 (12)
O13—Si08—O12107.2 (9)Si05—O21—Si01iv147.4 (10)
O07—Si08—O12113.6 (9)Si07iv—O22—Si11149.6 (10)
O13—Si08—O08106.9 (11)Si07—O23—Si07v152.3 (16)
O07—Si08—O08106.3 (8)Si12—O24—Si12v148.8 (16)
O12—Si08—O08111.4 (8)Si09v—O25—Si09150.5 (13)
O08—Si09—O09109.7 (7)Si10v—O26—Si10147.8 (14)
Symmetry codes: (i) x+1/2, y, z1/2; (ii) x+1/2, y, z+1/2; (iii) x+1/2, y, z1/2; (iv) x1/2, y, z1/2; (v) x, y1/2, z.
(dataset9) top
Crystal data top
O192Si96F(000) = 939
Mr = 5768.06Dx = 1.796 Mg m3
Orthorhombic, PnmaCell parameters from 10305 reflections
a = 20.022 (4) Åθ = 0.1–0.8°
b = 19.899 (4) ŵ = 0.000 mm1
c = 13.383 (3) ÅT = 293 K
V = 5332.0 (19) Å3Plate, white
Z = 1
Data collection top
JEOL JEM-2100
diffractometer
θmax = 0.8°, θmin = 0.1°
17621 measured reflectionsh = 1818
2925 independent reflectionsk = 2222
2172 reflections with I > 2σ(I)l = 1515
Rint = 0.206
Refinement top
Refinement on F248 restraints
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.2364P)2 + 6.090P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.233(Δ/σ)max = 0.030
wR(F2) = 0.557Δρmax = 0.64 e Å3
S = 1.18Δρmin = 0.20 e Å3
2925 reflectionsExtinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
150 parametersExtinction coefficient: 3079 (82)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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*/Ueq
Si010.4244 (5)0.0571 (3)0.3349 (6)0.025 (2)*
Si020.3099 (5)0.0289 (4)0.1885 (6)0.031 (2)*
Si030.2798 (6)0.0625 (3)0.0353 (6)0.026 (2)*
Si040.1217 (5)0.0639 (3)0.0295 (6)0.027 (2)*
Si050.0714 (5)0.0271 (3)0.1803 (5)0.0246 (19)*
Si060.1884 (5)0.0609 (3)0.3234 (6)0.025 (2)*
Si070.4227 (5)0.1732 (3)0.3210 (5)0.026 (2)*
Si080.3088 (5)0.1297 (3)0.1812 (6)0.028 (2)*
Si090.2752 (6)0.1728 (3)0.0347 (6)0.029 (2)*
Si100.1183 (5)0.1731 (3)0.0301 (5)0.0252 (19)*
Si110.0703 (5)0.1304 (3)0.1821 (6)0.029 (2)*
Si120.1889 (5)0.1730 (4)0.3157 (6)0.038 (2)*
O010.3753 (11)0.0566 (7)0.2411 (13)0.066 (5)*
O020.3090 (9)0.0591 (6)0.0752 (10)0.043 (4)*
O030.2003 (10)0.0604 (9)0.0307 (17)0.079 (6)*
O040.0934 (11)0.0641 (6)0.0809 (9)0.056 (4)*
O050.1171 (10)0.0531 (7)0.2711 (12)0.062 (5)*
O060.2431 (14)0.0608 (11)0.235 (2)0.119 (9)*
O070.3776 (9)0.1547 (8)0.2275 (11)0.063 (5)*
O080.3112 (9)0.1584 (6)0.0708 (9)0.042 (3)*
O090.1963 (8)0.1552 (7)0.0315 (12)0.051 (4)*
O100.0888 (15)0.1648 (10)0.0789 (12)0.094 (7)*
O110.1177 (8)0.1560 (7)0.2689 (12)0.063 (5)*
O120.2435 (9)0.1550 (8)0.2343 (14)0.078 (6)*
O130.3056 (12)0.0503 (5)0.1759 (14)0.062 (5)*
O140.0779 (11)0.0519 (6)0.1701 (11)0.051 (4)*
O150.4187 (12)0.1272 (7)0.3897 (12)0.064 (5)*
O160.4080 (10)0.0023 (6)0.4101 (10)0.050 (4)*
O170.4004 (10)0.1321 (6)0.4173 (10)0.043 (3)*
O180.1903 (9)0.1317 (6)0.3793 (10)0.041 (4)*
O190.1939 (9)0.0002 (6)0.4037 (10)0.041 (3)*
O200.1964 (9)0.1300 (6)0.4150 (9)0.045 (4)*
O210.0019 (9)0.0513 (7)0.2064 (12)0.057 (4)*
O220.0042 (9)0.1504 (7)0.2097 (13)0.065 (5)*
O230.4257 (15)0.2500000.3515 (15)0.048 (5)*
O240.1953 (15)0.2500000.3459 (18)0.059 (6)*
O250.2872 (12)0.2500000.0623 (13)0.032 (4)*
O260.1055 (13)0.2500000.0632 (13)0.036 (4)*
Geometric parameters (Å, º) top
Si01—O21i1.579 (18)Si07—O231.582 (9)
Si01—O151.581 (14)Si07—O22i1.586 (18)
Si01—O161.586 (11)Si07—O071.587 (12)
Si01—O011.596 (17)Si07—O171.591 (13)
Si02—O011.585 (18)Si08—O121.572 (12)
Si02—O131.586 (13)Si08—O131.583 (11)
Si02—O061.60 (2)Si08—O081.584 (14)
Si02—O021.631 (14)Si08—O071.593 (16)
Si03—O20ii1.574 (13)Si09—O18ii1.571 (14)
Si03—O19ii1.579 (13)Si09—O251.599 (9)
Si03—O021.593 (15)Si09—O081.611 (14)
Si03—O031.593 (19)Si09—O091.620 (17)
Si04—O031.575 (19)Si10—O101.583 (15)
Si04—O041.582 (14)Si10—O15ii1.593 (16)
Si04—O16ii1.585 (13)Si10—O091.600 (17)
Si04—O17ii1.595 (13)Si10—O261.613 (9)
Si05—O141.584 (13)Si11—O141.577 (13)
Si05—O041.584 (11)Si11—O101.585 (12)
Si05—O211.584 (18)Si11—O111.586 (15)
Si05—O051.607 (16)Si11—O221.586 (18)
Si06—O181.595 (13)Si12—O121.583 (12)
Si06—O051.597 (18)Si12—O201.588 (11)
Si06—O061.62 (2)Si12—O241.589 (10)
Si06—O191.622 (13)Si12—O111.593 (13)
O21i—Si01—O15107.0 (11)O18ii—Si09—O08110.7 (10)
O21i—Si01—O16111.2 (10)O25—Si09—O08107.8 (10)
O15—Si01—O16110.4 (9)O18ii—Si09—O09109.6 (10)
O21i—Si01—O01107.5 (11)O25—Si09—O09111.1 (11)
O15—Si01—O01109.0 (10)O08—Si09—O09112.0 (9)
O16—Si01—O01111.5 (10)O10—Si10—O15ii112.8 (13)
O01—Si02—O13115.9 (11)O10—Si10—O09110.5 (13)
O01—Si02—O06112.3 (16)O15ii—Si10—O09108.6 (11)
O13—Si02—O06112.9 (14)O10—Si10—O26107.0 (11)
O01—Si02—O02107.0 (10)O15ii—Si10—O26106.5 (10)
O13—Si02—O02105.5 (9)O09—Si10—O26111.3 (11)
O06—Si02—O02101.6 (13)O14—Si11—O10108.4 (11)
O20ii—Si03—O19ii110.8 (9)O14—Si11—O11109.6 (10)
O20ii—Si03—O02108.5 (9)O10—Si11—O11111.0 (13)
O19ii—Si03—O02108.9 (9)O14—Si11—O22111.3 (11)
O20ii—Si03—O03109.9 (10)O10—Si11—O22108.3 (13)
O19ii—Si03—O03109.4 (10)O11—Si11—O22108.2 (10)
O02—Si03—O03109.2 (12)O12—Si12—O20112.9 (11)
O03—Si04—O04111.6 (13)O12—Si12—O24109.8 (13)
O03—Si04—O16ii109.6 (11)O20—Si12—O24107.4 (11)
O04—Si04—O16ii110.1 (10)O12—Si12—O11107.4 (12)
O03—Si04—O17ii108.1 (11)O20—Si12—O11107.4 (10)
O04—Si04—O17ii108.4 (9)O24—Si12—O11112.1 (13)
O16ii—Si04—O17ii109.0 (9)Si02—O01—Si01149.4 (13)
O14—Si05—O04111.5 (9)Si03—O02—Si02152.0 (12)
O14—Si05—O21113.4 (10)Si04—O03—Si03175.7 (14)
O04—Si05—O21107.5 (11)Si04—O04—Si05152.0 (10)
O14—Si05—O05109.8 (10)Si06—O05—Si05150.6 (14)
O04—Si05—O05109.1 (11)Si02—O06—Si06148.0 (19)
O21—Si05—O05105.2 (10)Si07—O07—Si08150.8 (14)
O18—Si06—O05108.3 (9)Si08—O08—Si09150.1 (13)
O18—Si06—O06109.2 (12)Si10—O09—Si09154.7 (10)
O05—Si06—O06106.5 (15)Si10—O10—Si11159.4 (17)
O18—Si06—O19110.2 (8)Si11—O11—Si12153.2 (14)
O05—Si06—O19106.2 (9)Si08—O12—Si12163.3 (16)
O06—Si06—O19116.1 (12)Si08—O13—Si02169.8 (15)
O23—Si07—O22i107.9 (13)Si11—O14—Si05165.1 (14)
O23—Si07—O07116.7 (11)Si01—O15—Si10iii148.4 (15)
O22i—Si07—O07104.7 (11)Si04iii—O16—Si01167.9 (14)
O23—Si07—O17107.4 (9)Si07—O17—Si04iii151.3 (10)
O22i—Si07—O17108.8 (10)Si09iii—O18—Si06144.5 (11)
O07—Si07—O17111.1 (10)Si03iii—O19—Si06162.4 (13)
O12—Si08—O13107.9 (11)Si03iii—O20—Si12147.4 (11)
O12—Si08—O08109.4 (10)Si01iv—O21—Si05144.1 (12)
O13—Si08—O08108.7 (9)Si11—O22—Si07iv151.4 (13)
O12—Si08—O07116.3 (12)Si07—O23—Si07v149.8 (15)
O13—Si08—O07111.4 (11)Si12—O24—Si12v149.1 (18)
O08—Si08—O07102.9 (10)Si09v—O25—Si09148.0 (15)
O18ii—Si09—O25105.4 (9)Si10—O26—Si10v143.0 (14)
Symmetry codes: (i) x+1/2, y, z1/2; (ii) x+1/2, y, z+1/2; (iii) x+1/2, y, z1/2; (iv) x1/2, y, z1/2; (v) x, y1/2, z.
(dataset10) top
Crystal data top
O24Si12F(000) = 939
Mr = 721.01Dx = 1.796 Mg m3
Orthorhombic, PnmaCell parameters from 11450 reflections
a = 20.022 (4) Åθ = 0.1–0.8°
b = 19.899 (4) ŵ = 0.000 mm1
c = 13.383 (3) ÅT = 293 K
V = 5332.0 (19) Å3Plate, white
Z = 8
Data collection top
JEOL JEM-2100
diffractometer
θmax = 0.8°, θmin = 0.1°
19842 measured reflectionsh = 2323
3795 independent reflectionsk = 2222
2402 reflections with I > 2σ(I)l = 1414
Rint = 0.265
Refinement top
Refinement on F248 restraints
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.2396P)2 + 8.340P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.265(Δ/σ)max = 0.103
wR(F2) = 0.623Δρmax = 0.49 e Å3
S = 1.12Δρmin = 0.23 e Å3
3795 reflectionsExtinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
150 parametersExtinction coefficient: 9830 (75)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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*/Ueq
Si010.4235 (4)0.0597 (4)0.3339 (7)0.029 (2)*
Si020.3081 (4)0.0304 (5)0.1855 (8)0.046 (3)*
Si030.2794 (4)0.0622 (4)0.0349 (7)0.031 (2)*
Si040.1218 (4)0.0627 (4)0.0293 (7)0.030 (2)*
Si050.0735 (3)0.0283 (3)0.1830 (6)0.0216 (18)*
Si060.1873 (4)0.0570 (4)0.3275 (7)0.036 (2)*
Si070.4229 (4)0.1709 (4)0.3250 (7)0.041 (2)*
Si080.3104 (4)0.1301 (4)0.1814 (7)0.031 (2)*
Si090.2745 (4)0.1729 (4)0.0333 (7)0.031 (2)*
Si100.1199 (4)0.1738 (4)0.0300 (7)0.038 (2)*
Si110.0697 (4)0.1294 (4)0.1821 (7)0.033 (2)*
Si120.1888 (4)0.1739 (4)0.3160 (7)0.036 (2)*
O010.3742 (7)0.0560 (7)0.2407 (12)0.055 (4)*
O020.3097 (7)0.0599 (7)0.0751 (10)0.053 (4)*
O030.2010 (5)0.0583 (9)0.0291 (18)0.069 (5)*
O040.0947 (8)0.0641 (8)0.0811 (12)0.058 (4)*
O050.1155 (7)0.0537 (7)0.2754 (12)0.051 (4)*
O060.2452 (7)0.0548 (8)0.2470 (13)0.063 (5)*
O070.3776 (7)0.1556 (8)0.2312 (12)0.055 (4)*
O080.3096 (8)0.1592 (9)0.0703 (12)0.061 (4)*
O090.1970 (6)0.1573 (8)0.0199 (14)0.057 (4)*
O100.0870 (10)0.1633 (10)0.0773 (13)0.076 (5)*
O110.1193 (8)0.1590 (8)0.2647 (14)0.065 (5)*
O120.2424 (8)0.1503 (10)0.2355 (15)0.081 (6)*
O130.3086 (10)0.0505 (6)0.172 (2)0.077 (6)*
O140.0774 (9)0.0509 (7)0.1720 (16)0.063 (5)*
O150.4209 (7)0.1271 (6)0.3951 (12)0.056 (4)*
O160.4053 (8)0.0019 (7)0.4102 (14)0.061 (4)*
O170.4033 (8)0.1325 (6)0.4244 (11)0.057 (4)*
O180.1913 (7)0.1321 (6)0.3769 (12)0.041 (3)*
O190.1877 (7)0.0013 (7)0.4080 (12)0.056 (4)*
O200.1981 (8)0.1302 (7)0.4137 (13)0.059 (5)*
O210.0015 (6)0.0492 (7)0.2057 (13)0.051 (4)*
O220.0042 (6)0.1525 (8)0.2125 (14)0.060 (4)*
O230.4234 (11)0.2500000.349 (2)0.056 (6)*
O240.1893 (13)0.2500000.352 (2)0.075 (8)*
O250.2862 (10)0.2500000.0557 (17)0.042 (5)*
O260.1071 (10)0.2500000.0633 (17)0.045 (5)*
Geometric parameters (Å, º) top
Si01—O151.573 (11)Si07—O071.578 (16)
Si01—O161.581 (15)Si07—O171.583 (11)
Si01—O011.593 (12)Si07—O22i1.588 (12)
Si01—O21i1.607 (14)Si07—O231.607 (10)
Si02—O061.579 (11)Si08—O071.585 (15)
Si02—O021.590 (15)Si08—O131.588 (12)
Si02—O011.598 (14)Si08—O121.594 (11)
Si02—O131.620 (15)Si08—O081.596 (17)
Si03—O031.574 (10)Si09—O081.578 (16)
Si03—O19ii1.576 (11)Si09—O251.581 (9)
Si03—O20ii1.583 (11)Si09—O091.593 (11)
Si03—O021.593 (12)Si09—O18ii1.605 (15)
Si04—O041.575 (16)Si10—O091.582 (14)
Si04—O031.589 (8)Si10—O15ii1.592 (9)
Si04—O17ii1.600 (9)Si10—O101.595 (17)
Si04—O16ii1.613 (15)Si10—O261.601 (11)
Si05—O051.578 (15)Si11—O141.576 (14)
Si05—O141.584 (14)Si11—O101.594 (17)
Si05—O211.588 (11)Si11—O111.599 (16)
Si05—O041.596 (15)Si11—O221.600 (14)
Si06—O191.583 (11)Si12—O111.579 (16)
Si06—O061.584 (11)Si12—O201.581 (15)
Si06—O051.599 (15)Si12—O241.589 (13)
Si06—O181.636 (14)Si12—O121.591 (12)
O15—Si01—O16106.0 (11)O08—Si09—O09107.6 (10)
O15—Si01—O01115.3 (10)O25—Si09—O09110.8 (10)
O16—Si01—O01109.2 (10)O08—Si09—O18ii112.3 (9)
O15—Si01—O21i108.2 (9)O25—Si09—O18ii106.6 (10)
O16—Si01—O21i109.5 (9)O09—Si09—O18ii113.7 (9)
O01—Si01—O21i108.4 (10)O09—Si10—O15ii115.7 (10)
O06—Si02—O02112.8 (10)O09—Si10—O10107.4 (11)
O06—Si02—O01108.8 (11)O15ii—Si10—O10106.1 (11)
O02—Si02—O01107.2 (9)O09—Si10—O26112.1 (10)
O06—Si02—O13111.6 (11)O15ii—Si10—O26107.2 (10)
O02—Si02—O13105.3 (11)O10—Si10—O26108.0 (12)
O01—Si02—O13111.2 (10)O14—Si11—O10108.8 (11)
O03—Si03—O19ii113.7 (10)O14—Si11—O11111.3 (10)
O03—Si03—O20ii110.3 (10)O10—Si11—O11108.6 (11)
O19ii—Si03—O20ii109.2 (11)O14—Si11—O22113.3 (10)
O03—Si03—O02109.4 (11)O10—Si11—O22107.7 (11)
O19ii—Si03—O02105.5 (9)O11—Si11—O22107.0 (10)
O20ii—Si03—O02108.6 (10)O11—Si12—O20111.1 (10)
O04—Si04—O03110.0 (12)O11—Si12—O24108.4 (13)
O04—Si04—O17ii103.9 (9)O20—Si12—O24105.9 (13)
O03—Si04—O17ii111.2 (10)O11—Si12—O12104.2 (11)
O04—Si04—O16ii111.7 (10)O20—Si12—O12108.5 (11)
O03—Si04—O16ii107.0 (10)O24—Si12—O12118.7 (14)
O17ii—Si04—O16ii113.1 (11)Si01—O01—Si02152.8 (12)
O05—Si05—O14111.4 (10)Si02—O02—Si03149.5 (11)
O05—Si05—O21105.6 (9)Si03—O03—Si04173.3 (14)
O14—Si05—O21109.0 (9)Si04—O04—Si05152.3 (11)
O05—Si05—O04112.6 (9)Si05—O05—Si06146.4 (12)
O14—Si05—O04110.7 (10)Si02—O06—Si06161.1 (13)
O21—Si05—O04107.3 (10)Si07—O07—Si08152.1 (13)
O19—Si06—O06116.0 (10)Si09—O08—Si08152.4 (12)
O19—Si06—O05105.8 (9)Si10—O09—Si09154.2 (13)
O06—Si06—O05111.2 (11)Si11—O10—Si10159.7 (14)
O19—Si06—O18113.1 (10)Si12—O11—Si11156.5 (14)
O06—Si06—O18105.3 (9)Si12—O12—Si08163.4 (16)
O05—Si06—O18105.0 (8)Si08—O13—Si02169.3 (18)
O07—Si07—O17115.6 (10)Si11—O14—Si05166.8 (14)
O07—Si07—O22i103.5 (10)Si01—O15—Si10iii147.4 (11)
O17—Si07—O22i112.5 (11)Si01—O16—Si04iii169.0 (14)
O07—Si07—O23110.6 (12)Si07—O17—Si04iii145.2 (12)
O17—Si07—O23107.9 (11)Si09iii—O18—Si06141.9 (11)
O22i—Si07—O23106.4 (11)Si03iii—O19—Si06153.6 (12)
O07—Si08—O13111.7 (10)Si12—O20—Si03iii149.6 (13)
O07—Si08—O12116.9 (12)Si05—O21—Si01iv148.8 (13)
O13—Si08—O12105.5 (11)Si07iv—O22—Si11146.7 (14)
O07—Si08—O08106.5 (10)Si07—O23—Si07v156.9 (19)
O13—Si08—O08106.9 (12)Si12v—O24—Si12145 (2)
O12—Si08—O08108.9 (11)Si09v—O25—Si09152.1 (16)
O08—Si09—O25105.6 (11)Si10v—O26—Si10142.6 (17)
Symmetry codes: (i) x+1/2, y, z1/2; (ii) x+1/2, y, z+1/2; (iii) x+1/2, y, z1/2; (iv) x1/2, y, z1/2; (v) x, y1/2, z.
 

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