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The phase Na
5FeSi
4O
12 [pentasodium iron(III) silicate] crystallizes readily from the Na
2O–Fe
2O
3–SiO
2 glass system in a relatively large compositional range. However, its crystal structure and properties have not been studied in detail since its discovery in 1930. In this work, the Na
5FeSi
4O
12 phase was crystallized from a host glass with 5Na
2O·Fe
2O
3·8SiO
2 stoichiometry, and both the glass and the crystal were studied. It was found that the Na
5FeSi
4O
12 phase crystallizes at ∼720 °C from the glass and melts at ∼830 °C when heated at a rate of 10 °C min
−1. The crystal structure was solved using single-crystal X-ray diffraction and the refined data are reported for the first time for the Na
5FeSi
4O
12 phase. It exhibits trigonal symmetry, space group
Rc, with
a = 21.418 and
c = 12.2911 Å. The Na atoms located between adjacent structural channels exhibit positional disorder and splitting which was only refined by using low-temperature data collection (150 K). While ∼7% of the total Fe cations occur as Fe
2+ in the glass, four-coordinated Fe
3+ constitutes ∼93% of the total Fe cations. However, iron in the crystal, which exhibits a paramagnetic behavior, is solely present as six-coordinated Fe
3+. The magnetic and vibrational properties of the glass and crystal are discussed to provide additional insight into the structure.
Supporting information
CCDC reference: 1872659
Data collection: APEX2 (Bruker, 2014); cell refinement: APEX2 (Bruker, 2014); data reduction: APEX2 (Bruker, 2014) and SAINT (Bruker, 2014); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2015b); molecular graphics: CrystalMaker (CrystalMaker, 2018); software used to prepare material for publication: SHELXL2013 (Sheldrick, 2015a).
Pentasodium iron(III) silicate
top
Crystal data top
Na5FeSi4O12 | Dx = 2.903 Mg m−3 |
Mr = 474.27 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3c | Cell parameters from 4854 reflections |
a = 21.418 (3) Å | θ = 3.3–30.7° |
c = 12.2911 (18) Å | µ = 2.10 mm−1 |
V = 4883.0 (16) Å3 | T = 150 K |
Z = 18 | Plate, red orange |
F(000) = 4186 | 0.02 × 0.01 × 0.003 mm |
Data collection top
Bruker SMART APEXII three-circle diffractometer | 892 reflections with I > 2σ(I) |
Radiation source: X-ray tube | Rint = 0.069 |
ω scans | θmax = 26.4°, θmin = 3.3° |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | h = −26→26 |
Tmin = 0.640, Tmax = 0.746 | k = −26→26 |
15291 measured reflections | l = −15→15 |
1108 independent reflections | |
Refinement top
Refinement on F2 | 118 parameters |
Least-squares matrix: full | 0 restraints |
R[F2 > 2σ(F2)] = 0.019 | w = 1/[σ2(Fo2) + (0.022P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.046 | (Δ/σ)max < 0.001 |
S = 1.01 | Δρmax = 0.37 e Å−3 |
1108 reflections | Δρmin = −0.35 e Å−3 |
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. A thin plate exhibiting sharp extinction under cross polarized light was
selected and mounted on a Mitegen cryoloop for the single crystal X-ray
diffraction experiment at 150 (2) K. Data were collected using Mo Kα
X-rays and an Apex II CCD-based detectormounted to a Bruker Smart Apex II
three-circle diffractometer. Reflections were integrated and corrected for
Lorentz, polarization, and background effects using the Bruker program
SAINT. A multi-scan semi-empirical absorption correction was applied
using equivalent reflections in SADABS-2015. An initial structure model was
obtained by the charge-flipping method using SHELXT (Sheldrick, 2015a), and
refinements were made by full-matrix least-squares on F2 using
SHELXL-2013 (Sheldrick, 2015b). |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Fe1 | 0.6667 | 0.08597 (2) | 0.0833 | 0.00531 (12) | |
Si1 | 0.77731 (3) | 0.01612 (3) | 0.01782 (5) | 0.00555 (15) | |
Si2 | 0.90941 (3) | 0.09550 (3) | −0.12341 (5) | 0.00597 (14) | |
Na1 | 1.0000 | 0.0000 | −0.2500 | 0.0053 (4) | |
Na2 | 1.0000 | 0.0000 | 0.0000 | 0.0091 (4) | |
Na3 | 0.92352 (5) | 0.06573 (5) | −0.36144 (7) | 0.0119 (2) | |
Na4 | 0.61847 (6) | −0.04819 (6) | −0.0833 | 0.0143 (3) | |
Na5 | 0.8333 | 0.1667 | 0.1667 | 0.0318 (11) | 0.682 (7) |
Na51 | 0.8493 (4) | 0.1771 (4) | 0.0653 (13) | 0.008 (3)* | 0.144 (9) |
Na52 | 0.8512 (3) | 0.1796 (4) | 0.0211 (14) | 0.004 (3)* | 0.145 (10) |
Na53 | 0.840 (5) | 0.168 (5) | −0.031 (11) | 0.04 (3)* | 0.017 (7) |
O1 | 0.95460 (8) | 0.05533 (8) | −0.13075 (13) | 0.0122 (4) | |
O2 | 0.73849 (8) | −0.02816 (8) | −0.08974 (13) | 0.0097 (3) | |
O3 | 0.85626 (8) | 0.07936 (8) | −0.22531 (13) | 0.0093 (3) | |
O4 | 0.96207 (8) | 0.18437 (8) | −0.11467 (13) | 0.0094 (3) | |
O5 | 0.86316 (8) | 0.07307 (8) | −0.00744 (13) | 0.0111 (4) | |
O6 | 0.74346 (9) | 0.05886 (9) | 0.07485 (13) | 0.0126 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0050 (2) | 0.00458 (17) | 0.0065 (2) | 0.00249 (11) | 0.00023 (18) | 0.00011 (9) |
Si1 | 0.0051 (3) | 0.0058 (3) | 0.0064 (3) | 0.0032 (2) | 0.0002 (2) | 0.0006 (2) |
Si2 | 0.0048 (3) | 0.0050 (3) | 0.0072 (3) | 0.0018 (2) | −0.0008 (2) | −0.0005 (2) |
Na1 | 0.0053 (6) | 0.0053 (6) | 0.0051 (10) | 0.0027 (3) | 0.000 | 0.000 |
Na2 | 0.0093 (7) | 0.0093 (7) | 0.0088 (11) | 0.0046 (3) | 0.000 | 0.000 |
Na3 | 0.0130 (5) | 0.0099 (5) | 0.0137 (5) | 0.0065 (4) | 0.0023 (4) | 0.0013 (4) |
Na4 | 0.0131 (5) | 0.0131 (5) | 0.0127 (7) | 0.0035 (6) | 0.0033 (3) | −0.0033 (3) |
Na5 | 0.0230 (14) | 0.0087 (12) | 0.061 (2) | 0.0058 (10) | −0.0258 (13) | −0.0051 (11) |
O1 | 0.0104 (8) | 0.0089 (8) | 0.0177 (9) | 0.0052 (7) | −0.0015 (7) | −0.0021 (7) |
O2 | 0.0092 (8) | 0.0085 (8) | 0.0090 (9) | 0.0026 (6) | −0.0007 (6) | 0.0010 (6) |
O3 | 0.0057 (8) | 0.0088 (8) | 0.0110 (9) | 0.0016 (6) | −0.0014 (6) | −0.0005 (7) |
O4 | 0.0103 (8) | 0.0062 (8) | 0.0081 (9) | 0.0015 (7) | −0.0006 (6) | 0.0003 (6) |
O5 | 0.0067 (8) | 0.0141 (9) | 0.0088 (9) | 0.0023 (7) | −0.0004 (6) | 0.0002 (7) |
O6 | 0.0158 (9) | 0.0178 (9) | 0.0118 (9) | 0.0139 (8) | 0.0011 (7) | 0.0006 (7) |
Geometric parameters (Å, º) top
Fe1—O6 | 2.0021 (16) | Na4—O6xv | 2.4139 (16) |
Fe1—O6i | 2.0022 (16) | Na4—O4xvi | 2.5162 (18) |
Fe1—O3ii | 2.0333 (15) | Na4—O4xvii | 2.5163 (18) |
Fe1—O3iii | 2.0334 (15) | Na4—Na51iv | 2.953 (7) |
Fe1—O2iii | 2.0378 (16) | Na4—Na51xviii | 2.953 (7) |
Fe1—O2ii | 2.0379 (16) | Na4—Na52iv | 2.996 (8) |
Fe1—Na4 | 3.2486 (9) | Na4—Na52xviii | 2.996 (8) |
Fe1—Na4ii | 3.2486 (9) | Na4—Si1i | 3.0967 (9) |
Fe1—Na5 | 3.2572 (4) | Na4—Si1xv | 3.0968 (9) |
Fe1—Na5i | 3.2572 (4) | Na5—Na51xix | 1.282 (16) |
Fe1—Na51i | 3.395 (7) | Na5—Na51 | 1.282 (16) |
Fe1—Na51 | 3.396 (7) | Na5—Na52 | 1.822 (17) |
Si1—O6 | 1.5870 (16) | Na5—Na52xix | 1.822 (17) |
Si1—O2 | 1.5968 (17) | Na5—O6xix | 2.4218 (18) |
Si1—O5 | 1.6501 (17) | Na5—O6 | 2.4218 (17) |
Si1—O4iv | 1.6635 (17) | Na5—Na53 | 2.43 (13) |
Si1—Na53 | 2.89 (8) | Na5—Na53xix | 2.43 (13) |
Si1—Na52 | 3.038 (7) | Na5—O3v | 2.5336 (16) |
Si1—Na51 | 3.048 (7) | Na5—O3iii | 2.5336 (16) |
Si1—Na4ii | 3.0968 (9) | Na5—O2xii | 2.7383 (16) |
Si1—Na52iv | 3.136 (7) | Na5—O2ii | 2.7383 (16) |
Si1—Na4 | 3.2140 (12) | Na51—Na52 | 0.546 (11) |
Si1—Na53iv | 3.28 (9) | Na51—Na53 | 1.19 (13) |
Si1—Na3v | 3.2908 (11) | Na51—O2xii | 2.295 (7) |
Si2—O1 | 1.5868 (16) | Na51—O3iii | 2.359 (7) |
Si2—O3 | 1.6095 (17) | Na51—O6 | 2.414 (7) |
Si2—O4 | 1.6614 (16) | Na51—Na53iii | 2.49 (13) |
Si2—O5 | 1.6636 (18) | Na51—O5 | 2.552 (8) |
Si2—Na53iii | 2.84 (8) | Na51—Na51xix | 2.56 (3) |
Si2—Na53 | 2.86 (9) | Na51—O4iii | 2.899 (11) |
Si2—Na52iii | 2.944 (8) | Na51—Na4xii | 2.953 (7) |
Si2—Na3 | 3.0413 (11) | Na52—Na53 | 0.68 (13) |
Si2—Na3vi | 3.0601 (12) | Na52—Na53iii | 1.96 (13) |
Si2—Na51iii | 3.141 (9) | Na52—O2xii | 2.396 (9) |
Si2—Na52 | 3.194 (11) | Na52—O3iii | 2.411 (7) |
Si2—Na3vii | 3.2032 (12) | Na52—O5 | 2.446 (7) |
Na1—O1viii | 2.3770 (15) | Na52—O6 | 2.546 (8) |
Na1—O1 | 2.3771 (15) | Na52—Na52iii | 2.57 (3) |
Na1—O1vi | 2.3771 (15) | Na52—O4iii | 2.639 (8) |
Na1—O1ix | 2.3771 (15) | Na52—O4 | 2.862 (11) |
Na1—O1x | 2.3771 (15) | Na52—Si2iii | 2.944 (8) |
Na1—O1vii | 2.3771 (15) | Na53—Na53iii | 1.3 (3) |
Na1—Na3 | 2.9745 (9) | Na53—Na52iii | 1.96 (13) |
Na1—Na3vii | 2.9746 (9) | Na53—O5 | 2.33 (8) |
Na1—Na3ix | 2.9746 (9) | Na53—Na51iii | 2.49 (13) |
Na1—Na3x | 2.9746 (9) | Na53—O3iii | 2.54 (9) |
Na1—Na3vi | 2.9746 (9) | Na53—O6 | 2.57 (8) |
Na1—Na3viii | 2.9746 (9) | Na53—O4iii | 2.64 (8) |
Na2—O1xi | 2.4667 (16) | Na53—O4 | 2.66 (8) |
Na2—O1xii | 2.4668 (16) | Na53—Si2iii | 2.84 (8) |
Na2—O1ix | 2.4668 (16) | O1—Na3vii | 2.3300 (18) |
Na2—O1 | 2.4668 (16) | O1—Na3vi | 2.3783 (18) |
Na2—O1iv | 2.4668 (16) | O2—Fe1xv | 2.0378 (16) |
Na2—O1x | 2.4668 (16) | O2—Na51iv | 2.295 (7) |
Na2—Na1xi | 3.0728 (5) | O2—Na52iv | 2.396 (9) |
Na2—Na3vi | 3.1421 (9) | O2—Na5xv | 2.7383 (16) |
Na2—Na3xiii | 3.1421 (9) | O2—Na53iv | 2.85 (12) |
Na2—Na3v | 3.1421 (9) | O3—Fe1xv | 2.0333 (15) |
Na2—Na3viii | 3.1421 (9) | O3—Na51iii | 2.359 (7) |
Na3—O3 | 2.3195 (18) | O3—Na52iii | 2.411 (7) |
Na3—O1vii | 2.3299 (18) | O3—Na5iii | 2.5336 (16) |
Na3—O5xiv | 2.3311 (18) | O3—Na53iii | 2.54 (9) |
Na3—O1vi | 2.3781 (18) | O4—Si1xii | 1.6634 (17) |
Na3—O1 | 2.9462 (19) | O4—Na4xx | 2.5162 (18) |
Na3—O4vii | 3.0198 (18) | O4—Na53iii | 2.64 (8) |
Na3—Si2vi | 3.0601 (12) | O4—Na52iii | 2.639 (8) |
Na3—Na2viii | 3.1420 (9) | O4—Na51iii | 2.899 (11) |
Na3—Si2vii | 3.2032 (12) | O4—Na3vii | 3.0198 (18) |
Na3—Si1xiv | 3.2908 (11) | O5—Na3v | 2.3310 (18) |
Na4—O2 | 2.3864 (18) | O5—Na53iii | 2.97 (10) |
Na4—O2iii | 2.3865 (18) | O6—Na4ii | 2.4139 (16) |
Na4—O6i | 2.4138 (16) | | |
| | | |
O6—Fe1—O6i | 91.02 (10) | Na51xviii—Na4—Na52iv | 157.39 (16) |
O6—Fe1—O3ii | 174.17 (6) | O2—Na4—Na52xviii | 146.93 (19) |
O6i—Fe1—O3ii | 87.09 (7) | O2iii—Na4—Na52xviii | 51.36 (15) |
O6—Fe1—O3iii | 87.09 (7) | O6i—Na4—Na52xviii | 78.4 (3) |
O6i—Fe1—O3iii | 174.17 (6) | O6xv—Na4—Na52xviii | 101.8 (3) |
O3ii—Fe1—O3iii | 95.32 (9) | O4xvi—Na4—Na52xviii | 56.4 (2) |
O6—Fe1—O2iii | 97.56 (6) | O4xvii—Na4—Na52xviii | 108.5 (2) |
O6i—Fe1—O2iii | 82.39 (6) | Na51iv—Na4—Na52xviii | 157.40 (16) |
O3ii—Fe1—O2iii | 87.66 (6) | Na51xviii—Na4—Na52xviii | 10.5 (2) |
O3iii—Fe1—O2iii | 92.39 (6) | Na52iv—Na4—Na52xviii | 160.4 (2) |
O6—Fe1—O2ii | 82.39 (6) | O2—Na4—Si1i | 109.99 (4) |
O6i—Fe1—O2ii | 97.56 (6) | O2iii—Na4—Si1i | 97.53 (4) |
O3ii—Fe1—O2ii | 92.39 (6) | O6i—Na4—Si1i | 30.37 (4) |
O3iii—Fe1—O2ii | 87.66 (6) | O6xv—Na4—Si1i | 150.26 (6) |
O2iii—Fe1—O2ii | 179.92 (9) | O4xvi—Na4—Si1i | 108.68 (6) |
O6—Fe1—Na4 | 69.78 (5) | O4xvii—Na4—Si1i | 32.43 (4) |
O6i—Fe1—Na4 | 47.81 (5) | Na51iv—Na4—Si1i | 87.7 (3) |
O3ii—Fe1—Na4 | 112.56 (5) | Na51xviii—Na4—Si1i | 84.7 (3) |
O3iii—Fe1—Na4 | 126.43 (5) | Na52iv—Na4—Si1i | 78.0 (3) |
O2iii—Fe1—Na4 | 47.11 (5) | Na52xviii—Na4—Si1i | 94.6 (3) |
O2ii—Fe1—Na4 | 132.81 (5) | O2—Na4—Si1xv | 97.52 (4) |
O6—Fe1—Na4ii | 47.82 (5) | O2iii—Na4—Si1xv | 109.99 (4) |
O6i—Fe1—Na4ii | 69.78 (5) | O6i—Na4—Si1xv | 150.26 (6) |
O3ii—Fe1—Na4ii | 126.43 (5) | O6xv—Na4—Si1xv | 30.37 (4) |
O3iii—Fe1—Na4ii | 112.56 (5) | O4xvi—Na4—Si1xv | 32.43 (4) |
O2iii—Fe1—Na4ii | 132.81 (5) | O4xvii—Na4—Si1xv | 108.68 (6) |
O2ii—Fe1—Na4ii | 47.11 (5) | Na51iv—Na4—Si1xv | 84.7 (3) |
Na4—Fe1—Na4ii | 86.946 (16) | Na51xviii—Na4—Si1xv | 87.7 (3) |
O6—Fe1—Na5 | 47.85 (5) | Na52iv—Na4—Si1xv | 94.6 (3) |
O6i—Fe1—Na5 | 130.29 (5) | Na52xviii—Na4—Si1xv | 78.0 (3) |
O3ii—Fe1—Na5 | 130.68 (5) | Si1i—Na4—Si1xv | 135.81 (5) |
O3iii—Fe1—Na5 | 51.06 (5) | Na51xix—Na5—Na51 | 180.0 |
O2iii—Fe1—Na5 | 123.17 (4) | Na51xix—Na5—Na52 | 177.1 (4) |
O2ii—Fe1—Na5 | 56.83 (4) | Na51—Na5—Na52 | 2.9 (4) |
Na4—Fe1—Na5 | 116.582 (17) | Na51xix—Na5—Na52xix | 2.9 (4) |
Na4ii—Fe1—Na5 | 61.832 (15) | Na51—Na5—Na52xix | 177.1 (4) |
O6—Fe1—Na5i | 130.30 (5) | Na52—Na5—Na52xix | 180.0 |
O6i—Fe1—Na5i | 47.85 (5) | Na51xix—Na5—O6xix | 74.3 (3) |
O3ii—Fe1—Na5i | 51.06 (5) | Na51—Na5—O6xix | 105.7 (3) |
O3iii—Fe1—Na5i | 130.68 (5) | Na52—Na5—O6xix | 107.8 (2) |
O2iii—Fe1—Na5i | 56.82 (4) | Na52xix—Na5—O6xix | 72.2 (2) |
O2ii—Fe1—Na5i | 123.17 (4) | Na51xix—Na5—O6 | 105.7 (3) |
Na4—Fe1—Na5i | 61.832 (15) | Na51—Na5—O6 | 74.3 (3) |
Na4ii—Fe1—Na5i | 116.542 (17) | Na52—Na5—O6 | 72.2 (2) |
Na5—Fe1—Na5i | 178.070 (16) | Na52xix—Na5—O6 | 107.8 (2) |
O6—Fe1—Na51i | 135.44 (12) | O6xix—Na5—O6 | 180.0 |
O6i—Fe1—Na51i | 44.42 (12) | Na51xix—Na5—Na53 | 169 (2) |
O3ii—Fe1—Na51i | 43.00 (13) | Na51—Na5—Na53 | 11 (2) |
O3iii—Fe1—Na51i | 137.13 (12) | Na52—Na5—Na53 | 8 (2) |
O2iii—Fe1—Na51i | 78.9 (3) | Na52xix—Na5—Na53 | 172 (2) |
O2ii—Fe1—Na51i | 101.1 (3) | O6xix—Na5—Na53 | 116 (2) |
Na4—Fe1—Na51i | 76.4 (2) | O6—Na5—Na53 | 64 (2) |
Na4ii—Fe1—Na51i | 103.45 (19) | Na51xix—Na5—Na53xix | 11 (2) |
Na5—Fe1—Na51i | 157.9 (3) | Na51—Na5—Na53xix | 169 (2) |
Na5i—Fe1—Na51i | 22.1 (3) | Na52—Na5—Na53xix | 172 (2) |
O6—Fe1—Na51 | 44.42 (12) | Na52xix—Na5—Na53xix | 8 (2) |
O6i—Fe1—Na51 | 135.44 (12) | O6xix—Na5—Na53xix | 64 (2) |
O3ii—Fe1—Na51 | 137.14 (12) | O6—Na5—Na53xix | 116 (2) |
O3iii—Fe1—Na51 | 43.00 (13) | Na53—Na5—Na53xix | 180.0 |
O2iii—Fe1—Na51 | 101.1 (3) | Na51xix—Na5—O3v | 67.4 (3) |
O2ii—Fe1—Na51 | 78.9 (3) | Na51—Na5—O3v | 112.6 (3) |
Na4—Fe1—Na51 | 103.45 (19) | Na52—Na5—O3v | 115.2 (2) |
Na4ii—Fe1—Na51 | 76.5 (2) | Na52xix—Na5—O3v | 64.8 (2) |
Na5—Fe1—Na51 | 22.1 (3) | O6xix—Na5—O3v | 68.21 (5) |
Na5i—Fe1—Na51 | 157.9 (3) | O6—Na5—O3v | 111.79 (5) |
Na51i—Fe1—Na51 | 179.9 (2) | Na53—Na5—O3v | 118.5 (19) |
O6—Si1—O2 | 117.13 (9) | Na53xix—Na5—O3v | 61.5 (19) |
O6—Si1—O5 | 108.56 (9) | Na51xix—Na5—O3iii | 112.6 (3) |
O2—Si1—O5 | 109.88 (9) | Na51—Na5—O3iii | 67.4 (3) |
O6—Si1—O4iv | 104.36 (9) | Na52—Na5—O3iii | 64.8 (2) |
O2—Si1—O4iv | 111.19 (9) | Na52xix—Na5—O3iii | 115.2 (2) |
O5—Si1—O4iv | 104.93 (8) | O6xix—Na5—O3iii | 111.79 (5) |
O6—Si1—Na53 | 62.2 (19) | O6—Na5—O3iii | 68.21 (5) |
O2—Si1—Na53 | 108 (3) | Na53—Na5—O3iii | 61.5 (19) |
O5—Si1—Na53 | 53.7 (16) | Na53xix—Na5—O3iii | 118.5 (19) |
O4iv—Si1—Na53 | 140 (3) | O3v—Na5—O3iii | 180.0 |
O6—Si1—Na52 | 56.9 (2) | Na51xix—Na5—O2xii | 123.5 (3) |
O2—Si1—Na52 | 120.8 (3) | Na51—Na5—O2xii | 56.5 (3) |
O5—Si1—Na52 | 53.47 (14) | Na52—Na5—O2xii | 59.4 (2) |
O4iv—Si1—Na52 | 127.7 (3) | Na52xix—Na5—O2xii | 120.6 (2) |
Na53—Si1—Na52 | 13 (3) | O6xix—Na5—O2xii | 61.72 (5) |
O6—Si1—Na51 | 51.81 (19) | O6—Na5—O2xii | 118.28 (5) |
O2—Si1—Na51 | 130.5 (3) | Na53—Na5—O2xii | 67 (2) |
O5—Si1—Na51 | 56.85 (17) | Na53xix—Na5—O2xii | 113 (2) |
O4iv—Si1—Na51 | 118.3 (3) | O3v—Na5—O2xii | 64.53 (5) |
Na53—Si1—Na51 | 23 (3) | O3iii—Na5—O2xii | 115.47 (5) |
Na52—Si1—Na51 | 10.3 (2) | Na51xix—Na5—O2ii | 56.5 (3) |
O6—Si1—Na4ii | 50.28 (6) | Na51—Na5—O2ii | 123.5 (3) |
O2—Si1—Na4ii | 128.99 (7) | Na52—Na5—O2ii | 120.6 (2) |
O5—Si1—Na4ii | 121.02 (6) | Na52xix—Na5—O2ii | 59.4 (2) |
O4iv—Si1—Na4ii | 54.21 (6) | O6xix—Na5—O2ii | 118.27 (5) |
Na53—Si1—Na4ii | 104 (2) | O6—Na5—O2ii | 61.72 (5) |
Na52—Si1—Na4ii | 93.6 (3) | Na53—Na5—O2ii | 113 (2) |
Na51—Si1—Na4ii | 84.0 (3) | Na53xix—Na5—O2ii | 67 (2) |
O6—Si1—Na52iv | 115.86 (18) | O3v—Na5—O2ii | 115.47 (5) |
O2—Si1—Na52iv | 48.4 (3) | O3iii—Na5—O2ii | 64.53 (5) |
O5—Si1—Na52iv | 135.58 (18) | O2xii—Na5—O2ii | 180.0 |
O4iv—Si1—Na52iv | 65.0 (3) | Na52—Na51—Na53 | 14 (4) |
Na53—Si1—Na52iv | 155 (2) | Na52—Na51—Na5 | 170.1 (14) |
Na52—Si1—Na52iv | 165.25 (15) | Na53—Na51—Na5 | 158 (4) |
Na51—Si1—Na52iv | 167.25 (16) | Na52—Na51—O2xii | 94.1 (13) |
Na4ii—Si1—Na52iv | 89.2 (3) | Na53—Na51—O2xii | 105 (4) |
O6—Si1—Na4 | 74.17 (7) | Na5—Na51—O2xii | 95.7 (6) |
O2—Si1—Na4 | 45.57 (6) | Na52—Na51—O3iii | 88.9 (12) |
O5—Si1—Na4 | 142.52 (7) | Na53—Na51—O3iii | 84 (4) |
O4iv—Si1—Na4 | 110.55 (6) | Na5—Na51—O3iii | 82.5 (4) |
Na53—Si1—Na4 | 102 (2) | O2xii—Na51—O3iii | 146.7 (3) |
Na52—Si1—Na4 | 109.19 (18) | Na52—Na51—O6 | 97.8 (13) |
Na51—Si1—Na4 | 112.80 (15) | Na53—Na51—O6 | 84 (4) |
Na4ii—Si1—Na4 | 90.18 (2) | Na5—Na51—O6 | 75.0 (4) |
Na52iv—Si1—Na4 | 56.28 (17) | O2xii—Na51—O6 | 140.5 (4) |
O6—Si1—Na53iv | 113.1 (15) | O3iii—Na51—O6 | 71.24 (19) |
O2—Si1—Na53iv | 60 (2) | Na52—Na51—Na53iii | 10 (2) |
O5—Si1—Na53iv | 136.7 (14) | Na53—Na51—Na53iii | 7 (4) |
O4iv—Si1—Na53iv | 54 (2) | Na5—Na51—Na53iii | 160 (2) |
Na53—Si1—Na53iv | 165.0 (19) | O2xii—Na51—Na53iii | 104 (2) |
Na52—Si1—Na53iv | 169.8 (14) | O3iii—Na51—Na53iii | 82 (2) |
Na51—Si1—Na53iv | 163.1 (18) | O6—Na51—Na53iii | 89 (2) |
Na4ii—Si1—Na53iv | 80 (2) | Na52—Na51—O5 | 72.7 (11) |
Na52iv—Si1—Na53iv | 12 (2) | Na53—Na51—O5 | 66 (4) |
Na4—Si1—Na53iv | 63.6 (19) | Na5—Na51—O5 | 109.0 (5) |
O6—Si1—Na3v | 104.22 (7) | O2xii—Na51—O5 | 84.4 (2) |
O2—Si1—Na3v | 137.13 (7) | O3iii—Na51—O5 | 127.7 (4) |
O5—Si1—Na3v | 41.62 (6) | O6—Na51—O5 | 63.84 (17) |
O4iv—Si1—Na3v | 65.86 (6) | Na53iii—Na51—O5 | 72.2 (19) |
Na53—Si1—Na3v | 81 (2) | Na52—Na51—Na51xix | 170.1 (14) |
Na52—Si1—Na3v | 72.56 (19) | Na53—Na51—Na51xix | 158 (4) |
Na51—Si1—Na3v | 68.25 (16) | Na5—Na51—Na51xix | 0.003 (1) |
Na4ii—Si1—Na3v | 85.85 (3) | O2xii—Na51—Na51xix | 95.7 (6) |
Na52iv—Si1—Na3v | 122.13 (18) | O3iii—Na51—Na51xix | 82.5 (4) |
Na4—Si1—Na3v | 175.78 (3) | O6—Na51—Na51xix | 75.0 (4) |
Na53iv—Si1—Na3v | 114 (2) | Na53iii—Na51—Na51xix | 160 (2) |
O1—Si2—O3 | 113.39 (9) | O5—Na51—Na51xix | 109.0 (5) |
O1—Si2—O4 | 112.09 (8) | Na52—Na51—O4iii | 56.6 (11) |
O3—Si2—O4 | 107.36 (9) | Na53—Na51—O4iii | 65 (4) |
O1—Si2—O5 | 109.19 (9) | Na5—Na51—O4iii | 121.4 (4) |
O3—Si2—O5 | 110.47 (9) | O2xii—Na51—O4iii | 95.5 (3) |
O4—Si2—O5 | 103.92 (8) | O3iii—Na51—O4iii | 59.1 (2) |
O1—Si2—Na53iii | 173 (3) | O6—Na51—O4iii | 122.4 (4) |
O3—Si2—Na53iii | 62 (2) | Na53iii—Na51—O4iii | 58 (2) |
O4—Si2—Na53iii | 65.6 (18) | O5—Na51—O4iii | 129.2 (6) |
O5—Si2—Na53iii | 78 (3) | Na51xix—Na51—O4iii | 121.4 (4) |
O1—Si2—Na53 | 160 (3) | Na52—Na51—Na4xii | 89.3 (13) |
O3—Si2—Na53 | 86 (3) | Na53—Na51—Na4xii | 103 (4) |
O4—Si2—Na53 | 65.9 (18) | Na5—Na51—Na4xii | 96.2 (5) |
O5—Si2—Na53 | 54.6 (19) | O2xii—Na51—Na4xii | 52.29 (14) |
Na53iii—Si2—Na53 | 27 (5) | O3iii—Na51—Na4xii | 94.7 (2) |
O1—Si2—Na52iii | 159.7 (3) | O6—Na51—Na4xii | 164.0 (4) |
O3—Si2—Na52iii | 54.9 (3) | Na53iii—Na51—Na4xii | 97 (2) |
O4—Si2—Na52iii | 62.86 (15) | O5—Na51—Na4xii | 132.1 (3) |
O5—Si2—Na52iii | 91.0 (3) | Na51xix—Na51—Na4xii | 96.2 (5) |
Na53iii—Si2—Na52iii | 13 (3) | O4iii—Na51—Na4xii | 50.92 (14) |
Na53—Si2—Na52iii | 39 (3) | Na52—Na51—Si1 | 83.8 (12) |
O1—Si2—Na3 | 71.35 (6) | Na53—Na51—Si1 | 71 (4) |
O3—Si2—Na3 | 48.71 (6) | Na5—Na51—Si1 | 92.8 (4) |
O4—Si2—Na3 | 102.75 (6) | O2xii—Na51—Si1 | 114.7 (2) |
O5—Si2—Na3 | 150.56 (7) | O3iii—Na51—Si1 | 98.6 (2) |
Na53iii—Si2—Na3 | 102 (3) | O6—Na51—Si1 | 31.11 (9) |
Na53—Si2—Na3 | 129 (2) | Na53iii—Na51—Si1 | 78 (2) |
Na52iii—Si2—Na3 | 90.2 (3) | O5—Na51—Si1 | 32.77 (9) |
O1—Si2—Na3vi | 50.13 (6) | Na51xix—Na51—Si1 | 92.8 (4) |
O3—Si2—Na3vi | 83.84 (6) | O4iii—Na51—Si1 | 132.2 (5) |
O4—Si2—Na3vi | 162.21 (6) | Na4xii—Na51—Si1 | 164.9 (4) |
O5—Si2—Na3vi | 84.22 (6) | Na51—Na52—Na53 | 154 (7) |
Na53iii—Si2—Na3vi | 132.1 (17) | Na51—Na52—Na5 | 6.9 (10) |
Na53—Si2—Na3vi | 130.1 (17) | Na53—Na52—Na5 | 149 (7) |
Na52iii—Si2—Na3vi | 133.69 (16) | Na51—Na52—Na53iii | 167 (3) |
Na3—Si2—Na3vi | 73.90 (3) | Na53—Na52—Na53iii | 15 (6) |
O1—Si2—Na51iii | 150.9 (3) | Na5—Na52—Na53iii | 161 (3) |
O3—Si2—Na51iii | 47.0 (2) | Na51—Na52—O2xii | 72.8 (13) |
O4—Si2—Na51iii | 66.15 (17) | Na53—Na52—O2xii | 126 (7) |
O5—Si2—Na51iii | 99.0 (2) | Na5—Na52—O2xii | 79.7 (5) |
Na53iii—Si2—Na51iii | 22 (3) | Na53iii—Na52—O2xii | 120 (3) |
Na53—Si2—Na51iii | 49 (2) | Na51—Na52—O3iii | 78.1 (11) |
Na52iii—Si2—Na51iii | 9.6 (2) | Na53—Na52—O3iii | 93 (7) |
Na3—Si2—Na51iii | 80.6 (3) | Na5—Na52—O3iii | 72.0 (4) |
Na3vi—Si2—Na51iii | 128.93 (18) | Na53iii—Na52—O3iii | 93 (2) |
O1—Si2—Na52 | 148.6 (3) | O2xii—Na52—O3iii | 136.1 (6) |
O3—Si2—Na52 | 96.9 (3) | Na51—Na52—O5 | 95.0 (12) |
O4—Si2—Na52 | 63.29 (14) | Na53—Na52—O5 | 72 (7) |
O5—Si2—Na52 | 48.9 (2) | Na5—Na52—O5 | 96.3 (4) |
Na53iii—Si2—Na52 | 37 (3) | Na53iii—Na52—O5 | 84 (2) |
Na53—Si2—Na52 | 11 (2) | O2xii—Na52—O5 | 84.7 (2) |
Na52iii—Si2—Na52 | 49.4 (6) | O3iii—Na52—O5 | 130.4 (3) |
Na3—Si2—Na52 | 139.5 (3) | Na51—Na52—O6 | 69.9 (11) |
Na3vi—Si2—Na52 | 130.37 (16) | Na53—Na52—O6 | 84 (7) |
Na51iii—Si2—Na52 | 58.9 (5) | Na5—Na52—O6 | 64.9 (3) |
O1—Si2—Na3vii | 43.70 (6) | Na53iii—Na52—O6 | 99 (3) |
O3—Si2—Na3vii | 125.56 (7) | O2xii—Na52—O6 | 127.5 (5) |
O4—Si2—Na3vii | 68.50 (6) | O3iii—Na52—O6 | 68.2 (2) |
O5—Si2—Na3vii | 123.43 (6) | O5—Na52—O6 | 63.50 (17) |
Na53iii—Si2—Na3vii | 133 (2) | Na51—Na52—Na52iii | 174.4 (13) |
Na53—Si2—Na3vii | 131 (2) | Na53—Na52—Na52iii | 21 (7) |
Na52iii—Si2—Na3vii | 125.81 (16) | Na5—Na52—Na52iii | 167.5 (3) |
Na3—Si2—Na3vii | 78.29 (3) | Na53iii—Na52—Na52iii | 7 (3) |
Na3vi—Si2—Na3vii | 93.78 (3) | O2xii—Na52—Na52iii | 112.8 (4) |
Na51iii—Si2—Na3vii | 123.48 (14) | O3iii—Na52—Na52iii | 97.4 (5) |
Na52—Si2—Na3vii | 123.12 (15) | O5—Na52—Na52iii | 85.4 (5) |
O1viii—Na1—O1 | 174.87 (8) | O6—Na52—Na52iii | 105.4 (4) |
O1viii—Na1—O1vi | 85.97 (6) | Na51—Na52—O4iii | 113.4 (13) |
O1—Na1—O1vi | 97.65 (8) | Na53—Na52—O4iii | 82 (7) |
O1viii—Na1—O1ix | 97.65 (8) | Na5—Na52—O4iii | 112.3 (4) |
O1—Na1—O1ix | 85.97 (6) | Na53iii—Na52—O4iii | 69 (2) |
O1vi—Na1—O1ix | 90.65 (8) | O2xii—Na52—O4iii | 100.2 (2) |
O1viii—Na1—O1x | 90.65 (8) | O3iii—Na52—O4iii | 62.73 (16) |
O1—Na1—O1x | 85.97 (6) | O5—Na52—O4iii | 151.4 (7) |
O1vi—Na1—O1x | 174.87 (8) | O6—Na52—O4iii | 128.1 (3) |
O1ix—Na1—O1x | 85.97 (6) | Na52iii—Na52—O4iii | 66.6 (4) |
O1viii—Na1—O1vii | 85.97 (6) | Na51—Na52—O4 | 127.0 (12) |
O1—Na1—O1vii | 90.65 (8) | Na53—Na52—O4 | 66 (7) |
O1vi—Na1—O1vii | 85.97 (6) | Na5—Na52—O4 | 133.2 (4) |
O1ix—Na1—O1vii | 174.87 (8) | Na53iii—Na52—O4 | 63 (3) |
O1x—Na1—O1vii | 97.66 (8) | O2xii—Na52—O4 | 60.77 (17) |
O1viii—Na1—Na3 | 114.51 (4) | O3iii—Na52—O4 | 154.7 (7) |
O1—Na1—Na3 | 65.71 (4) | O5—Na52—O4 | 58.5 (2) |
O1vi—Na1—Na3 | 51.29 (4) | O6—Na52—O4 | 120.1 (3) |
O1ix—Na1—Na3 | 124.81 (4) | Na52iii—Na52—O4 | 57.8 (4) |
O1x—Na1—Na3 | 133.81 (4) | O4iii—Na52—O4 | 99.2 (4) |
O1vii—Na1—Na3 | 50.11 (4) | Na51—Na52—Si2iii | 106.3 (12) |
O1viii—Na1—Na3vii | 124.81 (4) | Na53—Na52—Si2iii | 75 (7) |
O1—Na1—Na3vii | 50.11 (4) | Na5—Na52—Si2iii | 101.5 (4) |
O1vi—Na1—Na3vii | 133.81 (4) | Na53iii—Na52—Si2iii | 68 (2) |
O1ix—Na1—Na3vii | 114.51 (4) | O2xii—Na52—Si2iii | 131.7 (3) |
O1x—Na1—Na3vii | 51.30 (4) | O3iii—Na52—Si2iii | 33.12 (11) |
O1vii—Na1—Na3vii | 65.71 (4) | O5—Na52—Si2iii | 141.7 (5) |
Na3—Na1—Na3vii | 83.05 (4) | O6—Na52—Si2iii | 94.0 (2) |
O1viii—Na1—Na3ix | 51.30 (4) | Na52iii—Na52—Si2iii | 70.4 (4) |
O1—Na1—Na3ix | 133.81 (4) | O4iii—Na52—Si2iii | 34.07 (10) |
O1vi—Na1—Na3ix | 50.11 (4) | O4—Na52—Si2iii | 122.9 (5) |
O1ix—Na1—Na3ix | 65.71 (4) | Na52—Na53—Na51 | 11 (4) |
O1x—Na1—Na3ix | 124.81 (4) | Na52—Na53—Na53iii | 157 (9) |
O1vii—Na1—Na3ix | 114.51 (4) | Na51—Na53—Na53iii | 167 (9) |
Na3—Na1—Na3ix | 100.48 (2) | Na52—Na53—Na52iii | 151 (10) |
Na3vii—Na1—Na3ix | 175.56 (3) | Na51—Na53—Na52iii | 163 (7) |
O1viii—Na1—Na3x | 50.11 (4) | Na53iii—Na53—Na52iii | 8 (4) |
O1—Na1—Na3x | 124.81 (4) | Na52—Na53—O5 | 91 (8) |
O1vi—Na1—Na3x | 114.51 (4) | Na51—Na53—O5 | 86 (5) |
O1ix—Na1—Na3x | 133.81 (4) | Na53iii—Na53—O5 | 106 (9) |
O1x—Na1—Na3x | 65.71 (4) | Na52iii—Na53—O5 | 105 (5) |
O1vii—Na1—Na3x | 51.30 (4) | Na52—Na53—Na5 | 23 (5) |
Na3—Na1—Na3x | 100.48 (2) | Na51—Na53—Na5 | 12 (2) |
Na3vii—Na1—Na3x | 76.12 (3) | Na53iii—Na53—Na5 | 168 (9) |
Na3ix—Na1—Na3x | 100.48 (2) | Na52iii—Na53—Na5 | 170 (5) |
O1viii—Na1—Na3vi | 133.81 (4) | O5—Na53—Na5 | 85 (3) |
O1—Na1—Na3vi | 51.30 (4) | Na52—Na53—Na51iii | 154 (9) |
O1vi—Na1—Na3vi | 65.71 (4) | Na51—Na53—Na51iii | 165 (6) |
O1ix—Na1—Na3vi | 50.11 (4) | Na53iii—Na53—Na51iii | 6 (4) |
O1x—Na1—Na3vi | 114.51 (4) | Na52iii—Na53—Na51iii | 2.8 (7) |
O1vii—Na1—Na3vi | 124.81 (4) | O5—Na53—Na51iii | 103 (4) |
Na3—Na1—Na3vi | 76.12 (3) | Na5—Na53—Na51iii | 172 (4) |
Na3vii—Na1—Na3vi | 100.48 (2) | Na52—Na53—O3iii | 72 (7) |
Na3ix—Na1—Na3vi | 83.05 (4) | Na51—Na53—O3iii | 68 (4) |
Na3x—Na1—Na3vi | 175.56 (3) | Na53iii—Na53—O3iii | 107 (7) |
O1viii—Na1—Na3viii | 65.71 (4) | Na52iii—Na53—O3iii | 112 (4) |
O1—Na1—Na3viii | 114.51 (4) | O5—Na53—O3iii | 130 (4) |
O1vi—Na1—Na3viii | 124.81 (4) | Na5—Na53—O3iii | 61 (3) |
O1ix—Na1—Na3viii | 51.29 (4) | Na51iii—Na53—O3iii | 112 (4) |
O1x—Na1—Na3viii | 50.11 (4) | Na52—Na53—O6 | 80 (7) |
O1vii—Na1—Na3viii | 133.81 (4) | Na51—Na53—O6 | 69 (4) |
Na3—Na1—Na3viii | 175.56 (4) | Na53iii—Na53—O6 | 121 (3) |
Na3vii—Na1—Na3viii | 100.48 (2) | Na52iii—Na53—O6 | 128 (6) |
Na3ix—Na1—Na3viii | 76.12 (3) | O5—Na53—O6 | 65 (2) |
Na3x—Na1—Na3viii | 83.05 (4) | Na5—Na53—O6 | 58 (2) |
Na3vi—Na1—Na3viii | 100.48 (2) | Na51iii—Na53—O6 | 125 (5) |
O1xi—Na2—O1xii | 82.15 (5) | O3iii—Na53—O6 | 66 (2) |
O1xi—Na2—O1ix | 97.85 (5) | Na52—Na53—O4iii | 83 (8) |
O1xii—Na2—O1ix | 180.00 (8) | Na51—Na53—O4iii | 90 (5) |
O1xi—Na2—O1 | 180.0 | Na53iii—Na53—O4iii | 77 (6) |
O1xii—Na2—O1 | 97.85 (5) | Na52iii—Na53—O4iii | 76 (3) |
O1ix—Na2—O1 | 82.15 (5) | O5—Na53—O4iii | 165 (4) |
O1xi—Na2—O1iv | 82.14 (5) | Na5—Na53—O4iii | 95 (4) |
O1xii—Na2—O1iv | 82.14 (5) | Na51iii—Na53—O4iii | 78 (3) |
O1ix—Na2—O1iv | 97.86 (5) | O3iii—Na53—O4iii | 61.2 (19) |
O1—Na2—O1iv | 97.85 (5) | O6—Na53—O4iii | 127 (3) |
O1xi—Na2—O1x | 97.86 (5) | Na52—Na53—O4 | 101 (8) |
O1xii—Na2—O1x | 97.86 (5) | Na51—Na53—O4 | 107 (6) |
O1ix—Na2—O1x | 82.14 (5) | Na53iii—Na53—O4 | 75 (7) |
O1—Na2—O1x | 82.15 (5) | Na52iii—Na53—O4 | 68 (3) |
O1iv—Na2—O1x | 180.00 (8) | O5—Na53—O4 | 63 (2) |
O1xi—Na2—Na1xi | 49.34 (4) | Na5—Na53—O4 | 116 (4) |
O1xii—Na2—Na1xi | 49.35 (4) | Na51iii—Na53—O4 | 68 (3) |
O1ix—Na2—Na1xi | 130.65 (4) | O3iii—Na53—O4 | 164 (4) |
O1—Na2—Na1xi | 130.65 (4) | O6—Na53—O4 | 128 (3) |
O1iv—Na2—Na1xi | 49.35 (4) | O4iii—Na53—O4 | 105 (3) |
O1x—Na2—Na1xi | 130.65 (4) | Na52—Na53—Si2iii | 92 (8) |
O1xi—Na2—Na1 | 130.66 (4) | Na51—Na53—Si2iii | 93 (5) |
O1xii—Na2—Na1 | 130.65 (4) | Na53iii—Na53—Si2iii | 78 (7) |
O1ix—Na2—Na1 | 49.35 (4) | Na52iii—Na53—Si2iii | 81 (3) |
O1—Na2—Na1 | 49.35 (4) | O5—Na53—Si2iii | 159 (4) |
O1iv—Na2—Na1 | 130.65 (4) | Na5—Na53—Si2iii | 91 (3) |
O1x—Na2—Na1 | 49.35 (4) | Na51iii—Na53—Si2iii | 82 (3) |
Na1xi—Na2—Na1 | 180.0 | O3iii—Na53—Si2iii | 34.2 (10) |
O1xi—Na2—Na3vi | 131.65 (4) | O6—Na53—Si2iii | 96 (3) |
O1xii—Na2—Na3vi | 132.78 (4) | O4iii—Na53—Si2iii | 35.1 (10) |
O1ix—Na2—Na3vi | 47.22 (4) | O4—Na53—Si2iii | 136 (3) |
O1—Na2—Na3vi | 48.35 (4) | Si2—O1—Na3vii | 108.23 (8) |
O1iv—Na2—Na3vi | 73.48 (4) | Si2—O1—Na1 | 144.87 (9) |
O1x—Na2—Na3vi | 106.52 (4) | Na3vii—O1—Na1 | 78.38 (5) |
Na1xi—Na2—Na3vi | 122.822 (17) | Si2—O1—Na3vi | 99.07 (8) |
Na1—Na2—Na3vi | 57.178 (17) | Na3vii—O1—Na3vi | 152.51 (8) |
O1xi—Na2—Na3xiii | 48.35 (4) | Na1—O1—Na3vi | 77.44 (5) |
O1xii—Na2—Na3xiii | 47.22 (4) | Si2—O1—Na2 | 135.83 (9) |
O1ix—Na2—Na3xiii | 132.78 (4) | Na3vii—O1—Na2 | 81.79 (5) |
O1—Na2—Na3xiii | 131.65 (4) | Na1—O1—Na2 | 78.72 (5) |
O1iv—Na2—Na3xiii | 106.52 (4) | Na3vi—O1—Na2 | 80.84 (5) |
O1x—Na2—Na3xiii | 73.48 (4) | Si2—O1—Na3 | 77.97 (6) |
Na1xi—Na2—Na3xiii | 57.178 (17) | Na3vii—O1—Na3 | 96.04 (6) |
Na1—Na2—Na3xiii | 122.822 (17) | Na1—O1—Na3 | 66.96 (4) |
Na3vi—Na2—Na3xiii | 180.00 (4) | Na3vi—O1—Na3 | 86.38 (6) |
O1xi—Na2—Na3v | 106.52 (4) | Na2—O1—Na3 | 145.24 (6) |
O1xii—Na2—Na3v | 48.35 (4) | Si1—O2—Fe1xv | 131.94 (9) |
O1ix—Na2—Na3v | 131.65 (4) | Si1—O2—Na51iv | 114.3 (4) |
O1—Na2—Na3v | 73.48 (4) | Fe1xv—O2—Na51iv | 112.4 (4) |
O1iv—Na2—Na3v | 47.22 (4) | Si1—O2—Na4 | 105.88 (8) |
O1x—Na2—Na3v | 132.78 (4) | Fe1xv—O2—Na4 | 94.16 (6) |
Na1xi—Na2—Na3v | 57.178 (17) | Na51iv—O2—Na4 | 78.18 (17) |
Na1—Na2—Na3v | 122.822 (17) | Si1—O2—Na52iv | 101.7 (4) |
Na3vi—Na2—Na3v | 86.60 (2) | Fe1xv—O2—Na52iv | 125.4 (4) |
Na3xiii—Na2—Na3v | 93.40 (2) | Na51iv—O2—Na52iv | 13.1 (3) |
O1xi—Na2—Na3viii | 73.48 (4) | Na4—O2—Na52iv | 77.56 (16) |
O1xii—Na2—Na3viii | 131.65 (4) | Si1—O2—Na5xv | 140.62 (9) |
O1ix—Na2—Na3viii | 48.35 (4) | Fe1xv—O2—Na5xv | 84.65 (5) |
O1—Na2—Na3viii | 106.52 (4) | Na51iv—O2—Na5xv | 27.8 (4) |
O1iv—Na2—Na3viii | 132.78 (4) | Na4—O2—Na5xv | 81.11 (5) |
O1x—Na2—Na3viii | 47.22 (4) | Na52iv—O2—Na5xv | 40.9 (4) |
Na1xi—Na2—Na3viii | 122.822 (17) | Si1—O2—Na53iv | 91 (2) |
Na1—Na2—Na3viii | 57.178 (17) | Fe1xv—O2—Na53iv | 136 (2) |
Na3vi—Na2—Na3viii | 93.40 (2) | Na51iv—O2—Na53iv | 24 (2) |
Na3xiii—Na2—Na3viii | 86.60 (2) | Na4—O2—Na53iv | 81.2 (17) |
Na3v—Na2—Na3viii | 180.00 (4) | Na52iv—O2—Na53iv | 11 (2) |
O3—Na3—O1vii | 130.97 (7) | Na5xv—O2—Na53iv | 51 (2) |
O3—Na3—O5xiv | 106.96 (7) | Si2—O3—Fe1xv | 130.90 (9) |
O1vii—Na3—O5xiv | 95.39 (6) | Si2—O3—Na3 | 99.86 (8) |
O3—Na3—O1vi | 110.83 (6) | Fe1xv—O3—Na3 | 105.91 (7) |
O1vii—Na3—O1vi | 87.01 (8) | Si2—O3—Na51iii | 103.0 (4) |
O5xiv—Na3—O1vi | 126.84 (7) | Fe1xv—O3—Na51iii | 101.0 (2) |
O3—Na3—O1 | 59.56 (5) | Na3—O3—Na51iii | 117.5 (3) |
O1vii—Na3—O1 | 78.74 (6) | Si2—O3—Na52iii | 91.9 (3) |
O5xiv—Na3—O1 | 148.85 (6) | Fe1xv—O3—Na52iii | 103.89 (17) |
O1vi—Na3—O1 | 83.73 (6) | Na3—O3—Na52iii | 127.3 (3) |
O3—Na3—Na1 | 104.54 (5) | Na51iii—O3—Na52iii | 13.1 (3) |
O1vii—Na3—Na1 | 51.51 (4) | Si2—O3—Na5iii | 128.80 (8) |
O5xiv—Na3—Na1 | 144.98 (5) | Fe1xv—O3—Na5iii | 90.31 (6) |
O1vi—Na3—Na1 | 51.26 (4) | Na3—O3—Na5iii | 94.40 (6) |
O1—Na3—Na1 | 47.34 (3) | Na51iii—O3—Na5iii | 30.1 (4) |
O3—Na3—O4vii | 98.08 (6) | Na52iii—O3—Na5iii | 43.2 (4) |
O1vii—Na3—O4vii | 58.81 (5) | Si2—O3—Na53iii | 83 (2) |
O5xiv—Na3—O4vii | 57.09 (5) | Fe1xv—O3—Na53iii | 100 (2) |
O1vi—Na3—O4vii | 145.13 (6) | Na3—O3—Na53iii | 142 (3) |
O1—Na3—O4vii | 95.10 (5) | Na51iii—O3—Na53iii | 28 (3) |
Na1—Na3—O4vii | 103.72 (4) | Na52iii—O3—Na53iii | 15 (3) |
O3—Na3—Si2 | 31.43 (4) | Na5iii—O3—Na53iii | 57 (3) |
O1vii—Na3—Si2 | 100.66 (5) | Si2—O4—Si1xii | 133.26 (10) |
O5xiv—Na3—Si2 | 125.28 (5) | Si2—O4—Na4xx | 133.09 (9) |
O1vi—Na3—Si2 | 106.08 (5) | Si1xii—O4—Na4xx | 93.37 (7) |
O1—Na3—Si2 | 30.68 (3) | Si2—O4—Na53iii | 79.3 (19) |
Na1—Na3—Si2 | 78.01 (3) | Si1xii—O4—Na53iii | 117 (2) |
O4vii—Na3—Si2 | 88.36 (4) | Na4xx—O4—Na53iii | 83 (3) |
O3—Na3—Si2vi | 90.67 (5) | Si2—O4—Na52iii | 83.07 (15) |
O1vii—Na3—Si2vi | 117.68 (5) | Si1xii—O4—Na52iii | 124.6 (3) |
O5xiv—Na3—Si2vi | 116.49 (5) | Na4xx—O4—Na52iii | 71.0 (3) |
O1vi—Na3—Si2vi | 30.80 (4) | Na53iii—O4—Na52iii | 15 (3) |
O1—Na3—Si2vi | 92.76 (4) | Si2—O4—Na53 | 79 (2) |
Na1—Na3—Si2vi | 77.71 (2) | Si1xii—O4—Na53 | 96 (3) |
O4vii—Na3—Si2vi | 170.38 (5) | Na4xx—O4—Na53 | 104.2 (19) |
Si2—Na3—Si2vi | 101.22 (3) | Na53iii—O4—Na53 | 29 (6) |
O3—Na3—Na2viii | 160.58 (5) | Na52iii—O4—Na53 | 43 (3) |
O1vii—Na3—Na2viii | 50.99 (4) | Si2—O4—Na52 | 85.47 (15) |
O5xiv—Na3—Na2viii | 91.28 (5) | Si1xii—O4—Na52 | 83.2 (3) |
O1vi—Na3—Na2viii | 50.81 (4) | Na4xx—O4—Na52 | 108.8 (2) |
O1—Na3—Na2viii | 107.43 (4) | Na53iii—O4—Na52 | 41 (3) |
Na1—Na3—Na2viii | 60.240 (19) | Na52iii—O4—Na52 | 55.6 (6) |
O4vii—Na3—Na2viii | 97.44 (4) | Na53—O4—Na52 | 13 (3) |
Si2—Na3—Na2viii | 138.08 (3) | Si2—O4—Na51iii | 82.25 (14) |
Si2vi—Na3—Na2viii | 74.87 (2) | Si1xii—O4—Na51iii | 131.5 (2) |
O3—Na3—Si2vii | 117.06 (5) | Na4xx—O4—Na51iii | 65.63 (19) |
O1vii—Na3—Si2vii | 28.07 (4) | Na53iii—O4—Na51iii | 24 (3) |
O5xiv—Na3—Si2vii | 76.82 (5) | Na52iii—O4—Na51iii | 9.9 (3) |
O1vi—Na3—Si2vii | 114.97 (5) | Na53—O4—Na51iii | 53 (3) |
O1—Na3—Si2vii | 85.01 (4) | Na52—O4—Na51iii | 65.5 (5) |
Na1—Na3—Si2vii | 75.50 (2) | Si2—O4—Na3vii | 80.72 (6) |
O4vii—Na3—Si2vii | 30.79 (3) | Si1xii—O4—Na3vii | 83.96 (7) |
Si2—Na3—Si2vii | 94.32 (3) | Na4xx—O4—Na3vii | 103.29 (6) |
Si2vi—Na3—Si2vii | 145.35 (3) | Na53iii—O4—Na3vii | 157.6 (18) |
Na2viii—Na3—Si2vii | 72.91 (2) | Na52iii—O4—Na3vii | 150.6 (3) |
O3—Na3—Si1xiv | 98.52 (5) | Na53—O4—Na3vii | 152.5 (18) |
O1vii—Na3—Si1xiv | 81.26 (5) | Na52—O4—Na3vii | 146.0 (3) |
O5xiv—Na3—Si1xiv | 28.05 (4) | Na51iii—O4—Na3vii | 141.5 (3) |
O1vi—Na3—Si1xiv | 148.84 (5) | Si1—O5—Si2 | 131.09 (10) |
O1—Na3—Si1xiv | 121.54 (4) | Si1—O5—Na3v | 110.33 (8) |
Na1—Na3—Si1xiv | 131.54 (3) | Si2—O5—Na3v | 111.42 (8) |
O4vii—Na3—Si1xiv | 30.18 (3) | Si1—O5—Na53 | 92 (2) |
Si2—Na3—Si1xiv | 104.43 (3) | Si2—O5—Na53 | 90 (3) |
Si2vi—Na3—Si1xiv | 144.41 (4) | Na3v—O5—Na53 | 119 (3) |
Na2viii—Na3—Si1xiv | 100.76 (3) | Si1—O5—Na52 | 93.71 (18) |
Si2vii—Na3—Si1xiv | 56.05 (2) | Si2—O5—Na52 | 100.3 (4) |
O2—Na4—O2iii | 102.12 (9) | Na3v—O5—Na52 | 103.4 (4) |
O2—Na4—O6i | 112.10 (6) | Na53—O5—Na52 | 16 (3) |
O2iii—Na4—O6i | 67.32 (5) | Si1—O5—Na51 | 90.38 (19) |
O2—Na4—O6xv | 67.32 (5) | Si2—O5—Na51 | 111.1 (3) |
O2iii—Na4—O6xv | 112.11 (6) | Na3v—O5—Na51 | 93.6 (3) |
O6i—Na4—O6xv | 179.16 (10) | Na53—O5—Na51 | 28 (3) |
O2—Na4—O4xvi | 129.28 (5) | Na52—O5—Na51 | 12.3 (3) |
O2iii—Na4—O4xvi | 104.01 (5) | Si1—O5—Na53iii | 94.6 (19) |
O6i—Na4—O4xvi | 117.92 (6) | Si2—O5—Na53iii | 69 (2) |
O6xv—Na4—O4xvi | 62.74 (5) | Na3v—O5—Na53iii | 139.0 (16) |
O2—Na4—O4xvii | 104.01 (5) | Na53—O5—Na53iii | 25 (5) |
O2iii—Na4—O4xvii | 129.28 (5) | Na52—O5—Na53iii | 41 (2) |
O6i—Na4—O4xvii | 62.75 (5) | Na51—O5—Na53iii | 53 (2) |
O6xv—Na4—O4xvii | 117.91 (6) | Si1—O6—Fe1 | 150.31 (11) |
O4xvi—Na4—O4xvii | 91.74 (8) | Si1—O6—Na4ii | 99.35 (8) |
O2—Na4—Na51iv | 49.53 (13) | Fe1—O6—Na4ii | 94.26 (7) |
O2iii—Na4—Na51iv | 150.61 (15) | Si1—O6—Na51 | 97.1 (2) |
O6i—Na4—Na51iv | 112.2 (3) | Fe1—O6—Na51 | 100.09 (17) |
O6xv—Na4—Na51iv | 67.9 (3) | Na4ii—O6—Na51 | 116.8 (4) |
O4xvi—Na4—Na51iv | 101.6 (2) | Si1—O6—Na5 | 112.41 (9) |
O4xvii—Na4—Na51iv | 63.4 (2) | Fe1—O6—Na5 | 94.35 (6) |
O2—Na4—Na51xviii | 150.60 (15) | Na4ii—O6—Na5 | 87.45 (5) |
O2iii—Na4—Na51xviii | 49.53 (13) | Na51—O6—Na5 | 30.7 (4) |
O6i—Na4—Na51xviii | 67.9 (3) | Si1—O6—Na52 | 91.6 (2) |
O6xv—Na4—Na51xviii | 112.2 (3) | Fe1—O6—Na52 | 100.22 (15) |
O4xvi—Na4—Na51xviii | 63.4 (2) | Na4ii—O6—Na52 | 128.8 (4) |
O4xvii—Na4—Na51xviii | 101.6 (2) | Na51—O6—Na52 | 12.3 (3) |
Na51iv—Na4—Na51xviii | 159.6 (3) | Na5—O6—Na52 | 42.9 (4) |
O2—Na4—Na52iv | 51.37 (15) | Si1—O6—Na53 | 85 (2) |
O2iii—Na4—Na52iv | 146.93 (19) | Fe1—O6—Na53 | 99.8 (18) |
O6i—Na4—Na52iv | 101.8 (3) | Na4ii—O6—Na53 | 143 (3) |
O6xv—Na4—Na52iv | 78.4 (3) | Na51—O6—Na53 | 27 (3) |
O4xvi—Na4—Na52iv | 108.5 (2) | Na5—O6—Na53 | 58 (3) |
O4xvii—Na4—Na52iv | 56.4 (2) | Na52—O6—Na53 | 15 (3) |
Na51iv—Na4—Na52iv | 10.5 (2) | | |
Symmetry codes: (i) −x+4/3, −x+y+2/3, −z+1/6; (ii) −y+2/3, x−y−2/3, z+1/3; (iii) y+2/3, x−2/3, −z−1/6; (iv) x−y, x−1, −z; (v) −y+1, −x+1, z+1/2; (vi) x−y, −y, −z−1/2; (vii) −x+2, −x+y+1, −z−1/2; (viii) y+1, x−1, −z−1/2; (ix) −y+1, x−y−1, z; (x) −x+y+2, −x+1, z; (xi) −x+2, −y, −z; (xii) y+1, −x+y+1, −z; (xiii) −x+y+2, y, z+1/2; (xiv) −y+1, −x+1, z−1/2; (xv) −x+y+4/3, −x+2/3, z−1/3; (xvi) y+1/3, −x+y+2/3, −z−1/3; (xvii) −x+y+4/3, y−1/3, z+1/6; (xviii) x−1/3, x−y−2/3, z−1/6; (xix) −x+5/3, −y+1/3, −z+1/3; (xx) x−y+1/3, x−1/3, −z−1/3. |
Bond valence sums (valence units*) for Na5FeSi4O12 topAtoms | Fe1 | Si1 | Si2 | Na1 | Na2 | Na3 | Na4 | Na5 | Sum |
O1 | | | 1.10 | 0.20 ×6↓ | 0.16 ×6↓ | 0.22/0.20/0.05 | | | 1.92 |
O2 | 0.52 ×2↓ | 1.07 | | | | 0.04 | 0.19 ×2↓ | 0.08 ×2↓ | 2.06 |
O3 | 0.47 ×2↓ | | 1.04 | | | 0.23 | | 0.14 ×2↓ | 1.87 |
O4 | | 0.90 | 0.91 | | | 0.04 | 0.14 ×2↓ | | 1.96 |
O5 | | 0.94 | 0.90 | | | 0.22 | | | 2.06 |
O6 | 0.51 ×2↓ | 1.10 | | | | | 0.18 ×2↓ | 0.28 ×2↓ | 2.07 |
Sum | 3.00 | 4.01 | 3.95 | 1.18 | 0.95 | 0.99 | 1.03 | 1.01 | |
Note: (*) bond valence parameters are from Gagné & Hawthorne (2015).
BVS for disordered Na atoms (Na51, Na52 and Na53) are not included. These
disordered Na atoms contribute limited BV to atoms O2, O3, O4, O5
and O6, depending on site occupancy. |
Selected interatomic distances (Å) for Na5FeSi4O12 topFe1—O2 | 2.038 (2) | Na1—O1 | 2.377 (2) | Na4—O2 | 2.386 (2) | Na52—O2 | 2.396 (8) |
Fe1—O3 | 2.034 (2) | | | Na4—O4 | 2.516 (2) | Na52—O3 | 2.411 (9) |
Fe1–O6 | 2.002 (2) | Na2—O4 | 2.467 (2) | Na4—O6 | 2.413 (2) | Na52—O4 | 2.640 (11) |
<Fe1—O> | 2.025 | | | <Na4—O> | 2.438 | Na52—O4 | 2.862 (12) |
| | | | | | Na52—O5 | 2.445 (10) |
Si1—O2 | 1.597 (2) | Na3—O1 | 2.330 (2) | Na5—O2 | 2.738 (2) | Na52—O6 | 2.546 (15) |
Si1—O4 | 1.663 (2) | Na3—O1 | 2.378 (2) | Na5—O3 | 2.533 (2) | <Na52—O> | 2.550 |
Si1—O5 | 1.650 (1) | Na3—O1 | 2.946 (2) | Na5—O6 | 2.422 (1) | | |
Si1—O6 | 1.587 (2) | Na3—O2 | 3.097 (2) | <Na5—O> | 2.564 | Na53—O2 | 2.86 (11) |
<Si1—O> | 1.624 | Na3—O3 | 2.320 (2) | | | Na53–O3 | 2.53 (12) |
| | Na3—O4 | 3.020 (2) | Na51—O2 | 2.295 (8) | Na53—O4 | 2.63 (12) |
Si2—O1 | 1.587 (2) | Na3—O5 | 2.331 (2) | Na51–O3 | 2.359 (10) | Na53—O4 | 2.66 (12) |
Si2—O3 | 1.610 (2) | <Na3—O> | 2.632 | Na51—O4 | 2.899 (12) | Na53—O5 | 2.33 (13) |
Si2—O4 | 1.661 (1) | | | Na51—O5 | 2.552 (11) | Na53—O5 | 2.96 (13) |
Si2—O5 | 1.664 (2) | | | Na51—O6 | 2.414 (6) | Na53—O6 | 2.57 (10) |
<Si2—O> | 1.631 | | | <Na51—O> | 2.504 | <Na53—O> | 2.65 |
Refined occupancies: Na5 0.682 (7), Na51 0.144 (9), Na51 0.145 (10) and Na53
0.017 (7). |
Comparison of unit-cell parameters of Na5FeSi4O12 to analogues from
Shannon et al. (1978) (unless otherwise noted) topPhase | a (Å) | c (Å) | V (Å) |
Na5FeSi4O12 (this study) | 21.418 (3) | 12.291 (18) | 4883 |
Na5FeSi4O12 | 21.425 (2) | 12.300 (2) | 4889 |
Na5ScSi4O12 | 21.672 (3) | 12.437 (2) | 5058 |
Na5ScSi4O12 (Maximov et al., 1982) | 21.679 (6) | 12.446 (3) | 5066 |
Na5InSi4O12 | 21.725 (2) | 12.460 (2) | 5093 |
Na5LuSi4O12 | 21.920 (2) | 12.576 (2) | 5233 |
Na5YbSi4O12 | 21.940 (2) | 12.567 (2) | 5239 |
Na5TmSi4O12 | 21.958 (3) | 12.579 (2) | 5252 |
Na5ErSi4O12 | 21.989 (2) | 12.610 (2) | 5280 |
Na5HoSi4O12 | 22.034 (2) | 12.607 (2) | 5301 |
Na5YSi4O12 | 22.035 (1) | 12.604 (1) | 5300 |
Na5YSi4O12 (Maximov et al., 1982) | 22.062 (8) | 12.621 (4) | 5320 |
Na5DySi4O12 | 22.058 (2) | 12.623 (3) | 5319 |
Na5TbSi4O12 | 22.083 (1) | 12.627 (1) | 5332 |
Na5GdSi4O12 | 22.126 (5) | 12.650 (4) | 5363 |
Na5SmSi4O12 | 22.164 (4) | 12.661 (4) | 5386 |
xVBF fitting parameters for Mössbauer spectra of 5.1.8 glass and crystal topSample | Signal | CS1 ±0.02 (mm/s) | QS2 ±0.02 (mm/s) | Area ±2 (%) | Fit reduced χ2 |
Glass | Doublet 1 (Fe3+) | 0.26 | 0.85 | 90.1 | 0.614 |
| Doublet 2 (Fe2+) | 1.02 | 1.97 | 9.9 | |
Crystal | Singlet 1 (Fe3+) | 0.42 | | 100 | 0.852 |
Notes: (1) chemical Shift relative to α-Fe foil; (2) quadrupole splitting. |
Iron redox values determined from Mössbauer spectroscopy and wet
chemistry for 5.1.8 glass and crystal top | | | Glass | Crystal |
| Mössbauer Spectroscopy | | 0.901 | 1.000 |
Fe3+/ΣFe | Wet chemistry | Average | 0.927 | 0.994 |
| (triplicates) | Standard Deviation | 0.017 | 0.001 |
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