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The crystal structure of the new mineral aravaite Ba2Ca18(SiO4)6(PO4)3(CO3)F3O [R{\bar 3}m, a = 7.12550 (11), c = 66.2902 (13) Å, V = 2914.81 (8) Å3, Z = 3] was solved from single-crystal diffraction data, collected using synchrotron radiation at the X06DA beamline of the Swiss Light Source. The unit cell of this modular mineral contains six layers of {Ba(PO4)1.5(CO3)0.5}3.5− (T-layer), three triple antiperovskite layers (tAP) {(F2OCa12)(SiO4)4}4+, and three single antiperovskite layers (sAP) {(FCa6)(SiO4)2}3+. The structure refinement confirms a model with a layer sequence of T–sAP–T–tAP as an average structure of this mineral. However, one-dimensional diffuse scattering observed parallel to c* implies imperfections in the stacking sequence of the average structure. Qualitative modelling of disorder confirms that the alternating sequence of T–sAP and T–tAP blocks is disturbed. The blocks occurring in this new mineral are known from other so-called hexagonal intercalated antiperovskite structures: T–sAP (stracherite and zadovite group), T–tAP (ariegilatite and nabimusaite group).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520618012271/lo5031sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520618012271/lo5031Isup2.hkl
Contains datablock I

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052520618012271/lo5031sup3.pdf
Properties of aravaite

CCDC reference: 1864463

Computing details top

Data collection: Wojdyla, J. A.; Kaminski, J. W.; Panepucci, E.; Ebner, S.; Wang, X.; Gabadinho, J. & Wang, M. DA+ data acquisition and analysis software at the Swiss Light Source macromolecular crystallography beamlines Journal of Synchroton Radiation, 2018, 25 doi:10.1107/S1600577517014503; cell refinement: CrysAlis PRO 1.171.38.43 (Rigaku OD, 2015); data reduction: XDS Version 2016-11-01 Kabsch, W. Integration, scaling, space-group assignment and post refinement Acta Crystallographica, 2010, D66, 133-144; program(s) used to solve structure: SIR2004, Burla et al. 2005; program(s) used to refine structure: Jana2006 Version: 6/5/2017; molecular graphics: Vesta 3.

(I) top
Crystal data top
C0.919Ba2Ca17.621F3.462Na0.379O39.7P2.96Si6F(000) = 2854
Mr = 1961.8Dx = 3.353 Mg m3
Trigonal, R3mCell parameters from 2944 reflections
Hall symbol: -R 3;-2θ = 2.8–32.0°
a = 7.12550 (11) ŵ = 4.70 mm1
c = 66.2902 (13) ÅT = 293 K
V = 2914.81 (8) Å3Prism, black
Z = 30.06 × 0.03 × 0.03 mm
Data collection top
PRIGo
diffractometer
1291 independent reflections
Radiation source: SLS super-bending magnet 2.9T, X06DA1145 reflections with I > 3σ(I)
Bartels Monochromator with dual channel cut crystals (DCCM) in (±) geometry monochromatorRint = 0.049
Detector resolution: 5.81 pixels mm-1θmax = 32.0°, θmin = 0.9°
φ scansh = 89
Absorption correction: empirical (using intensity measurements)
XDS Version 2016-11-01 Kabsch, W. Integration, scaling, space-group assignment and post refinement Acta Crystallographica, 2010, D66, 133-144
k = 106
l = 8496
5677 measured reflections
Refinement top
Refinement on F20 restraints
R[F2 > 2σ(F2)] = 0.0820 constraints
wR(F2) = 0.184Weighting scheme based on measured s.u.'s w = 1/(σ2(I) + 0.0004I2)
S = 3.60(Δ/σ)max = 0.049
1291 reflectionsΔρmax = 12.08 e Å3
85 parametersΔρmin = 2.45 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ba1000.270337 (10)0.0140 (3)
Ca10.49749 (8)0.99499 (16)0.23253 (2)0.0066 (4)
Ca20.98845 (19)0.49422 (9)0.30918 (2)0.0086 (4)
Ca30.48954 (9)0.97909 (18)0.146883 (19)0.0058 (4)0.937 (12)
Na30.48954 (9)0.97909 (18)0.146883 (19)0.0058 (4)0.063 (12)
T10.6666670.3333330.19130 (4)0.0022 (5)
T20.3333330.6666670.34596 (4)0.0015 (5)*
T3000.21838 (4)0.0022 (5)
T40.6666670.3333330.26572 (5)0.0063 (8)0.940 (12)
T5p0.3333330.6666670.27450 (7)0.0071 (13)*0.54 (2)
T5c0.3333330.6666670.27450 (7)0.0071 (13)*0.46 (2)
O10.2223 (4)0.7777 (4)0.28273 (8)0.017 (2)0.865 (14)
O20.3333330.6666670.25243 (12)0.012 (2)
O30.4578 (4)0.9155 (7)0.35310 (8)0.0193 (16)
O40.6666670.3333330.28903 (12)0.0103 (19)
O50.5421 (3)0.0842 (7)0.18354 (7)0.0101 (8)*
O60.3333330.6666670.32173 (13)0.018 (2)
O70.6666670.3333330.21597 (11)0.0088 (19)
O80.7482 (6)0.8741 (3)0.22475 (7)0.0111 (14)
O90.7834 (3)0.2166 (3)0.25706 (6)0.0114 (14)
O10000.19203 (11)0.0031*
O110.3333330.6666670.1666670.002 (2)*0.53 (16)
F10.3333330.6666670.1666670.002 (2)*0.47 (16)
F20.6666670.3333330.3333330.013 (2)
F30.3333330.6666670.12406 (10)0.0082 (18)0.993 (19)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba10.0142 (3)0.0142 (3)0.0135 (4)0.00711 (16)00
Ca10.0017 (5)0.0015 (6)0.0164 (7)0.0008 (3)0.0007 (2)0.0014 (4)
Ca20.0033 (6)0.0028 (5)0.0201 (8)0.0016 (3)0.0010 (4)0.0005 (2)
Ca30.0023 (5)0.0034 (6)0.0119 (7)0.0017 (3)0.0006 (2)0.0012 (4)
Na30.0023 (5)0.0034 (6)0.0119 (7)0.0017 (3)0.0006 (2)0.0012 (4)
T10.0003 (5)0.0003 (5)0.0058 (9)0.0002 (3)00
T30.0003 (5)0.0003 (5)0.0058 (9)0.0002 (3)00
T40.0069 (10)0.0069 (10)0.0051 (14)0.0035 (5)00
O10.022 (2)0.022 (2)0.010 (3)0.013 (2)0.0006 (10)0.0006 (10)
O20.014 (2)0.014 (2)0.008 (4)0.0072 (12)00
O30.0065 (15)0.0035 (19)0.047 (3)0.0017 (10)0.0052 (10)0.010 (2)
O40.013 (2)0.013 (2)0.005 (4)0.0066 (11)00
O60.021 (3)0.021 (3)0.012 (4)0.0104 (14)00
O70.009 (2)0.009 (2)0.008 (4)0.0046 (11)00
O80.0023 (18)0.0063 (14)0.023 (3)0.0011 (9)0.0020 (16)0.0010 (8)
O90.0129 (15)0.0129 (15)0.012 (2)0.0092 (18)0.0013 (8)0.0013 (8)
F20.016 (3)0.016 (3)0.007 (4)0.0079 (14)00
F30.008 (2)0.008 (2)0.009 (3)0.0038 (10)00
Bond lengths (Å) top
Ba1—T2i3.339 (3)T1—O5xii1.621 (5)
Ba1—T33.444 (3)T1—O71.636 (8)
Ba1—O1ii2.864 (4)T1—O10xxii3.314 (8)
Ba1—O1iii2.864 (4)T2—O31.607 (5)
Ba1—O1iv2.864 (4)T2—O3iii1.607 (5)
Ba1—O3i3.251 (5)T2—O3ix1.607 (5)
Ba1—O3v3.251 (5)T2—O61.606 (9)
Ba1—O3vi3.251 (6)T3—O8vii1.610 (4)
Ba1—O8vii3.398 (5)T3—O8viii1.610 (5)
Ba1—O8viii3.398 (5)T3—O8ix1.610 (4)
Ba1—O8ix3.398 (5)T3—O101.747 (7)
Ba1—O9x2.815 (3)T4—O41.545 (8)
Ba1—O9xi2.815 (3)T4—O73.298 (8)
Ba1—O9xii2.815 (3)T4—O91.551 (3)
Ca1—T1xiii3.439 (3)T4—O9viii1.551 (3)
Ca1—T4xiii3.033 (2)T4—O9xii1.551 (3)
Ca1—T5p3.442 (4)T5p—T5c0
Ca1—T5c3.442 (4)T5p—O11.475 (4)
Ca1—O22.418 (4)T5p—O1iii1.475 (4)
Ca1—O5xiii3.294 (5)T5p—O1ix1.475 (4)
Ca1—O7xiii2.359 (4)T5p—O21.463 (9)
Ca1—O82.395 (5)T5p—O63.130 (10)
Ca1—O8iii2.395 (3)T5c—O11.475 (4)
Ca1—O9xiii2.464 (3)T5c—O1iii1.475 (4)
Ca1—O9xiv2.464 (4)T5c—O1ix1.475 (4)
Ca1—F3xv2.546 (4)T5c—O21.463 (9)
Ca2—Ca2viii3.4393 (17)T5c—O63.130 (10)
Ca2—Ca2xii3.4393 (12)O1—O1iii2.373 (6)
Ca2—T2xvi3.236 (2)O1—O1ix2.373 (6)
Ca2—T43.499 (3)O1—O22.431 (8)
Ca2—T5pxvi3.133 (3)O1—O3xxiv3.139 (6)
Ca2—T5cxvi3.133 (3)O1—O3xxv3.139 (7)
Ca2—O1xvi2.563 (4)O1—O62.926 (9)
Ca2—O1xvii2.563 (5)O1—O9xxvi3.199 (5)
Ca2—O3xvii2.971 (6)O1—O9xiv3.199 (5)
Ca2—O3xviii2.357 (7)O2—O83.150 (6)
Ca2—O3xix2.357 (6)O2—O8iii3.150 (7)
Ca2—O42.393 (4)O2—O8ix3.150 (6)
Ca2—O6xvi2.285 (3)O2—F3xv2.861 (10)
Ca2—F22.5507 (12)O3—O3iii2.660 (5)
Ca3—Ca3iii3.3392 (12)O3—O3ix2.660 (7)
Ca3—Ca3ix3.3392 (16)O3—O4xxvii3.048 (6)
Ca3—Ca3xv3.2552 (18)O3—O62.585 (9)
Ca3—Ca3xx3.2552 (15)O3—F2xiii2.892 (5)
Ca3—Na30O4—O92.563 (7)
Ca3—Na3iii3.3392 (12)O4—O9viii2.563 (7)
Ca3—Na3ix3.3392 (16)O4—O9xii2.563 (7)
Ca3—Na3xv3.2552 (18)O4—F22.937 (8)
Ca3—Na3xx3.2552 (15)O5—O5viii2.663 (5)
Ca3—T3xxi3.043 (2)O5—O5xii2.663 (6)
Ca3—O5xiii2.515 (5)O5—O5xxviii3.412 (7)
Ca3—O5xxii2.329 (5)O5—O5xx3.412 (5)
Ca3—O5xxiii2.329 (3)O5—O72.643 (7)
Ca3—O8xv2.616 (5)O5—O10xxii3.194 (7)
Ca3—O10xxi2.2170 (16)O5—O11ii2.809 (4)
Ca3—O112.3317 (12)O5—F1ii2.809 (4)
Ca3—F12.3317 (12)O5—F3xxix3.090 (6)
Ca3—F32.451 (4)O7—O93.081 (8)
Na3—Na3iii3.3392 (12)O7—O9viii3.081 (8)
Na3—Na3ix3.3392 (16)O7—O9xii3.081 (8)
Na3—Na3xv3.2552 (18)O8—O8xvii2.691 (6)
Na3—Na3xx3.2552 (15)O8—O8xiv2.691 (4)
Na3—T3xxi3.043 (2)O8—O9xiii3.162 (5)
Na3—O5xiii2.515 (5)O8—O9viii3.162 (6)
Na3—O5xxii2.329 (5)O8—O10xxx2.668 (7)
Na3—O5xxiii2.329 (3)O8—F3xv2.758 (5)
Na3—O8xv2.616 (5)O9—O9viii2.495 (5)
Na3—O10xxi2.2170 (16)O9—O9xii2.495 (5)
Na3—O112.3317 (12)O11—F10
Na3—F12.3317 (12)O11—F32.825 (6)
Na3—F32.451 (4)O11—F3xv2.825 (6)
T1—O51.621 (4)F1—F32.825 (6)
T1—O5viii1.621 (4)F1—F3xv2.825 (6)
Symmetry codes: (i) y2/3, x1/3, z+2/3; (ii) x, y1, z; (iii) y+1, xy+1, z; (iv) x+y1, x, z; (v) xy+1/3, y+2/3, z+2/3; (vi) x+1/3, x+y1/3, z+2/3; (vii) x1, y1, z; (viii) y+1, xy, z; (ix) x+y, x+1, z; (x) x1, y, z; (xi) y, xy1, z; (xii) x+y+1, x+1, z; (xiii) x, y+1, z; (xiv) x+y+1, x+2, z; (xv) y1/3, x+1/3, z+1/3; (xvi) x+1, y, z; (xvii) y+2, xy+1, z; (xviii) xy+4/3, y+5/3, z+2/3; (xix) x+4/3, x+y1/3, z+2/3; (xx) x+2/3, x+y+1/3, z+1/3; (xxi) y+2/3, x+4/3, z+1/3; (xxii) y+2/3, x+1/3, z+1/3; (xxiii) x+2/3, x+y+4/3, z+1/3; (xxiv) y2/3, x+2/3, z+2/3; (xxv) xy+1/3, y+5/3, z+2/3; (xxvi) y, xy, z; (xxvii) y+1/3, x+2/3, z+2/3; (xxviii) y+2/3, x2/3, z+1/3; (xxix) y1/3, x2/3, z+1/3; (xxx) x+1, y+1, z.
 

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