Achyrophanite, (K,Na)3(Fe3+,Ti,Al,Mg)5O2(AsO4)5, a New Mineral with the Novel Structure Type from Fumarolic Exhalations of the Tolbachik Volcano, Kamchatka, Russia
Abstract
1. Introduction
2. Occurrence and Mineral Association
3. Methods
4. Results
4.1. General Appearance and Physical Properties
4.2. Optical Data
4.3. Raman Spectroscopy
4.4. Chemical Data
4.5. X-Ray Crystallography and Crystal Structure
5. Discussion
5.1. Structure Description
5.2. Comparative Crystal Chemistry
5.3. Genetic Notes
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
References
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Constituent | Mean (for 8 Spot Analyses) | Range | Standard Deviation |
---|---|---|---|
Na2O | 3.68 | 3.41–3.92 | 0.20 |
K2O | 9.32 | 8.98–9.66 | 0.23 |
CaO | 0.38 | 0.30–0.44 | 0.05 |
MgO | 1.27 | 1.04–1.60 | 0.22 |
MnO | 0.08 | 0.06–0.11 | 0.02 |
CuO | 0.82 | 0.71–0.95 | 0.13 |
ZnO | 0.48 | 0.37–0.58 | 0.08 |
Al2O3 | 2.09 | 1.53–2.81 | 0.47 |
Fe2O3 * | 20.42 | 18.64–22.71 | 1.59 |
TiO2 | 7.35 | 6.60–7.96 | 0.55 |
SiO2 | 0.12 | 0.04–0.19 | 0.05 |
P2O5 | 0.14 | 0.04–0.20 | 0.05 |
V2O5 | 0.33 | 0.14–0.50 | 0.12 |
As2O5 | 51.88 | 50.61–54.25 | 1.17 |
SO3 | 1.04 | 0.21–1.91 | 0.70 |
Total | 99.40 |
Iobs | dobs | Icalc * | dcalc ** | h k l |
---|---|---|---|---|
5 | 13.21 | 13 | 13.249 | 010 |
2 | 8.36 | 8 | 8.353 | 011 |
9 | 6.62 | 8, 1 | 6.624, 6.582 | 020, 100 |
11 | 5.900 | 11 | 5.894 | 110 |
59 | 5.615 | 6, 88 | 5.641, 5.615 | 021, 101 |
9 | 5.376 | 10 | 5.381 | 002 |
4 | 4.980 | 2 | 4.985 | 012 |
3 | 4.683 | 1 | 4.669 | 120 |
3 | 4.417 | 1 | 4.416 | 030 |
1 | 4.278 | 1 | 4.283 | 121 |
42 | 4.174 | 41 | 4.177 | 022 |
2 | 4.077 | 1 | 4.086 | 031 |
3 | 3.972 | 2 | 3.974 | 112 |
31 | 3.669 | 39 | 3.667 | 130 |
6 | 3.527 | 5 | 3.527 | 122 |
4 | 3.469 | 3 | 3.471 | 131 |
14 | 3.413 | 13 | 3.414 | 032 |
6 | 3.315 | 1, 6 | 3.312, 3.291 | 040, 200 |
33 | 3.148 | 5, 37 | 3.154, 3.150 | 023, 103 |
8 | 3.064 | 1, 17 | 3.064, 3.062 | 113, 211 |
5 | 3.032 | 6 | 3.030 | 132 |
11 | 2.951 | 2, 17 | 2.959, 2.947 | 140, 220 |
43 | 2.852 | 45 | 2.853 | 141 |
100 | 2.814 | 61, 100 | 2.821, 2.808 | 042, 202 |
29 | 2.689 | 43 | 2.690 | 004 |
5 | 2.642 | 2, 4, 2 | 2.650, 2.639, 2.637 | 050, 230, 014 |
7 | 2.587 | 9 | 2.585 | 222 |
5 | 2.565 | 1, 9 | 2.564, 2.563 | 133, 231 |
1 | 2.490 | 1 | 2.490 | 104 |
2 | 2.443 | 1 | 2.447 | 114 |
1 | 2.398 | 1 | 2.396 | 151 |
1 | 2.371 | 1 | 2.369 | 232 |
2 | 2.296 | 2 | 2.298 | 034 |
2 | 2.284 | 3, 1 | 2.282, 2.282 | 143, 241 |
28 | 2.237 | 37 | 2.236 | 152 |
2 | 2.210 | 1 | 2.208 | 060 |
9 | 2.169 | 11, 1 | 2.169, 2.165 | 134, 310 |
2 | 2.144 | 1 | 2.142 | 242 |
6 | 2.127 | 8 | 2.126 | 233 |
4 | 2.087 | 3, 1, 1 | 2.088, 2.083, 2.083 | 044, 204, 320 |
4 | 2.041 | 3 | 2.046 | 105 |
5 | 2.029 | 9 | 2.027 | 251 |
5 | 2.009 | 4 | 2.008 | 312 |
1 | 1.929 | 2 | 1.927 | 252 |
2 | 1.884 | 2 | 1.884 | 234 |
3 | 1.873 | 6 | 1.872 | 303 |
5 | 1.847 | 12 | 1.846 | 332 |
2 | 1.834 | 3 | 1.834 | 260 |
10 | 1.815 | 1, 17 | 1.819, 1.815 | 170, 154 |
4 | 1.789 | 6, 3 | 1.789, 1.785 | 253, 215 |
17 | 1.764 | 31 | 1.763 | 244 |
6 | 1.739 | 8, 5 | 1.740, 1.736 | 145, 262 |
2 | 1.707 | 3 | 1.707 | 064 |
5 | 1.692 | 16, 2 | 1.690, 1.687 | 350, 314 |
2 | 1.667 | 2 | 1.668 | 235 |
4 | 1.658 | 1, 5 | 1.662, 1.656 | 036, 080 |
2 | 1.647 | 1, 10 | 1.647, 1.646 | 324, 400 |
2 | 1.631 | 4 | 1.630 | 343 |
2 | 1.614 | 3, 3, 1 | 1.615, 1.612, 1.611 | 411, 352, 136 |
7 | 1.585 | 6, 7 | 1.588, 1.583 | 181, 082 |
10 | 1.576 | 10, 17, 6 | 1.577, 1.575, 1.574 | 046, 206, 402 |
2 | 1.539 | 2, 1 | 1.539, 1.536 | 182, 305 |
1 | 1.530 | 3 | 1.526 | 431 |
2 | 1.515 | 3 | 1.515 | 264 |
2 | 1.509 | 2 | 1.507 | 174 |
3 | 1.495 | 6 | 1.497 | 107 |
3 | 1.481 | 1, 1, 4 | 1.483, 1.482, 1.479 | 236, 432, 280 |
4 | 1.467 | 7 | 1.466 | 183 |
3 | 1.449 | 12 | 1.449 | 156 |
4 | 1.438 | 6 | 1.437 | 190 |
8 | 1.432 | 27, 1 | 1.431, 1.428 | 354, 363 |
2 | 1.419 | 5, 4 | 1.421, 1.417 | 442, 433 |
2 | 1.405 | 5 | 1.404 | 404 |
2 | 1.393 | 4 | 1.394 | 345 |
3 | 1.388 | 3, 1, 3 | 1.388, 1.386, 1.385 | 192, 451, 372 |
2 | 1.374 | 5 | 1.373 | 424 |
Structural Formula | (K0.47Na0.47?0.06)2(K0.50?0.50)4(?0.75K0.25)4 (?0.94Ca0.03Na0.03)4(Fe0.48Ti0.30Al0.22)2 (Fe0.70Ti0.30)4(Fe0.36Mg0.28Al0.20Ti0.16)2(Fe0.74Mg0.05Na0.17Al0.04)2(?0.75Cu0.11Na0.08Zn0.06)2 (AsO4)8[(As0.68S0.32)O4]2[(?0.75As0.25)O0.5 (?0.75O0.25)2]2O3 |
Formula weight | 2171.74 |
Temperature, K | 293(2) |
Radiation and wavelength, Å | MoKα; 0.71073 |
Crystal system, space group, Z | Orthorhombic, P2221, 1 |
Unit-cell dimensions, Å/° | a = 6.5824(2) b = 13.2488(4) c = 10.7613(3) |
V, Å3 | 938.48(5) |
Absorption coefficient μ, mm−1 | 12.140 |
F000 | 1022 |
Crystal size, mm | 0.02 × 0.17 × 0.77 |
Diffractometer | Xcalibur S CCD |
θ range for data collection, °/Collection mode | 3.09–28.27/full sphere |
Index ranges | −8 ≤ h ≤ 8, −17 ≤ k ≤ 17, −14 ≤ l ≤ 14 |
Reflections collected | 15,862 |
Independent reflections | 2335 (Rint = 0.0626) |
Independent reflections with I > 2σ(I) | 2088 |
Data reduction | CrysAlisPro, Agilent Technologies (Oxfordshire, UK), v. 1.171.37.34 [10] |
Absorption correction | gaussian |
Structure solution | direct methods |
Refinement method | full-matrix least-squares on F2 |
Number of refined parameters | 190 |
Final R indices [I > 2σ(I)] | R1 = 0.0447, wR2 = 0.1065 |
R indices (all data) | R1 = 0.0507, wR2 = 0.1102 |
GoF | 1.089 |
Largest diff. peak and hole, e/Å3 | 1.76 and −1.59 |
Site | x | y | z | Ueq | s.o.f. | Q |
---|---|---|---|---|---|---|
A(1) | 0.6728(7) | 0.0 | 0.5 | 0.0545(15) | K0.47Na0.47 | 2 |
A(2) | 0.198(2) | 0.3889(8) | 0.828(2) | 0.035(4) | K0.25 | 4 |
A(3) | 0.2239(7) | 0.3724(5) | 0.9404(7) | 0.0472(17) | K0.50 | 4 |
A’ | 0.730(7) | 0.184(4) | 0.500(6) | 0.033(10) * | Ca0.03Na0.03 | 4 |
M(1) | 0.0 | 0.13054(17) | 0.75 | 0.0113(4) | Fe3+0.48Ti0.30Al0.22 | 2 |
M(2) | 0.24503(16) | 0.25063(9) | 0.50445(16) | 0.0082(2) | Fe3+0.70Ti0.30 | 4 |
M(3) | 0.5 | 0.39561(17) | 0.25 | 0.0077(5) | Fe3+0.36Mg0.28Al0.20Ti0.16 | 2 |
M(4) | 0.0 | 0.11671(15) | 0.25 | 0.0087(4) | Fe3+0.74Na0.17Mg0.05Al0.04 | 2 |
M’ | 0.5 | 0.6055(6) | 0.25 | 0.025(2) | Cu0.11Na0.08Zn0.06 | 2 |
T(1) | 0.5 | 0.18623(9) | 0.75 | 0.0084(2) | As1.00 | 2 |
T(2) | 0.18208(15) | 0.0 | 0.50 | 0.0070(2) | As1.00 | 2 |
T(3) | 0.31817(15) | 0.5 | 0.50 | 0.0088(2) | As1.00 | 2 |
T(4) | 0.0 | 0.32747(10) | 0.25 | 0.0087(3) | As0.68S0.32 ** | 2 |
T(5) | 0.5 | 0.18211(9) | 0.25 | 0.0084(2) | As1.00 | 2 |
T’ | 0.0 | 0.3259(4) | 0.75 | 0.0174(10) | As0.25 | 2 |
O(1) | 0.2967(10) | 0.1146(5) | 0.7845(6) | 0.0125(14) | O1.00 | 4 |
O(2) | 0.4763(10) | 0.4944(6) | 0.3774(5) | 0.0223(14) | O1.00 | 4 |
O(3) | 0.6994(11) | 0.1136(5) | 0.2905(5) | 0.0121(14) | O1.00 | 4 |
O(4) | 0.1940(8) | 0.3968(5) | 0.2086(6) | 0.0205(16) | O1.00 | 4 |
O(5) | 0.0245(8) | 0.0004(5) | 0.3750(4) | 0.0123(10) | O1.00 | 4 |
O(6) | 0.3291(8) | 0.1020(4) | 0.4949(7) | 0.0142(11) | O1.00 | 4 |
O(7) | 0.4531(10) | 0.2698(4) | 0.3642(6) | 0.0115(15) | O1.00 | 4 |
O(8) | 0.1699(8) | 0.3972(4) | 0.5045(8) | 0.0188(12) | O1.00 | 4 |
O(9) | 0.4580(10) | 0.2679(4) | 0.6306(5) | 0.0109(15) | O1.00 | 4 |
O(10) | 0.0404(9) | 0.2279(4) | 0.6294(5) | 0.0116(14) | O1.00 | 4 |
O(11) | 0.0396(13) | 0.2421(4) | 0.3606(5) | 0.029(2) | O1.00 | 4 |
O(12) | 0.175(8) | 0.405(3) | 0.799(8) | 0.035(4) | O0.25 | 4 |
T(1)—O(1) | 1.682(6) × 2 | T(4)—O(4) | 1.635(3) × 2 |
—O(9) | 1.702(6) × 2 | —O(11) | 1.663(3) × 2 |
T(2)—O(6) | 1.663(5) × 2 | T(5)—O(3) | 1.655(7) × 2 |
—O(5) | 1.698(5) × 2 | —O(7) | 1.719(6) × 2 |
T(3)—O(8) | 1.677(5) × 2 | M’—O(12) | 1.649(11) × 2 |
—O(2) | 1.682(6) × 2 | —O(10) | 1.855(4) × 2 |
M(1)—O(10) | 1.849(6) × 2 | M(3)—O(2) | 1.901(7) × 2 |
—O(1) | 1.999(7) × 2 | —O(4) | 2.063(6) × 2 |
—O(5) | 2.201(6) × 2 | —O(7) | 2.093(6) × 2 |
M(2)—O(10) | 1.927(6) | M(4)—O(3) | 2.026(7) × 2 |
—O(9) | 1.965(6) | —O(5) | 2.052(6) × 2 |
—O(8) | 2.004(6) | —O(11) | 2.060(7) × 2 |
—O(6) | 2.048(6) | ||
—O(7) | 2.054(6) | A(1)—O(6) | 2.636(7) × 2 |
—O(11) | 2.058(7) | —O(5) | 2.677(7) × 2 |
—O(3) | 2.716(6) × 2 | ||
M’—O(2) | 2.018(9) × 2 | —O(1) | 2.780(6) × 2 |
—O(9) | 2.131(9) × 2 | ||
—O(12) | 2.21(7) × 2 | A(2)—O(10) | 2.689(13) |
—O(2) | 2.695(12) | ||
A’—O(3) | 2.45(6) | —O(9) | 2.810(15) |
—O(1) | 2.50(6) | —O(12) | 2.82(3) |
—O(9) | 2.53(5) | —O(4) | 2.867(11) |
—O(10) | 2.54(5) | —O(8) | 3.02(3) |
—O(7) | 2.60(5) | ||
—O(11) | 2.64(5) | A(3)—O(9) | 2.624(8) |
—O(6) | 2.86(5) | —O(8) | 2.680(7) |
—O(10) | 2.695(8) | ||
—O(2) | 2.733(9) | ||
—O(4) | 2.911(10) |
T(1) | T(2) | T(3) | T(4) | T(5) | T’ 0.25 | M(1) | M(2) | M(3) | M(4) | M’ | A(1) | A(2) | A(3) | Σ | |
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
O(1) | 1.26 x2↓ | 0.52 ×2↓ | 0.11 ×2↓ | 1.89 | |||||||||||
O(2) | 1.26 ×2↓ | 0.64 ×2↓ | 0.11 ×2↓ | 0.05 | 0.10 | 2.16 | |||||||||
O(3) | 1.35 ×2↓ | 0.48 ×2↓ | 0.14 ×2↓ | 1.97 | |||||||||||
O(4) | 1.28 ×2↓ | 0.41 ×2↓ | 0.03 | 0.06 | 1.78 | ||||||||||
O(5) | 1.20 ×2↓ | 0.31 ×2↓ | 0.46 ×2↓ | 0.15 ×2↓ | 2.12 | ||||||||||
O(6) | 1.32 ×2↓ | 0.48 | 0.17 ×2↓ | 1.97 | |||||||||||
O(7) | 1.14 ×2↓ | 0.47 | 0.43 ×2↓ | 2.04 | |||||||||||
O(8) | 1.28 ×2↓ | 0.54 | 0.02 | 0.11 | 1.95 | ||||||||||
O(9) | 1.19 ×2↓ | 0.60 | 0.08 ×2↓ | 0.04 | 0.13 | 2.04 | |||||||||
O(10) | 0.20 ×2↓ | 0.78 ×2↓ | 0.66 | 0.06 | 0.11 | 1.81 | |||||||||
O(11) | 1.19 ×2↓ | 0.47 | 0.44 ×2↓ | 2.10 | |||||||||||
O(12) | 0.34 ×2↓ | 0.08 ×2↓ | 0.04 | 0.46 | |||||||||||
Σ | 4.90 | 5.04 | 5.08 | 4.94 * | 4.98 | 1.08 | 3.22 | 3.22 | 2.76 | 2.76 | 0.60 | 1.14 | 0.24 | 0.51 |
Mineral/ Compound | Achyrophanite | Synthetic Fe3+AsO4 | Katiarsite KTiO(AsO4) | Synthetic KTiO(AsO4) (KTA) | Synthetic (NH4)Fe3+(AsO4)F |
---|---|---|---|---|---|
Sp. gr. Unit cell a (Å) b (Å) c (Å) V (Å3) | P2221 6.5824(2) 13.2488(4) 10.7613(3) 938.48(5) | Imam 13.468(2) 6.525(1) 10.768(2) 946.3(3) | Pna21 13.174(4) 6.5635(10) 10.805(2) 934.3(3) | Pna21 13.1185(5) 6.5656(2) 10.7804(3) 928.5 | Pna21 13.270(2) 6.629(1) 10.866(1) 955.8(2) |
Reference | This work | [13,14] | [20] | [22] | [13,14] |
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Pekov, I.V.; Zubkova, N.V.; Koshlyakova, N.N.; Belakovskiy, D.I.; Vigasina, M.F.; Agakhanov, A.A.; Britvin, S.N.; Turchkova, A.G.; Sidorov, E.G.; Zhegunov, P.S.; et al. Achyrophanite, (K,Na)3(Fe3+,Ti,Al,Mg)5O2(AsO4)5, a New Mineral with the Novel Structure Type from Fumarolic Exhalations of the Tolbachik Volcano, Kamchatka, Russia. Minerals 2025, 15, 706. https://doi.org/10.3390/min15070706
Pekov IV, Zubkova NV, Koshlyakova NN, Belakovskiy DI, Vigasina MF, Agakhanov AA, Britvin SN, Turchkova AG, Sidorov EG, Zhegunov PS, et al. Achyrophanite, (K,Na)3(Fe3+,Ti,Al,Mg)5O2(AsO4)5, a New Mineral with the Novel Structure Type from Fumarolic Exhalations of the Tolbachik Volcano, Kamchatka, Russia. Minerals. 2025; 15(7):706. https://doi.org/10.3390/min15070706
Chicago/Turabian StylePekov, Igor V., Natalia V. Zubkova, Natalia N. Koshlyakova, Dmitry I. Belakovskiy, Marina F. Vigasina, Atali A. Agakhanov, Sergey N. Britvin, Anna G. Turchkova, Evgeny G. Sidorov, Pavel S. Zhegunov, and et al. 2025. "Achyrophanite, (K,Na)3(Fe3+,Ti,Al,Mg)5O2(AsO4)5, a New Mineral with the Novel Structure Type from Fumarolic Exhalations of the Tolbachik Volcano, Kamchatka, Russia" Minerals 15, no. 7: 706. https://doi.org/10.3390/min15070706
APA StylePekov, I. V., Zubkova, N. V., Koshlyakova, N. N., Belakovskiy, D. I., Vigasina, M. F., Agakhanov, A. A., Britvin, S. N., Turchkova, A. G., Sidorov, E. G., Zhegunov, P. S., & Pushcharovsky, D. Y. (2025). Achyrophanite, (K,Na)3(Fe3+,Ti,Al,Mg)5O2(AsO4)5, a New Mineral with the Novel Structure Type from Fumarolic Exhalations of the Tolbachik Volcano, Kamchatka, Russia. Minerals, 15(7), 706. https://doi.org/10.3390/min15070706