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
CCDC references: 1844586; 1844587; 1844588; 1844589; 1844590; 1844591; 1844592; 1844593; 1844594; 1844595
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.
Crystal data top
FFeO3Se | Z = 4 |
Mr = 201.80 | F(000) = 88 |
Monoclinic, P21/n | Dx = 4.359 Mg m−3 |
a = 4.956 (1) Å | Cell parameters from 640 reflections |
b = 5.202 (1) Å | θ = 0.1–0.9° |
c = 12.040 (2) Å | µ = 0.000 mm−1 |
β = 97.87 (3)° | T = 293 K |
V = 307.48 (11) Å3 | Plate, white |
Data collection top
JEOL JEM-2100 diffractometer | θmax = 0.9°, θmin = 0.1° |
1257 measured reflections | h = −6→6 |
462 independent reflections | k = −5→5 |
317 reflections with I > 2σ(I) | l = −15→15 |
Rint = 0.210 | |
Refinement top
Refinement on F2 | 0 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) = 0.368 | Δρmax = 0.35 e Å−3 |
S = 1.25 | Δρmin = −0.36 e Å−3 |
462 reflections | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
26 parameters | Extinction 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 | x | y | z | Uiso*/Ueq | |
Se1 | 0.5168 (9) | 0.3609 (11) | 0.3332 (3) | 0.0052 (13)* | |
Fe1 | 0.4583 (10) | 0.2562 (13) | 0.0724 (4) | 0.0052 (14)* | |
O1 | 0.337 (3) | 0.628 (4) | 0.3507 (11) | 0.013 (3)* | |
O2 | 0.806 (3) | 0.440 (3) | 0.4234 (10) | 0.007 (3)* | |
O3 | 0.623 (3) | 0.426 (3) | 0.2093 (9) | 0.006 (3)* | |
F1 | 0.270 (3) | 0.570 (3) | 0.0114 (10) | 0.009 (3)* | |
Geometric parameters (Å, º) top
Se1—O1 | 1.680 (18) | Fe1—O2iii | 2.014 (16) |
Se1—O3 | 1.682 (12) | Fe1—O2iv | 2.111 (15) |
Se1—O2 | 1.727 (14) | O1—Fe1v | 1.952 (16) |
Fe1—O3 | 1.947 (15) | O2—Fe1vi | 2.014 (16) |
Fe1—O1i | 1.952 (16) | O2—Fe1vii | 2.111 (15) |
Fe1—F1 | 1.970 (16) | F1—Fe1ii | 2.006 (14) |
Fe1—F1ii | 2.006 (14) | | |
| | | |
O1—Se1—O3 | 100.4 (7) | F1ii—Fe1—O2iii | 87.4 (6) |
O1—Se1—O2 | 97.8 (8) | O3—Fe1—O2iv | 176.0 (6) |
O3—Se1—O2 | 100.2 (7) | O1i—Fe1—O2iv | 92.0 (7) |
O3—Fe1—O1i | 90.4 (6) | F1—Fe1—O2iv | 89.3 (6) |
O3—Fe1—F1 | 93.6 (6) | F1ii—Fe1—O2iv | 88.6 (5) |
O1i—Fe1—F1 | 96.5 (7) | O2iii—Fe1—O2iv | 76.4 (6) |
O3—Fe1—F1ii | 89.4 (6) | Se1—O1—Fe1v | 142.0 (10) |
O1i—Fe1—F1ii | 172.3 (8) | Se1—O2—Fe1vi | 129.7 (8) |
F1—Fe1—F1ii | 75.8 (6) | Se1—O2—Fe1vii | 126.1 (8) |
O3—Fe1—O2iii | 100.1 (6) | Fe1vi—O2—Fe1vii | 103.6 (6) |
O1i—Fe1—O2iii | 100.2 (7) | Se1—O3—Fe1 | 120.9 (9) |
F1—Fe1—O2iii | 158.2 (5) | Fe1—F1—Fe1ii | 104.2 (6) |
Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) −x+1, −y+1, −z; (iii) −x+3/2, y−1/2, −z+1/2; (iv) x−1/2, −y+1/2, z−1/2; (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. |
Crystal data top
FFeO3Se | Z = 4 |
Mr = 201.80 | F(000) = 88 |
Monoclinic, P21/n | Dx = 4.359 Mg m−3 |
a = 4.956 (1) Å | Cell parameters from 714 reflections |
b = 5.202 (1) Å | θ = 0.2–0.9° |
c = 12.040 (2) Å | µ = 0.000 mm−1 |
β = 97.87 (3)° | T = 293 K |
V = 307.48 (11) Å3 | Plate, white |
Data collection top
JEOL JEM-2100 diffractometer | θmax = 0.9°, θmin = 0.2° |
1319 measured reflections | h = −6→6 |
487 independent reflections | k = −6→6 |
418 reflections with I > 2σ(I) | l = −13→13 |
Rint = 0.210 | |
Refinement top
Refinement on F2 | 0 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) = 0.471 | Δρmax = 0.39 e Å−3 |
S = 1.24 | Δρmin = −0.38 e Å−3 |
487 reflections | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
26 parameters | Extinction 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 | x | y | z | Uiso*/Ueq | |
Se1 | 0.5181 (11) | 0.3574 (13) | 0.3345 (6) | 0.0010 (17)* | |
Fe1 | 0.4575 (12) | 0.2581 (14) | 0.0722 (6) | 0.0020 (17)* | |
O1 | 0.329 (4) | 0.624 (4) | 0.3470 (19) | 0.011 (4)* | |
O2 | 0.807 (3) | 0.434 (4) | 0.4238 (18) | 0.009 (4)* | |
O3 | 0.616 (3) | 0.425 (4) | 0.2070 (17) | 0.006 (4)* | |
F1 | 0.271 (3) | 0.573 (4) | 0.0107 (17) | 0.006 (3)* | |
Geometric parameters (Å, º) top
Se1—O1 | 1.69 (2) | Fe1—O2iii | 2.05 (2) |
Se1—O3 | 1.71 (2) | Fe1—O2iv | 2.09 (2) |
Se1—O2 | 1.72 (2) | O1—Fe1v | 1.96 (2) |
Fe1—O3 | 1.91 (2) | O2—Fe1vi | 2.05 (2) |
Fe1—O1i | 1.96 (2) | O2—Fe1vii | 2.09 (2) |
Fe1—F1 | 1.976 (19) | F1—Fe1ii | 1.986 (19) |
Fe1—F1ii | 1.986 (19) | | |
| | | |
O1—Se1—O3 | 98.1 (11) | F1ii—Fe1—O2iii | 87.2 (8) |
O1—Se1—O2 | 100.2 (10) | O3—Fe1—O2iv | 176.5 (8) |
O3—Se1—O2 | 101.5 (9) | O1i—Fe1—O2iv | 93.2 (9) |
O3—Fe1—O1i | 88.9 (9) | F1—Fe1—O2iv | 89.0 (9) |
O3—Fe1—F1 | 93.4 (9) | F1ii—Fe1—O2iv | 88.2 (8) |
O1i—Fe1—F1 | 98.5 (8) | O2iii—Fe1—O2iv | 76.2 (9) |
O3—Fe1—F1ii | 89.9 (8) | Se1—O1—Fe1v | 141.7 (13) |
O1i—Fe1—F1ii | 174.4 (9) | Se1—O2—Fe1vi | 129.1 (12) |
F1—Fe1—F1ii | 76.1 (8) | Se1—O2—Fe1vii | 126.4 (12) |
O3—Fe1—O2iii | 100.8 (9) | Fe1vi—O2—Fe1vii | 103.8 (9) |
O1i—Fe1—O2iii | 98.4 (9) | Se1—O3—Fe1 | 122.4 (11) |
F1—Fe1—O2iii | 158.1 (10) | Fe1—F1—Fe1ii | 103.9 (8) |
Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) −x+1, −y+1, −z; (iii) −x+3/2, y−1/2, −z+1/2; (iv) x−1/2, −y+1/2, z−1/2; (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. |
Crystal data top
FFeO3Se | Z = 4 |
Mr = 201.80 | F(000) = 88 |
Monoclinic, P21/n | Dx = 4.359 Mg m−3 |
a = 4.956 (1) Å | Cell parameters from 725 reflections |
b = 5.202 (1) Å | θ = 0.2–0.9° |
c = 12.040 (2) Å | µ = 0.000 mm−1 |
β = 97.87 (3)° | T = 293 K |
V = 307.48 (11) Å3 | Plate, white |
Data collection top
JEOL JEM-2100 diffractometer | θmax = 0.9°, θmin = 0.2° |
1497 measured reflections | h = −6→6 |
495 independent reflections | k = −6→6 |
400 reflections with I > 2σ(I) | l = −12→12 |
Rint = 0.205 | |
Refinement top
Refinement on F2 | 0 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) = 0.393 | Δρmax = 0.36 e Å−3 |
S = 1.19 | Δρmin = −0.40 e Å−3 |
495 reflections | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
26 parameters | Extinction 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 | x | y | z | Uiso*/Ueq | |
Se1 | 0.5172 (10) | 0.3574 (9) | 0.3342 (6) | 0.0027 (13)* | |
Fe1 | 0.4566 (11) | 0.2557 (10) | 0.0721 (6) | 0.0072 (14)* | |
O1 | 0.327 (3) | 0.621 (3) | 0.3474 (19) | 0.015 (3)* | |
O2 | 0.809 (3) | 0.432 (2) | 0.4234 (18) | 0.010 (3)* | |
O3 | 0.620 (3) | 0.419 (2) | 0.2088 (17) | 0.008 (3)* | |
F1 | 0.268 (3) | 0.573 (2) | 0.0091 (17) | 0.011 (3)* | |
Geometric parameters (Å, º) top
Se1—O1 | 1.686 (16) | Fe1—O2iii | 2.042 (14) |
Se1—O3 | 1.69 (2) | Fe1—O2iv | 2.08 (2) |
Se1—O2 | 1.722 (17) | O1—Fe1v | 1.94 (2) |
Fe1—O3 | 1.929 (19) | O2—Fe1vi | 2.042 (14) |
Fe1—O1i | 1.94 (2) | O2—Fe1vii | 2.08 (2) |
Fe1—F1ii | 1.994 (17) | F1—Fe1ii | 1.994 (17) |
Fe1—F1 | 1.994 (15) | | |
| | | |
O1—Se1—O3 | 99.8 (9) | F1—Fe1—O2iii | 158.0 (9) |
O1—Se1—O2 | 100.9 (8) | O3—Fe1—O2iv | 175.8 (7) |
O3—Se1—O2 | 100.7 (9) | O1i—Fe1—O2iv | 93.8 (8) |
O3—Fe1—O1i | 88.9 (8) | F1ii—Fe1—O2iv | 88.4 (7) |
O3—Fe1—F1ii | 89.2 (7) | F1—Fe1—O2iv | 88.3 (7) |
O1i—Fe1—F1ii | 174.4 (6) | O2iii—Fe1—O2iv | 76.6 (8) |
O3—Fe1—F1 | 94.5 (7) | Se1—O1—Fe1v | 142.4 (12) |
O1i—Fe1—F1 | 98.9 (7) | Se1—O2—Fe1vi | 129.0 (10) |
F1ii—Fe1—F1 | 76.1 (7) | Se1—O2—Fe1vii | 126.6 (8) |
O3—Fe1—O2iii | 99.8 (7) | Fe1vi—O2—Fe1vii | 103.4 (8) |
O1i—Fe1—O2iii | 98.0 (7) | Se1—O3—Fe1 | 122.4 (8) |
F1ii—Fe1—O2iii | 87.5 (6) | Fe1ii—F1—Fe1 | 103.9 (7) |
Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) −x+1, −y+1, −z; (iii) −x+3/2, y−1/2, −z+1/2; (iv) x−1/2, −y+1/2, z−1/2; (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. |
Crystal data top
FFeO3Se | Z = 4 |
Mr = 201.80 | F(000) = 88 |
Monoclinic, P21/n | Dx = 4.359 Mg m−3 |
a = 4.956 (1) Å | Cell parameters from 643 reflections |
b = 5.202 (1) Å | θ = 0.2–0.9° |
c = 12.040 (2) Å | µ = 0.000 mm−1 |
β = 97.87 (3)° | T = 293 K |
V = 307.48 (11) Å3 | Plate, white |
Data collection top
JEOL JEM-2100 diffractometer | θmax = 0.9°, θmin = 0.2° |
1198 measured reflections | h = −6→6 |
460 independent reflections | k = −6→6 |
394 reflections with I > 2σ(I) | l = −12→13 |
Rint = 0.196 | |
Refinement top
Refinement on F2 | 0 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) = 0.447 | Δρmax = 0.40 e Å−3 |
S = 1.22 | Δρmin = −0.49 e Å−3 |
460 reflections | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
26 parameters | Extinction 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 | x | y | z | Uiso*/Ueq | |
Se1 | 0.5189 (10) | 0.3569 (13) | 0.3344 (6) | 0.0010 (16)* | |
Fe1 | 0.4581 (12) | 0.2558 (13) | 0.0726 (7) | 0.0031 (17)* | |
O1 | 0.329 (3) | 0.620 (4) | 0.3480 (18) | 0.007 (4)* | |
O2 | 0.810 (3) | 0.438 (4) | 0.427 (2) | 0.011 (4)* | |
O3 | 0.620 (3) | 0.424 (4) | 0.2102 (17) | 0.004 (4)* | |
F1 | 0.269 (3) | 0.568 (4) | 0.0159 (18) | 0.011 (4)* | |
Geometric parameters (Å, º) top
Se1—O3 | 1.68 (2) | Fe1—F1iii | 2.05 (2) |
Se1—O1 | 1.682 (19) | Fe1—O2iv | 2.06 (2) |
Se1—O2 | 1.75 (2) | O1—Fe1v | 1.951 (19) |
Fe1—O3 | 1.95 (2) | O2—Fe1vi | 2.02 (2) |
Fe1—F1 | 1.95 (2) | O2—Fe1vii | 2.06 (2) |
Fe1—O1i | 1.951 (19) | F1—Fe1iii | 2.05 (2) |
Fe1—O2ii | 2.02 (2) | | |
| | | |
O3—Se1—O1 | 99.0 (10) | O2ii—Fe1—F1iii | 87.1 (8) |
O3—Se1—O2 | 101.5 (9) | O3—Fe1—O2iv | 176.2 (8) |
O1—Se1—O2 | 99.5 (10) | F1—Fe1—O2iv | 90.6 (9) |
O3—Fe1—F1 | 92.6 (9) | O1i—Fe1—O2iv | 92.2 (8) |
O3—Fe1—O1i | 89.4 (8) | O2ii—Fe1—O2iv | 74.7 (9) |
F1—Fe1—O1i | 97.3 (8) | F1iii—Fe1—O2iv | 87.8 (8) |
O3—Fe1—O2ii | 101.6 (8) | Se1—O1—Fe1v | 142.9 (12) |
F1—Fe1—O2ii | 158.4 (10) | Se1—O2—Fe1vi | 128.1 (13) |
O1i—Fe1—O2ii | 99.1 (8) | Se1—O2—Fe1vii | 126.3 (12) |
O3—Fe1—F1iii | 90.9 (8) | Fe1vi—O2—Fe1vii | 105.3 (9) |
F1—Fe1—F1iii | 76.3 (8) | Se1—O3—Fe1 | 121.6 (10) |
O1i—Fe1—F1iii | 173.6 (8) | Fe1—F1—Fe1iii | 103.7 (8) |
Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) −x+3/2, y−1/2, −z+1/2; (iii) −x+1, −y+1, −z; (iv) x−1/2, −y+1/2, z−1/2; (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. |
Crystal data top
FFeO3Se | Z = 4 |
Mr = 201.80 | F(000) = 88 |
Monoclinic, P21/n | Dx = 4.359 Mg m−3 |
a = 4.956 (1) Å | Cell parameters from 769 reflections |
b = 5.202 (1) Å | θ = 0.1–0.9° |
c = 12.040 (2) Å | µ = 0.000 mm−1 |
β = 97.87 (3)° | T = 293 K |
V = 307.48 (11) Å3 | Plate, white |
Data collection top
JEOL JEM-2100 diffractometer | θmax = 0.9°, θmin = 0.1° |
1459 measured reflections | h = −6→6 |
582 independent reflections | k = −6→6 |
394 reflections with I > 2σ(I) | l = −15→15 |
Rint = 0.308 | |
Refinement top
Refinement on F2 | 4 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) = 0.532 | Δρmax = 0.51 e Å−3 |
S = 1.41 | Δρmin = −0.56 e Å−3 |
582 reflections | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
26 parameters | Extinction 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 | x | y | z | Uiso*/Ueq | |
Se1 | 0.5186 (14) | 0.3578 (10) | 0.3342 (4) | 0.0010 (17)* | |
Fe1 | 0.4581 (14) | 0.2575 (10) | 0.0731 (5) | 0.0010 (17)* | |
O1 | 0.324 (4) | 0.625 (3) | 0.3455 (13) | 0.002 (2)* | |
O2 | 0.796 (4) | 0.431 (3) | 0.4195 (13) | 0.002 (2)* | |
O3 | 0.620 (4) | 0.424 (3) | 0.2096 (13) | 0.002 (2)* | |
F1 | 0.271 (4) | 0.571 (3) | 0.0105 (13) | 0.003 (2)* | |
Geometric parameters (Å, º) top
Se1—O2 | 1.644 (17) | Fe1—O2iii | 2.085 (17) |
Se1—O3 | 1.681 (18) | Fe1—O2iv | 2.149 (16) |
Se1—O1 | 1.710 (16) | O1—Fe1v | 1.94 (2) |
Fe1—O3 | 1.932 (17) | O2—Fe1vi | 2.085 (17) |
Fe1—O1i | 1.94 (2) | O2—Fe1vii | 2.149 (16) |
Fe1—F1 | 1.975 (16) | F1—Fe1ii | 1.993 (17) |
Fe1—F1ii | 1.993 (18) | | |
| | | |
O2—Se1—O3 | 100.6 (10) | F1ii—Fe1—O2iii | 87.5 (7) |
O2—Se1—O1 | 101.2 (8) | O3—Fe1—O2iv | 177.4 (8) |
O3—Se1—O1 | 98.4 (8) | O1i—Fe1—O2iv | 93.6 (7) |
O3—Fe1—O1i | 88.4 (7) | F1—Fe1—O2iv | 87.0 (6) |
O3—Fe1—F1 | 94.2 (7) | F1ii—Fe1—O2iv | 88.1 (7) |
O1i—Fe1—F1 | 98.9 (7) | O2iii—Fe1—O2iv | 79.2 (7) |
O3—Fe1—F1ii | 90.0 (7) | Se1—O1—Fe1v | 141.6 (9) |
O1i—Fe1—F1ii | 174.1 (7) | Se1—O2—Fe1vi | 130.5 (9) |
F1—Fe1—F1ii | 75.5 (8) | Se1—O2—Fe1vii | 127.9 (9) |
O3—Fe1—O2iii | 99.0 (7) | Fe1vi—O2—Fe1vii | 100.8 (7) |
O1i—Fe1—O2iii | 98.4 (7) | Se1—O3—Fe1 | 121.9 (10) |
F1—Fe1—O2iii | 158.5 (8) | Fe1—F1—Fe1ii | 104.5 (8) |
Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) −x+1, −y+1, −z; (iii) −x+3/2, y−1/2, −z+1/2; (iv) x−1/2, −y+1/2, z−1/2; (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. |
Crystal data top
FFeO3Se | Z = 4 |
Mr = 201.80 | F(000) = 88 |
Monoclinic, P21/n | Dx = 4.359 Mg m−3 |
a = 4.956 (1) Å | Cell parameters from 590 reflections |
b = 5.202 (1) Å | θ = 0.2–0.9° |
c = 12.040 (2) Å | µ = 0.000 mm−1 |
β = 97.87 (3)° | T = 293 K |
V = 307.48 (11) Å3 | Plate, white |
Data collection top
JEOL JEM-2100 diffractometer | θmax = 0.9°, θmin = 0.2° |
1173 measured reflections | h = −6→6 |
498 independent reflections | k = −6→6 |
400 reflections with I > 2σ(I) | l = −12→13 |
Rint = 0.158 | |
Refinement top
Refinement on F2 | 0 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) = 0.386 | Δρmax = 0.33 e Å−3 |
S = 1.18 | Δρmin = −0.36 e Å−3 |
498 reflections | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
26 parameters | Extinction 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 | x | y | z | Uiso*/Ueq | |
Se1 | 0.5180 (8) | 0.3599 (7) | 0.3345 (5) | 0.0049 (12)* | |
Fe1 | 0.4595 (9) | 0.2557 (8) | 0.0717 (5) | 0.0091 (13)* | |
O1 | 0.332 (3) | 0.621 (2) | 0.3468 (16) | 0.017 (3)* | |
O2 | 0.809 (3) | 0.439 (2) | 0.4254 (15) | 0.013 (3)* | |
O3 | 0.617 (2) | 0.422 (2) | 0.2083 (14) | 0.010 (2)* | |
F1 | 0.268 (2) | 0.5717 (19) | 0.0096 (13) | 0.012 (2)* | |
Geometric parameters (Å, º) top
Se1—O1 | 1.660 (13) | Fe1—O2iii | 2.007 (12) |
Se1—O3 | 1.690 (16) | Fe1—O2iv | 2.079 (17) |
Se1—O2 | 1.735 (15) | O1—Fe1v | 1.983 (16) |
Fe1—O3 | 1.928 (16) | O2—Fe1vi | 2.007 (12) |
Fe1—O1i | 1.983 (16) | O2—Fe1vii | 2.079 (17) |
Fe1—F1ii | 1.986 (13) | F1—Fe1ii | 1.986 (13) |
Fe1—F1 | 1.991 (13) | | |
| | | |
O1—Se1—O3 | 99.0 (8) | F1—Fe1—O2iii | 157.9 (7) |
O1—Se1—O2 | 100.0 (7) | O3—Fe1—O2iv | 176.7 (5) |
O3—Se1—O2 | 101.8 (7) | O1i—Fe1—O2iv | 92.6 (6) |
O3—Fe1—O1i | 88.5 (7) | F1ii—Fe1—O2iv | 89.6 (6) |
O3—Fe1—F1ii | 89.7 (6) | F1—Fe1—O2iv | 89.2 (6) |
O1i—Fe1—F1ii | 173.6 (5) | O2iii—Fe1—O2iv | 75.7 (7) |
O3—Fe1—F1 | 93.7 (6) | Se1—O1—Fe1v | 141.7 (9) |
O1i—Fe1—F1 | 97.8 (6) | Se1—O2—Fe1vi | 129.0 (8) |
F1ii—Fe1—F1 | 76.2 (5) | Se1—O2—Fe1vii | 126.2 (7) |
O3—Fe1—O2iii | 101.0 (6) | Fe1vi—O2—Fe1vii | 104.3 (7) |
O1i—Fe1—O2iii | 99.0 (5) | Se1—O3—Fe1 | 123.2 (7) |
F1ii—Fe1—O2iii | 87.4 (5) | Fe1ii—F1—Fe1 | 103.8 (5) |
Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) −x+1, −y+1, −z; (iii) −x+3/2, y−1/2, −z+1/2; (iv) x−1/2, −y+1/2, z−1/2; (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. |
Crystal data top
O24Si12 | F(000) = 939 |
Mr = 721.01 | Dx = 1.796 Mg m−3 |
Orthorhombic, Pnma | Cell parameters from 8815 reflections |
a = 20.022 (4) Å | θ = 0.1–0.8° |
b = 19.899 (4) Å | µ = 0.000 mm−1 |
c = 13.383 (3) Å | T = 293 K |
V = 5332.0 (19) Å3 | Plate, white |
Z = 8 | |
Data collection top
JEOL JEM-2100 diffractometer | θmax = 0.8°, θmin = 0.1° |
16752 measured reflections | h = −23→23 |
3330 independent reflections | k = −20→20 |
1743 reflections with I > 2σ(I) | l = −13→13 |
Rint = 0.232 | |
Refinement top
Refinement on F2 | 48 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) = 0.508 | Δρmax = 0.35 e Å−3 |
S = 1.13 | Δρmin = −0.19 e Å−3 |
3330 reflections | Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
150 parameters | Extinction 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 | x | y | z | Uiso*/Ueq | |
Si01 | 0.4231 (2) | 0.0571 (3) | −0.3341 (5) | 0.0143 (16)* | |
Si02 | 0.3093 (2) | 0.0296 (4) | −0.1864 (6) | 0.0184 (17)* | |
Si03 | 0.2794 (2) | 0.0616 (3) | 0.0361 (5) | 0.0164 (17)* | |
Si04 | 0.1223 (2) | 0.0637 (3) | 0.0309 (5) | 0.0149 (16)* | |
Si05 | 0.0723 (2) | 0.0284 (3) | −0.1822 (5) | 0.0110 (16)* | |
Si06 | 0.1883 (2) | 0.0597 (3) | −0.3238 (6) | 0.0155 (16)* | |
Si07 | 0.4231 (2) | −0.1720 (3) | −0.3231 (5) | 0.0141 (16)* | |
Si08 | 0.3093 (2) | −0.1300 (4) | −0.1804 (6) | 0.0174 (17)* | |
Si09 | 0.2743 (2) | −0.1724 (3) | 0.0341 (5) | 0.0153 (17)* | |
Si10 | 0.1194 (3) | −0.1726 (4) | 0.0308 (6) | 0.0193 (17)* | |
Si11 | 0.0695 (2) | −0.1304 (3) | −0.1813 (5) | 0.0124 (16)* | |
Si12 | 0.1879 (3) | −0.1725 (4) | −0.3144 (6) | 0.0226 (18)* | |
O01 | 0.3743 (5) | 0.0552 (6) | −0.2407 (9) | 0.041 (3)* | |
O02 | 0.3081 (5) | 0.0586 (7) | −0.0747 (10) | 0.038 (3)* | |
O03 | 0.2008 (3) | 0.0578 (7) | 0.0292 (12) | 0.042 (3)* | |
O04 | 0.0951 (6) | 0.0627 (7) | −0.0807 (9) | 0.049 (3)* | |
O05 | 0.1164 (5) | 0.0550 (6) | −0.2712 (10) | 0.035 (3)* | |
O06 | 0.2455 (5) | 0.0556 (7) | −0.2433 (11) | 0.049 (3)* | |
O07 | 0.3753 (5) | −0.1570 (7) | −0.2303 (10) | 0.040 (3)* | |
O08 | 0.3093 (5) | −0.1554 (7) | −0.0690 (9) | 0.038 (3)* | |
O09 | 0.1966 (4) | −0.1542 (6) | 0.0242 (10) | 0.029 (3)* | |
O10 | 0.0863 (6) | −0.1634 (9) | −0.0769 (10) | 0.063 (4)* | |
O11 | 0.1179 (5) | −0.1591 (7) | −0.2645 (11) | 0.041 (3)* | |
O12 | 0.2441 (5) | −0.1542 (7) | −0.2363 (10) | 0.051 (4)* | |
O13 | 0.3072 (7) | −0.0509 (8) | −0.1751 (18) | 0.075 (5)* | |
O14 | 0.0788 (6) | −0.0512 (6) | −0.1717 (12) | 0.047 (3)* | |
O15 | 0.4160 (5) | 0.1276 (5) | −0.3879 (9) | 0.035 (3)* | |
O16 | 0.4083 (6) | −0.0019 (7) | −0.4109 (12) | 0.053 (4)* | |
O17 | 0.4009 (5) | −0.1323 (6) | −0.4196 (10) | 0.039 (3)* | |
O18 | 0.1915 (4) | 0.1301 (6) | −0.3790 (10) | 0.034 (3)* | |
O19 | 0.1926 (5) | 0.0024 (6) | −0.4060 (11) | 0.047 (3)* | |
O20 | 0.1977 (5) | −0.1304 (7) | −0.4129 (11) | 0.047 (3)* | |
O21 | −0.0030 (4) | 0.0489 (6) | −0.2077 (10) | 0.032 (3)* | |
O22 | −0.0038 (4) | −0.1516 (6) | −0.2109 (10) | 0.039 (3)* | |
O23 | 0.4236 (8) | −0.250000 | −0.3504 (17) | 0.046 (5)* | |
O24 | 0.1911 (6) | −0.250000 | −0.3473 (15) | 0.036 (4)* | |
O25 | 0.2853 (7) | −0.250000 | 0.0599 (14) | 0.032 (4)* | |
O26 | 0.1104 (6) | −0.250000 | 0.0615 (14) | 0.030 (4)* | |
Geometric parameters (Å, º) top
Si01—O15 | 1.582 (10) | Si07—O17 | 1.578 (13) |
Si01—O01 | 1.587 (10) | Si07—O22i | 1.585 (9) |
Si01—O16 | 1.588 (14) | Si07—O23 | 1.593 (8) |
Si01—O21i | 1.591 (10) | Si07—O07 | 1.597 (13) |
Si02—O06 | 1.574 (12) | Si08—O08 | 1.574 (14) |
Si02—O01 | 1.575 (11) | Si08—O07 | 1.575 (11) |
Si02—O02 | 1.602 (14) | Si08—O13 | 1.577 (16) |
Si02—O13 | 1.609 (16) | Si08—O12 | 1.580 (9) |
Si03—O03 | 1.577 (7) | Si09—O08 | 1.584 (13) |
Si03—O02 | 1.592 (14) | Si09—O18ii | 1.592 (12) |
Si03—O19ii | 1.592 (8) | Si09—O25 | 1.598 (8) |
Si03—O20ii | 1.597 (13) | Si09—O09 | 1.601 (9) |
Si04—O03 | 1.577 (7) | Si10—O15ii | 1.578 (10) |
Si04—O16ii | 1.579 (14) | Si10—O09 | 1.592 (9) |
Si04—O17ii | 1.587 (13) | Si10—O10 | 1.597 (13) |
Si04—O04 | 1.590 (13) | Si10—O26 | 1.604 (8) |
Si05—O05 | 1.574 (12) | Si11—O22 | 1.577 (9) |
Si05—O04 | 1.587 (11) | Si11—O10 | 1.580 (12) |
Si05—O14 | 1.597 (13) | Si11—O11 | 1.583 (12) |
Si05—O21 | 1.598 (10) | Si11—O14 | 1.593 (13) |
Si06—O06 | 1.575 (13) | Si12—O11 | 1.574 (11) |
Si06—O18 | 1.584 (13) | Si12—O20 | 1.575 (14) |
Si06—O19 | 1.587 (10) | Si12—O12 | 1.579 (10) |
Si06—O05 | 1.605 (10) | Si12—O24 | 1.605 (9) |
| | | |
O15—Si01—O01 | 109.0 (7) | O08—Si09—O25 | 109.5 (9) |
O15—Si01—O16 | 110.1 (9) | O18ii—Si09—O25 | 107.1 (9) |
O01—Si01—O16 | 112.2 (8) | O08—Si09—O09 | 108.0 (7) |
O15—Si01—O21i | 109.5 (6) | O18ii—Si09—O09 | 111.0 (7) |
O01—Si01—O21i | 107.1 (7) | O25—Si09—O09 | 111.8 (7) |
O16—Si01—O21i | 109.0 (7) | O15ii—Si10—O09 | 110.1 (7) |
O06—Si02—O01 | 109.9 (9) | O15ii—Si10—O10 | 111.8 (8) |
O06—Si02—O02 | 108.8 (8) | O09—Si10—O10 | 109.0 (8) |
O01—Si02—O02 | 109.0 (7) | O15ii—Si10—O26 | 108.6 (8) |
O06—Si02—O13 | 110.6 (9) | O09—Si10—O26 | 110.2 (7) |
O01—Si02—O13 | 112.7 (8) | O10—Si10—O26 | 107.1 (9) |
O02—Si02—O13 | 105.7 (11) | O22—Si11—O10 | 108.0 (8) |
O03—Si03—O02 | 107.7 (8) | O22—Si11—O11 | 107.3 (7) |
O03—Si03—O19ii | 110.0 (7) | O10—Si11—O11 | 109.9 (8) |
O02—Si03—O19ii | 107.2 (8) | O22—Si11—O14 | 113.2 (7) |
O03—Si03—O20ii | 110.7 (7) | O10—Si11—O14 | 108.3 (10) |
O02—Si03—O20ii | 109.1 (8) | O11—Si11—O14 | 110.0 (8) |
O19ii—Si03—O20ii | 112.1 (9) | O11—Si12—O20 | 112.1 (8) |
O03—Si04—O16ii | 109.6 (8) | O11—Si12—O12 | 108.3 (8) |
O03—Si04—O17ii | 111.2 (7) | O20—Si12—O12 | 110.0 (8) |
O16ii—Si04—O17ii | 110.5 (9) | O11—Si12—O24 | 108.3 (8) |
O03—Si04—O04 | 109.1 (8) | O20—Si12—O24 | 106.1 (10) |
O16ii—Si04—O04 | 108.7 (8) | O12—Si12—O24 | 112.1 (9) |
O17ii—Si04—O04 | 107.6 (8) | Si02—O01—Si01 | 151.6 (10) |
O05—Si05—O04 | 110.0 (8) | Si03—O02—Si02 | 152.6 (9) |
O05—Si05—O14 | 110.7 (8) | Si03—O03—Si04 | 171.9 (11) |
O04—Si05—O14 | 109.1 (9) | Si05—O04—Si04 | 155.2 (11) |
O05—Si05—O21 | 106.4 (7) | Si05—O05—Si06 | 148.8 (9) |
O04—Si05—O21 | 110.2 (7) | Si02—O06—Si06 | 159.8 (11) |
O14—Si05—O21 | 110.4 (7) | Si08—O07—Si07 | 153.8 (10) |
O06—Si06—O18 | 109.6 (7) | Si08—O08—Si09 | 153.3 (7) |
O06—Si06—O19 | 113.4 (8) | Si10—O09—Si09 | 152.4 (9) |
O18—Si06—O19 | 108.1 (9) | Si11—O10—Si10 | 159.1 (12) |
O06—Si06—O05 | 110.4 (8) | Si12—O11—Si11 | 154.8 (10) |
O18—Si06—O05 | 107.0 (6) | Si12—O12—Si08 | 166.6 (11) |
O19—Si06—O05 | 108.1 (7) | Si08—O13—Si02 | 171.5 (17) |
O17—Si07—O22i | 111.5 (7) | Si11—O14—Si05 | 164.9 (10) |
O17—Si07—O23 | 107.6 (10) | Si10iii—O15—Si01 | 149.0 (9) |
O22i—Si07—O23 | 108.1 (8) | Si04iii—O16—Si01 | 165.3 (10) |
O17—Si07—O07 | 111.9 (7) | Si07—O17—Si04iii | 148.8 (10) |
O22i—Si07—O07 | 106.3 (7) | Si06—O18—Si09iii | 145.7 (9) |
O23—Si07—O07 | 111.3 (9) | Si06—O19—Si03iii | 158.6 (9) |
O08—Si08—O07 | 107.0 (7) | Si12—O20—Si03iii | 148.2 (12) |
O08—Si08—O13 | 106.1 (11) | Si01iv—O21—Si05 | 145.9 (10) |
O07—Si08—O13 | 112.5 (8) | Si11—O22—Si07iv | 148.7 (10) |
O08—Si08—O12 | 110.5 (8) | Si07—O23—Si07v | 153.5 (16) |
O07—Si08—O12 | 112.9 (9) | Si12v—O24—Si12 | 147.8 (15) |
O13—Si08—O12 | 107.7 (9) | Si09—O25—Si09v | 150.2 (13) |
O08—Si09—O18ii | 109.4 (7) | Si10v—O26—Si10 | 147.6 (13) |
Symmetry codes: (i) x+1/2, y, −z−1/2; (ii) −x+1/2, −y, z+1/2; (iii) −x+1/2, −y, z−1/2; (iv) x−1/2, y, −z−1/2; (v) x, −y−1/2, z. |
Crystal data top
O24Si12 | F(000) = 939 |
Mr = 721.01 | Dx = 1.796 Mg m−3 |
Orthorhombic, Pnma | Cell parameters from 9808 reflections |
a = 20.022 (4) Å | θ = 0.1–0.8° |
b = 19.899 (4) Å | µ = 0.000 mm−1 |
c = 13.383 (3) Å | T = 293 K |
V = 5332.0 (19) Å3 | Plate, white |
Z = 8 | |
Data collection top
JEOL JEM-2100 diffractometer | θmax = 0.8°, θmin = 0.1° |
17564 measured reflections | h = −23→23 |
3390 independent reflections | k = −20→20 |
2082 reflections with I > 2σ(I) | l = −13→13 |
Rint = 0.191 | |
Refinement top
Refinement on F2 | 48 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) = 0.508 | Δρmax = 0.24 e Å−3 |
S = 1.13 | Δρmin = −0.16 e Å−3 |
3390 reflections | Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
150 parameters | Extinction 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 | x | y | z | Uiso*/Ueq | |
Si01 | 0.4231 (3) | 0.0574 (3) | −0.3355 (5) | 0.0222 (17)* | |
Si02 | 0.3088 (3) | 0.0294 (4) | −0.1883 (6) | 0.0274 (19)* | |
Si03 | 0.2797 (3) | 0.0616 (3) | 0.0353 (6) | 0.0246 (18)* | |
Si04 | 0.1226 (2) | 0.0639 (3) | 0.0287 (6) | 0.0219 (17)* | |
Si05 | 0.0725 (3) | 0.0285 (3) | −0.1836 (5) | 0.0188 (17)* | |
Si06 | 0.1875 (3) | 0.0598 (3) | −0.3265 (6) | 0.0216 (17)* | |
Si07 | 0.4228 (2) | −0.1718 (3) | −0.3245 (5) | 0.0211 (17)* | |
Si08 | 0.3085 (3) | −0.1299 (4) | −0.1834 (6) | 0.0265 (18)* | |
Si09 | 0.2746 (3) | −0.1724 (3) | 0.0319 (5) | 0.0231 (18)* | |
Si10 | 0.1198 (3) | −0.1723 (4) | 0.0300 (6) | 0.0266 (18)* | |
Si11 | 0.0692 (2) | −0.1301 (3) | −0.1819 (5) | 0.0210 (17)* | |
Si12 | 0.1871 (3) | −0.1729 (4) | −0.3167 (6) | 0.0294 (19)* | |
O01 | 0.3738 (5) | 0.0543 (7) | −0.2432 (10) | 0.050 (3)* | |
O02 | 0.3080 (5) | 0.0598 (7) | −0.0762 (10) | 0.047 (3)* | |
O03 | 0.2011 (3) | 0.0574 (7) | 0.0316 (13) | 0.048 (3)* | |
O04 | 0.0960 (6) | 0.0617 (7) | −0.0822 (10) | 0.058 (4)* | |
O05 | 0.1163 (5) | 0.0555 (6) | −0.2733 (10) | 0.043 (3)* | |
O06 | 0.2451 (5) | 0.0559 (7) | −0.2457 (10) | 0.057 (4)* | |
O07 | 0.3746 (5) | −0.1572 (7) | −0.2330 (11) | 0.053 (3)* | |
O08 | 0.3094 (5) | −0.1550 (7) | −0.0715 (10) | 0.046 (3)* | |
O09 | 0.1971 (4) | −0.1546 (7) | 0.0263 (11) | 0.042 (3)* | |
O10 | 0.0868 (7) | −0.1647 (9) | −0.0789 (11) | 0.080 (5)* | |
O11 | 0.1175 (5) | −0.1580 (7) | −0.2663 (10) | 0.051 (3)* | |
O12 | 0.2429 (5) | −0.1529 (7) | −0.2391 (10) | 0.056 (4)* | |
O13 | 0.3078 (7) | −0.0508 (8) | −0.1803 (18) | 0.082 (5)* | |
O14 | 0.0787 (6) | −0.0510 (6) | −0.1716 (13) | 0.058 (4)* | |
O15 | 0.4163 (5) | 0.1279 (6) | −0.3890 (10) | 0.045 (3)* | |
O16 | 0.4082 (6) | −0.0023 (8) | −0.4117 (13) | 0.064 (4)* | |
O17 | 0.4014 (5) | −0.1319 (6) | −0.4222 (9) | 0.047 (3)* | |
O18 | 0.1902 (5) | 0.1304 (7) | −0.3809 (11) | 0.045 (3)* | |
O19 | 0.1918 (5) | 0.0026 (6) | −0.4079 (12) | 0.056 (4)* | |
O20 | 0.1973 (6) | −0.1295 (7) | −0.4152 (11) | 0.057 (4)* | |
O21 | −0.0027 (5) | 0.0495 (6) | −0.2060 (10) | 0.040 (3)* | |
O22 | −0.0044 (4) | −0.1523 (6) | −0.2096 (11) | 0.047 (3)* | |
O23 | 0.4250 (8) | −0.250000 | −0.3529 (17) | 0.053 (5)* | |
O24 | 0.1908 (7) | −0.250000 | −0.3482 (17) | 0.050 (5)* | |
O25 | 0.2851 (7) | −0.250000 | 0.0579 (14) | 0.039 (4)* | |
O26 | 0.1101 (7) | −0.250000 | 0.0600 (15) | 0.044 (4)* | |
Geometric parameters (Å, º) top
Si01—O01 | 1.582 (11) | Si07—O22i | 1.577 (9) |
Si01—O15 | 1.583 (13) | Si07—O07 | 1.586 (13) |
Si01—O21i | 1.593 (11) | Si07—O17 | 1.588 (11) |
Si01—O16 | 1.594 (15) | Si07—O23 | 1.602 (8) |
Si02—O01 | 1.575 (11) | Si08—O13 | 1.575 (16) |
Si02—O06 | 1.579 (10) | Si08—O07 | 1.576 (12) |
Si02—O13 | 1.599 (16) | Si08—O12 | 1.577 (9) |
Si02—O02 | 1.618 (15) | Si08—O08 | 1.580 (14) |
Si03—O20ii | 1.574 (13) | Si09—O08 | 1.587 (13) |
Si03—O03 | 1.577 (7) | Si09—O09 | 1.594 (10) |
Si03—O19ii | 1.593 (9) | Si09—O25 | 1.596 (8) |
Si03—O02 | 1.596 (14) | Si09—O18ii | 1.599 (13) |
Si04—O04 | 1.577 (13) | Si10—O15ii | 1.574 (13) |
Si04—O03 | 1.578 (7) | Si10—O09 | 1.588 (10) |
Si04—O17ii | 1.580 (12) | Si10—O10 | 1.608 (14) |
Si04—O16ii | 1.587 (14) | Si10—O26 | 1.608 (9) |
Si05—O05 | 1.581 (13) | Si11—O10 | 1.581 (12) |
Si05—O04 | 1.581 (11) | Si11—O22 | 1.582 (9) |
Si05—O21 | 1.591 (10) | Si11—O11 | 1.587 (10) |
Si05—O14 | 1.594 (14) | Si11—O14 | 1.592 (14) |
Si06—O19 | 1.577 (12) | Si12—O11 | 1.577 (9) |
Si06—O06 | 1.582 (10) | Si12—O12 | 1.578 (10) |
Si06—O18 | 1.582 (13) | Si12—O20 | 1.589 (11) |
Si06—O05 | 1.597 (11) | Si12—O24 | 1.592 (9) |
| | | |
O01—Si01—O15 | 109.5 (7) | O08—Si09—O25 | 110.1 (9) |
O01—Si01—O21i | 107.9 (8) | O09—Si09—O25 | 110.7 (8) |
O15—Si01—O21i | 109.0 (7) | O08—Si09—O18ii | 109.2 (8) |
O01—Si01—O16 | 110.7 (8) | O09—Si09—O18ii | 110.2 (7) |
O15—Si01—O16 | 110.8 (10) | O25—Si09—O18ii | 106.8 (9) |
O21i—Si01—O16 | 108.9 (7) | O15ii—Si10—O09 | 110.2 (8) |
O01—Si02—O06 | 109.6 (9) | O15ii—Si10—O10 | 112.5 (9) |
O01—Si02—O13 | 110.8 (9) | O09—Si10—O10 | 110.6 (8) |
O06—Si02—O13 | 110.9 (9) | O15ii—Si10—O26 | 108.2 (9) |
O01—Si02—O02 | 108.8 (7) | O09—Si10—O26 | 109.8 (8) |
O06—Si02—O02 | 108.5 (8) | O10—Si10—O26 | 105.5 (10) |
O13—Si02—O02 | 108.1 (11) | O10—Si11—O22 | 106.8 (8) |
O20ii—Si03—O03 | 110.5 (8) | O10—Si11—O11 | 109.4 (9) |
O20ii—Si03—O19ii | 112.6 (9) | O22—Si11—O11 | 107.6 (8) |
O03—Si03—O19ii | 109.2 (7) | O10—Si11—O14 | 109.2 (10) |
O20ii—Si03—O02 | 108.1 (8) | O22—Si11—O14 | 114.1 (7) |
O03—Si03—O02 | 108.9 (8) | O11—Si11—O14 | 109.6 (8) |
O19ii—Si03—O02 | 107.5 (8) | O11—Si12—O12 | 107.3 (8) |
O04—Si04—O03 | 111.0 (9) | O11—Si12—O20 | 111.5 (8) |
O04—Si04—O17ii | 108.2 (8) | O12—Si12—O20 | 108.5 (8) |
O03—Si04—O17ii | 111.3 (7) | O11—Si12—O24 | 109.6 (8) |
O04—Si04—O16ii | 108.7 (9) | O12—Si12—O24 | 112.6 (9) |
O03—Si04—O16ii | 108.2 (8) | O20—Si12—O24 | 107.3 (11) |
O17ii—Si04—O16ii | 109.5 (9) | Si02—O01—Si01 | 153.2 (10) |
O05—Si05—O04 | 110.1 (8) | Si03—O02—Si02 | 151.5 (9) |
O05—Si05—O21 | 107.0 (7) | Si03—O03—Si04 | 172.2 (10) |
O04—Si05—O21 | 109.5 (8) | Si04—O04—Si05 | 156.8 (11) |
O05—Si05—O14 | 111.8 (8) | Si05—O05—Si06 | 148.5 (9) |
O04—Si05—O14 | 107.8 (9) | Si02—O06—Si06 | 159.5 (11) |
O21—Si05—O14 | 110.7 (7) | Si08—O07—Si07 | 153.9 (11) |
O19—Si06—O06 | 113.4 (8) | Si08—O08—Si09 | 153.0 (8) |
O19—Si06—O18 | 108.7 (10) | Si10—O09—Si09 | 153.9 (10) |
O06—Si06—O18 | 109.5 (7) | Si11—O10—Si10 | 157.4 (13) |
O19—Si06—O05 | 108.5 (7) | Si12—O11—Si11 | 155.3 (10) |
O06—Si06—O05 | 110.0 (8) | Si08—O12—Si12 | 167.0 (11) |
O18—Si06—O05 | 106.4 (7) | Si08—O13—Si02 | 174.5 (18) |
O22i—Si07—O07 | 107.1 (8) | Si11—O14—Si05 | 164.4 (11) |
O22i—Si07—O17 | 111.4 (7) | Si10iii—O15—Si01 | 148.2 (9) |
O07—Si07—O17 | 112.3 (8) | Si04iii—O16—Si01 | 165.9 (11) |
O22i—Si07—O23 | 106.4 (8) | Si04iii—O17—Si07 | 148.5 (10) |
O07—Si07—O23 | 112.3 (9) | Si06—O18—Si09iii | 144.6 (9) |
O17—Si07—O23 | 107.3 (10) | Si06—O19—Si03iii | 158.1 (10) |
O13—Si08—O07 | 111.2 (9) | Si03iii—O20—Si12 | 148.6 (12) |
O13—Si08—O12 | 107.2 (9) | Si05—O21—Si01iv | 147.4 (10) |
O07—Si08—O12 | 113.6 (9) | Si07iv—O22—Si11 | 149.6 (10) |
O13—Si08—O08 | 106.9 (11) | Si07—O23—Si07v | 152.3 (16) |
O07—Si08—O08 | 106.3 (8) | Si12—O24—Si12v | 148.8 (16) |
O12—Si08—O08 | 111.4 (8) | Si09v—O25—Si09 | 150.5 (13) |
O08—Si09—O09 | 109.7 (7) | Si10v—O26—Si10 | 147.8 (14) |
Symmetry codes: (i) x+1/2, y, −z−1/2; (ii) −x+1/2, −y, z+1/2; (iii) −x+1/2, −y, z−1/2; (iv) x−1/2, y, −z−1/2; (v) x, −y−1/2, z. |
Crystal data top
O192Si96 | F(000) = 939 |
Mr = 5768.06 | Dx = 1.796 Mg m−3 |
Orthorhombic, Pnma | Cell parameters from 10305 reflections |
a = 20.022 (4) Å | θ = 0.1–0.8° |
b = 19.899 (4) Å | µ = 0.000 mm−1 |
c = 13.383 (3) Å | T = 293 K |
V = 5332.0 (19) Å3 | Plate, white |
Z = 1 | |
Data collection top
JEOL JEM-2100 diffractometer | θmax = 0.8°, θmin = 0.1° |
17621 measured reflections | h = −18→18 |
2925 independent reflections | k = −22→22 |
2172 reflections with I > 2σ(I) | l = −15→15 |
Rint = 0.206 | |
Refinement top
Refinement on F2 | 48 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) = 0.557 | Δρmax = 0.64 e Å−3 |
S = 1.18 | Δρmin = −0.20 e Å−3 |
2925 reflections | Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
150 parameters | Extinction 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 | x | y | z | Uiso*/Ueq | |
Si01 | 0.4244 (5) | 0.0571 (3) | −0.3349 (6) | 0.025 (2)* | |
Si02 | 0.3099 (5) | 0.0289 (4) | −0.1885 (6) | 0.031 (2)* | |
Si03 | 0.2798 (6) | 0.0625 (3) | 0.0353 (6) | 0.026 (2)* | |
Si04 | 0.1217 (5) | 0.0639 (3) | 0.0295 (6) | 0.027 (2)* | |
Si05 | 0.0714 (5) | 0.0271 (3) | −0.1803 (5) | 0.0246 (19)* | |
Si06 | 0.1884 (5) | 0.0609 (3) | −0.3234 (6) | 0.025 (2)* | |
Si07 | 0.4227 (5) | −0.1732 (3) | −0.3210 (5) | 0.026 (2)* | |
Si08 | 0.3088 (5) | −0.1297 (3) | −0.1812 (6) | 0.028 (2)* | |
Si09 | 0.2752 (6) | −0.1728 (3) | 0.0347 (6) | 0.029 (2)* | |
Si10 | 0.1183 (5) | −0.1731 (3) | 0.0301 (5) | 0.0252 (19)* | |
Si11 | 0.0703 (5) | −0.1304 (3) | −0.1821 (6) | 0.029 (2)* | |
Si12 | 0.1889 (5) | −0.1730 (4) | −0.3157 (6) | 0.038 (2)* | |
O01 | 0.3753 (11) | 0.0566 (7) | −0.2411 (13) | 0.066 (5)* | |
O02 | 0.3090 (9) | 0.0591 (6) | −0.0752 (10) | 0.043 (4)* | |
O03 | 0.2003 (10) | 0.0604 (9) | 0.0307 (17) | 0.079 (6)* | |
O04 | 0.0934 (11) | 0.0641 (6) | −0.0809 (9) | 0.056 (4)* | |
O05 | 0.1171 (10) | 0.0531 (7) | −0.2711 (12) | 0.062 (5)* | |
O06 | 0.2431 (14) | 0.0608 (11) | −0.235 (2) | 0.119 (9)* | |
O07 | 0.3776 (9) | −0.1547 (8) | −0.2275 (11) | 0.063 (5)* | |
O08 | 0.3112 (9) | −0.1584 (6) | −0.0708 (9) | 0.042 (3)* | |
O09 | 0.1963 (8) | −0.1552 (7) | 0.0315 (12) | 0.051 (4)* | |
O10 | 0.0888 (15) | −0.1648 (10) | −0.0789 (12) | 0.094 (7)* | |
O11 | 0.1177 (8) | −0.1560 (7) | −0.2689 (12) | 0.063 (5)* | |
O12 | 0.2435 (9) | −0.1550 (8) | −0.2343 (14) | 0.078 (6)* | |
O13 | 0.3056 (12) | −0.0503 (5) | −0.1759 (14) | 0.062 (5)* | |
O14 | 0.0779 (11) | −0.0519 (6) | −0.1701 (11) | 0.051 (4)* | |
O15 | 0.4187 (12) | 0.1272 (7) | −0.3897 (12) | 0.064 (5)* | |
O16 | 0.4080 (10) | −0.0023 (6) | −0.4101 (10) | 0.050 (4)* | |
O17 | 0.4004 (10) | −0.1321 (6) | −0.4173 (10) | 0.043 (3)* | |
O18 | 0.1903 (9) | 0.1317 (6) | −0.3793 (10) | 0.041 (4)* | |
O19 | 0.1939 (9) | 0.0002 (6) | −0.4037 (10) | 0.041 (3)* | |
O20 | 0.1964 (9) | −0.1300 (6) | −0.4150 (9) | 0.045 (4)* | |
O21 | −0.0019 (9) | 0.0513 (7) | −0.2064 (12) | 0.057 (4)* | |
O22 | −0.0042 (9) | −0.1504 (7) | −0.2097 (13) | 0.065 (5)* | |
O23 | 0.4257 (15) | −0.250000 | −0.3515 (15) | 0.048 (5)* | |
O24 | 0.1953 (15) | −0.250000 | −0.3459 (18) | 0.059 (6)* | |
O25 | 0.2872 (12) | −0.250000 | 0.0623 (13) | 0.032 (4)* | |
O26 | 0.1055 (13) | −0.250000 | 0.0632 (13) | 0.036 (4)* | |
Geometric parameters (Å, º) top
Si01—O21i | 1.579 (18) | Si07—O23 | 1.582 (9) |
Si01—O15 | 1.581 (14) | Si07—O22i | 1.586 (18) |
Si01—O16 | 1.586 (11) | Si07—O07 | 1.587 (12) |
Si01—O01 | 1.596 (17) | Si07—O17 | 1.591 (13) |
Si02—O01 | 1.585 (18) | Si08—O12 | 1.572 (12) |
Si02—O13 | 1.586 (13) | Si08—O13 | 1.583 (11) |
Si02—O06 | 1.60 (2) | Si08—O08 | 1.584 (14) |
Si02—O02 | 1.631 (14) | Si08—O07 | 1.593 (16) |
Si03—O20ii | 1.574 (13) | Si09—O18ii | 1.571 (14) |
Si03—O19ii | 1.579 (13) | Si09—O25 | 1.599 (9) |
Si03—O02 | 1.593 (15) | Si09—O08 | 1.611 (14) |
Si03—O03 | 1.593 (19) | Si09—O09 | 1.620 (17) |
Si04—O03 | 1.575 (19) | Si10—O10 | 1.583 (15) |
Si04—O04 | 1.582 (14) | Si10—O15ii | 1.593 (16) |
Si04—O16ii | 1.585 (13) | Si10—O09 | 1.600 (17) |
Si04—O17ii | 1.595 (13) | Si10—O26 | 1.613 (9) |
Si05—O14 | 1.584 (13) | Si11—O14 | 1.577 (13) |
Si05—O04 | 1.584 (11) | Si11—O10 | 1.585 (12) |
Si05—O21 | 1.584 (18) | Si11—O11 | 1.586 (15) |
Si05—O05 | 1.607 (16) | Si11—O22 | 1.586 (18) |
Si06—O18 | 1.595 (13) | Si12—O12 | 1.583 (12) |
Si06—O05 | 1.597 (18) | Si12—O20 | 1.588 (11) |
Si06—O06 | 1.62 (2) | Si12—O24 | 1.589 (10) |
Si06—O19 | 1.622 (13) | Si12—O11 | 1.593 (13) |
| | | |
O21i—Si01—O15 | 107.0 (11) | O18ii—Si09—O08 | 110.7 (10) |
O21i—Si01—O16 | 111.2 (10) | O25—Si09—O08 | 107.8 (10) |
O15—Si01—O16 | 110.4 (9) | O18ii—Si09—O09 | 109.6 (10) |
O21i—Si01—O01 | 107.5 (11) | O25—Si09—O09 | 111.1 (11) |
O15—Si01—O01 | 109.0 (10) | O08—Si09—O09 | 112.0 (9) |
O16—Si01—O01 | 111.5 (10) | O10—Si10—O15ii | 112.8 (13) |
O01—Si02—O13 | 115.9 (11) | O10—Si10—O09 | 110.5 (13) |
O01—Si02—O06 | 112.3 (16) | O15ii—Si10—O09 | 108.6 (11) |
O13—Si02—O06 | 112.9 (14) | O10—Si10—O26 | 107.0 (11) |
O01—Si02—O02 | 107.0 (10) | O15ii—Si10—O26 | 106.5 (10) |
O13—Si02—O02 | 105.5 (9) | O09—Si10—O26 | 111.3 (11) |
O06—Si02—O02 | 101.6 (13) | O14—Si11—O10 | 108.4 (11) |
O20ii—Si03—O19ii | 110.8 (9) | O14—Si11—O11 | 109.6 (10) |
O20ii—Si03—O02 | 108.5 (9) | O10—Si11—O11 | 111.0 (13) |
O19ii—Si03—O02 | 108.9 (9) | O14—Si11—O22 | 111.3 (11) |
O20ii—Si03—O03 | 109.9 (10) | O10—Si11—O22 | 108.3 (13) |
O19ii—Si03—O03 | 109.4 (10) | O11—Si11—O22 | 108.2 (10) |
O02—Si03—O03 | 109.2 (12) | O12—Si12—O20 | 112.9 (11) |
O03—Si04—O04 | 111.6 (13) | O12—Si12—O24 | 109.8 (13) |
O03—Si04—O16ii | 109.6 (11) | O20—Si12—O24 | 107.4 (11) |
O04—Si04—O16ii | 110.1 (10) | O12—Si12—O11 | 107.4 (12) |
O03—Si04—O17ii | 108.1 (11) | O20—Si12—O11 | 107.4 (10) |
O04—Si04—O17ii | 108.4 (9) | O24—Si12—O11 | 112.1 (13) |
O16ii—Si04—O17ii | 109.0 (9) | Si02—O01—Si01 | 149.4 (13) |
O14—Si05—O04 | 111.5 (9) | Si03—O02—Si02 | 152.0 (12) |
O14—Si05—O21 | 113.4 (10) | Si04—O03—Si03 | 175.7 (14) |
O04—Si05—O21 | 107.5 (11) | Si04—O04—Si05 | 152.0 (10) |
O14—Si05—O05 | 109.8 (10) | Si06—O05—Si05 | 150.6 (14) |
O04—Si05—O05 | 109.1 (11) | Si02—O06—Si06 | 148.0 (19) |
O21—Si05—O05 | 105.2 (10) | Si07—O07—Si08 | 150.8 (14) |
O18—Si06—O05 | 108.3 (9) | Si08—O08—Si09 | 150.1 (13) |
O18—Si06—O06 | 109.2 (12) | Si10—O09—Si09 | 154.7 (10) |
O05—Si06—O06 | 106.5 (15) | Si10—O10—Si11 | 159.4 (17) |
O18—Si06—O19 | 110.2 (8) | Si11—O11—Si12 | 153.2 (14) |
O05—Si06—O19 | 106.2 (9) | Si08—O12—Si12 | 163.3 (16) |
O06—Si06—O19 | 116.1 (12) | Si08—O13—Si02 | 169.8 (15) |
O23—Si07—O22i | 107.9 (13) | Si11—O14—Si05 | 165.1 (14) |
O23—Si07—O07 | 116.7 (11) | Si01—O15—Si10iii | 148.4 (15) |
O22i—Si07—O07 | 104.7 (11) | Si04iii—O16—Si01 | 167.9 (14) |
O23—Si07—O17 | 107.4 (9) | Si07—O17—Si04iii | 151.3 (10) |
O22i—Si07—O17 | 108.8 (10) | Si09iii—O18—Si06 | 144.5 (11) |
O07—Si07—O17 | 111.1 (10) | Si03iii—O19—Si06 | 162.4 (13) |
O12—Si08—O13 | 107.9 (11) | Si03iii—O20—Si12 | 147.4 (11) |
O12—Si08—O08 | 109.4 (10) | Si01iv—O21—Si05 | 144.1 (12) |
O13—Si08—O08 | 108.7 (9) | Si11—O22—Si07iv | 151.4 (13) |
O12—Si08—O07 | 116.3 (12) | Si07—O23—Si07v | 149.8 (15) |
O13—Si08—O07 | 111.4 (11) | Si12—O24—Si12v | 149.1 (18) |
O08—Si08—O07 | 102.9 (10) | Si09v—O25—Si09 | 148.0 (15) |
O18ii—Si09—O25 | 105.4 (9) | Si10—O26—Si10v | 143.0 (14) |
Symmetry codes: (i) x+1/2, y, −z−1/2; (ii) −x+1/2, −y, z+1/2; (iii) −x+1/2, −y, z−1/2; (iv) x−1/2, y, −z−1/2; (v) x, −y−1/2, z. |
Crystal data top
O24Si12 | F(000) = 939 |
Mr = 721.01 | Dx = 1.796 Mg m−3 |
Orthorhombic, Pnma | Cell parameters from 11450 reflections |
a = 20.022 (4) Å | θ = 0.1–0.8° |
b = 19.899 (4) Å | µ = 0.000 mm−1 |
c = 13.383 (3) Å | T = 293 K |
V = 5332.0 (19) Å3 | Plate, white |
Z = 8 | |
Data collection top
JEOL JEM-2100 diffractometer | θmax = 0.8°, θmin = 0.1° |
19842 measured reflections | h = −23→23 |
3795 independent reflections | k = −22→22 |
2402 reflections with I > 2σ(I) | l = −14→14 |
Rint = 0.265 | |
Refinement top
Refinement on F2 | 48 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) = 0.623 | Δρmax = 0.49 e Å−3 |
S = 1.12 | Δρmin = −0.23 e Å−3 |
3795 reflections | Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
150 parameters | Extinction 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 | x | y | z | Uiso*/Ueq | |
Si01 | 0.4235 (4) | 0.0597 (4) | −0.3339 (7) | 0.029 (2)* | |
Si02 | 0.3081 (4) | 0.0304 (5) | −0.1855 (8) | 0.046 (3)* | |
Si03 | 0.2794 (4) | 0.0622 (4) | 0.0349 (7) | 0.031 (2)* | |
Si04 | 0.1218 (4) | 0.0627 (4) | 0.0293 (7) | 0.030 (2)* | |
Si05 | 0.0735 (3) | 0.0283 (3) | −0.1830 (6) | 0.0216 (18)* | |
Si06 | 0.1873 (4) | 0.0570 (4) | −0.3275 (7) | 0.036 (2)* | |
Si07 | 0.4229 (4) | −0.1709 (4) | −0.3250 (7) | 0.041 (2)* | |
Si08 | 0.3104 (4) | −0.1301 (4) | −0.1814 (7) | 0.031 (2)* | |
Si09 | 0.2745 (4) | −0.1729 (4) | 0.0333 (7) | 0.031 (2)* | |
Si10 | 0.1199 (4) | −0.1738 (4) | 0.0300 (7) | 0.038 (2)* | |
Si11 | 0.0697 (4) | −0.1294 (4) | −0.1821 (7) | 0.033 (2)* | |
Si12 | 0.1888 (4) | −0.1739 (4) | −0.3160 (7) | 0.036 (2)* | |
O01 | 0.3742 (7) | 0.0560 (7) | −0.2407 (12) | 0.055 (4)* | |
O02 | 0.3097 (7) | 0.0599 (7) | −0.0751 (10) | 0.053 (4)* | |
O03 | 0.2010 (5) | 0.0583 (9) | 0.0291 (18) | 0.069 (5)* | |
O04 | 0.0947 (8) | 0.0641 (8) | −0.0811 (12) | 0.058 (4)* | |
O05 | 0.1155 (7) | 0.0537 (7) | −0.2754 (12) | 0.051 (4)* | |
O06 | 0.2452 (7) | 0.0548 (8) | −0.2470 (13) | 0.063 (5)* | |
O07 | 0.3776 (7) | −0.1556 (8) | −0.2312 (12) | 0.055 (4)* | |
O08 | 0.3096 (8) | −0.1592 (9) | −0.0703 (12) | 0.061 (4)* | |
O09 | 0.1970 (6) | −0.1573 (8) | 0.0199 (14) | 0.057 (4)* | |
O10 | 0.0870 (10) | −0.1633 (10) | −0.0773 (13) | 0.076 (5)* | |
O11 | 0.1193 (8) | −0.1590 (8) | −0.2647 (14) | 0.065 (5)* | |
O12 | 0.2424 (8) | −0.1503 (10) | −0.2355 (15) | 0.081 (6)* | |
O13 | 0.3086 (10) | −0.0505 (6) | −0.172 (2) | 0.077 (6)* | |
O14 | 0.0774 (9) | −0.0509 (7) | −0.1720 (16) | 0.063 (5)* | |
O15 | 0.4209 (7) | 0.1271 (6) | −0.3951 (12) | 0.056 (4)* | |
O16 | 0.4053 (8) | 0.0019 (7) | −0.4102 (14) | 0.061 (4)* | |
O17 | 0.4033 (8) | −0.1325 (6) | −0.4244 (11) | 0.057 (4)* | |
O18 | 0.1913 (7) | 0.1321 (6) | −0.3769 (12) | 0.041 (3)* | |
O19 | 0.1877 (7) | −0.0013 (7) | −0.4080 (12) | 0.056 (4)* | |
O20 | 0.1981 (8) | −0.1302 (7) | −0.4137 (13) | 0.059 (5)* | |
O21 | −0.0015 (6) | 0.0492 (7) | −0.2057 (13) | 0.051 (4)* | |
O22 | −0.0042 (6) | −0.1525 (8) | −0.2125 (14) | 0.060 (4)* | |
O23 | 0.4234 (11) | −0.250000 | −0.349 (2) | 0.056 (6)* | |
O24 | 0.1893 (13) | −0.250000 | −0.352 (2) | 0.075 (8)* | |
O25 | 0.2862 (10) | −0.250000 | 0.0557 (17) | 0.042 (5)* | |
O26 | 0.1071 (10) | −0.250000 | 0.0633 (17) | 0.045 (5)* | |
Geometric parameters (Å, º) top
Si01—O15 | 1.573 (11) | Si07—O07 | 1.578 (16) |
Si01—O16 | 1.581 (15) | Si07—O17 | 1.583 (11) |
Si01—O01 | 1.593 (12) | Si07—O22i | 1.588 (12) |
Si01—O21i | 1.607 (14) | Si07—O23 | 1.607 (10) |
Si02—O06 | 1.579 (11) | Si08—O07 | 1.585 (15) |
Si02—O02 | 1.590 (15) | Si08—O13 | 1.588 (12) |
Si02—O01 | 1.598 (14) | Si08—O12 | 1.594 (11) |
Si02—O13 | 1.620 (15) | Si08—O08 | 1.596 (17) |
Si03—O03 | 1.574 (10) | Si09—O08 | 1.578 (16) |
Si03—O19ii | 1.576 (11) | Si09—O25 | 1.581 (9) |
Si03—O20ii | 1.583 (11) | Si09—O09 | 1.593 (11) |
Si03—O02 | 1.593 (12) | Si09—O18ii | 1.605 (15) |
Si04—O04 | 1.575 (16) | Si10—O09 | 1.582 (14) |
Si04—O03 | 1.589 (8) | Si10—O15ii | 1.592 (9) |
Si04—O17ii | 1.600 (9) | Si10—O10 | 1.595 (17) |
Si04—O16ii | 1.613 (15) | Si10—O26 | 1.601 (11) |
Si05—O05 | 1.578 (15) | Si11—O14 | 1.576 (14) |
Si05—O14 | 1.584 (14) | Si11—O10 | 1.594 (17) |
Si05—O21 | 1.588 (11) | Si11—O11 | 1.599 (16) |
Si05—O04 | 1.596 (15) | Si11—O22 | 1.600 (14) |
Si06—O19 | 1.583 (11) | Si12—O11 | 1.579 (16) |
Si06—O06 | 1.584 (11) | Si12—O20 | 1.581 (15) |
Si06—O05 | 1.599 (15) | Si12—O24 | 1.589 (13) |
Si06—O18 | 1.636 (14) | Si12—O12 | 1.591 (12) |
| | | |
O15—Si01—O16 | 106.0 (11) | O08—Si09—O09 | 107.6 (10) |
O15—Si01—O01 | 115.3 (10) | O25—Si09—O09 | 110.8 (10) |
O16—Si01—O01 | 109.2 (10) | O08—Si09—O18ii | 112.3 (9) |
O15—Si01—O21i | 108.2 (9) | O25—Si09—O18ii | 106.6 (10) |
O16—Si01—O21i | 109.5 (9) | O09—Si09—O18ii | 113.7 (9) |
O01—Si01—O21i | 108.4 (10) | O09—Si10—O15ii | 115.7 (10) |
O06—Si02—O02 | 112.8 (10) | O09—Si10—O10 | 107.4 (11) |
O06—Si02—O01 | 108.8 (11) | O15ii—Si10—O10 | 106.1 (11) |
O02—Si02—O01 | 107.2 (9) | O09—Si10—O26 | 112.1 (10) |
O06—Si02—O13 | 111.6 (11) | O15ii—Si10—O26 | 107.2 (10) |
O02—Si02—O13 | 105.3 (11) | O10—Si10—O26 | 108.0 (12) |
O01—Si02—O13 | 111.2 (10) | O14—Si11—O10 | 108.8 (11) |
O03—Si03—O19ii | 113.7 (10) | O14—Si11—O11 | 111.3 (10) |
O03—Si03—O20ii | 110.3 (10) | O10—Si11—O11 | 108.6 (11) |
O19ii—Si03—O20ii | 109.2 (11) | O14—Si11—O22 | 113.3 (10) |
O03—Si03—O02 | 109.4 (11) | O10—Si11—O22 | 107.7 (11) |
O19ii—Si03—O02 | 105.5 (9) | O11—Si11—O22 | 107.0 (10) |
O20ii—Si03—O02 | 108.6 (10) | O11—Si12—O20 | 111.1 (10) |
O04—Si04—O03 | 110.0 (12) | O11—Si12—O24 | 108.4 (13) |
O04—Si04—O17ii | 103.9 (9) | O20—Si12—O24 | 105.9 (13) |
O03—Si04—O17ii | 111.2 (10) | O11—Si12—O12 | 104.2 (11) |
O04—Si04—O16ii | 111.7 (10) | O20—Si12—O12 | 108.5 (11) |
O03—Si04—O16ii | 107.0 (10) | O24—Si12—O12 | 118.7 (14) |
O17ii—Si04—O16ii | 113.1 (11) | Si01—O01—Si02 | 152.8 (12) |
O05—Si05—O14 | 111.4 (10) | Si02—O02—Si03 | 149.5 (11) |
O05—Si05—O21 | 105.6 (9) | Si03—O03—Si04 | 173.3 (14) |
O14—Si05—O21 | 109.0 (9) | Si04—O04—Si05 | 152.3 (11) |
O05—Si05—O04 | 112.6 (9) | Si05—O05—Si06 | 146.4 (12) |
O14—Si05—O04 | 110.7 (10) | Si02—O06—Si06 | 161.1 (13) |
O21—Si05—O04 | 107.3 (10) | Si07—O07—Si08 | 152.1 (13) |
O19—Si06—O06 | 116.0 (10) | Si09—O08—Si08 | 152.4 (12) |
O19—Si06—O05 | 105.8 (9) | Si10—O09—Si09 | 154.2 (13) |
O06—Si06—O05 | 111.2 (11) | Si11—O10—Si10 | 159.7 (14) |
O19—Si06—O18 | 113.1 (10) | Si12—O11—Si11 | 156.5 (14) |
O06—Si06—O18 | 105.3 (9) | Si12—O12—Si08 | 163.4 (16) |
O05—Si06—O18 | 105.0 (8) | Si08—O13—Si02 | 169.3 (18) |
O07—Si07—O17 | 115.6 (10) | Si11—O14—Si05 | 166.8 (14) |
O07—Si07—O22i | 103.5 (10) | Si01—O15—Si10iii | 147.4 (11) |
O17—Si07—O22i | 112.5 (11) | Si01—O16—Si04iii | 169.0 (14) |
O07—Si07—O23 | 110.6 (12) | Si07—O17—Si04iii | 145.2 (12) |
O17—Si07—O23 | 107.9 (11) | Si09iii—O18—Si06 | 141.9 (11) |
O22i—Si07—O23 | 106.4 (11) | Si03iii—O19—Si06 | 153.6 (12) |
O07—Si08—O13 | 111.7 (10) | Si12—O20—Si03iii | 149.6 (13) |
O07—Si08—O12 | 116.9 (12) | Si05—O21—Si01iv | 148.8 (13) |
O13—Si08—O12 | 105.5 (11) | Si07iv—O22—Si11 | 146.7 (14) |
O07—Si08—O08 | 106.5 (10) | Si07—O23—Si07v | 156.9 (19) |
O13—Si08—O08 | 106.9 (12) | Si12v—O24—Si12 | 145 (2) |
O12—Si08—O08 | 108.9 (11) | Si09v—O25—Si09 | 152.1 (16) |
O08—Si09—O25 | 105.6 (11) | Si10v—O26—Si10 | 142.6 (17) |
Symmetry codes: (i) x+1/2, y, −z−1/2; (ii) −x+1/2, −y, z+1/2; (iii) −x+1/2, −y, z−1/2; (iv) x−1/2, y, −z−1/2; (v) x, −y−1/2, z. |