Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520617006102/pi5032sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520617006102/pi5032Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2052520617006102/pi5032sup3.pdf | |
Text file https://doi.org/10.1107/S2052520617006102/pi5032sup4.txt |
CCDC reference: 1545443
Program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: VALRAY2000 (Stewart, Spackman & Flensburg, 2000)'.
2(AL)3(MG)3(SIO4) | Mo Kα radiation, λ = 0.71073 Å |
Mr = 403.16 | Cell parameters from 406 reflections |
Cubic, Ia3d | θ = 11.0–53.5° |
a = 11.4405 (3) Å | µ = 1.22 mm−1 |
V = 1497.39 (12) Å3 | T = 30 K |
Z = 8 | Sphere, colourless |
F(000) = 1600 | 0.45 × 0.45 × 0.45 × 0.45 (radius) mm |
Dx = 3.576 Mg m−3 |
Syntex P1- diffractometer | Rint = 0.013 |
Graphite monochromator | θmax = 54.5°, θmin = 1.0° |
2θ/ω scans | h = 0→26 |
Absorption correction: for a sphere TBAR, home written program | k = 0→18 |
Tmin = 0.668, Tmax = 0.687 | l = 0→14 |
7486 measured reflections | 3 standard reflections every 97 reflections |
788 independent reflections | intensity decay: none |
785 reflections with > 0 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.008 | |
wR(F2) = 0.008 | (Δ/σ)max = 0.001 |
S = 0.76 | Δρmax = 0.12 e Å−3 |
785 reflections | Δρmin = −0.16 e Å−3 |
93 parameters | Extinction correction: type 1 |
0 restraints | Extinction coefficient: 0.248 |
Experimental. To determine the cell dimensions 406 reflections were centered in both negative and positive 2theta regions. A least-square fit to the resulting values of (sin(theta))**2 gave the reported cell parameters. |
Refinement. Refinement of F2 against ALL reflections. To adjust for the deviations from kinematic theory, the formalism of Becker and Coppens was used, assuming type I crystals and a Lorentzian "mosaic" distribution. |
x | y | z | Uiso*/Ueq | ||
Al1 | 0.0000 | 0.0000 | 0.0000 | 0.00217 | |
Mg1 | 0.0000 | 0.2500 | 0.1250 | 0.00423 | |
Si1 | 0.0000 | 0.2500 | 0.3750 | 0.00171 | |
O1 | 0.03282 (3) | 0.05077 (3) | 0.65326 (3) | 0.00319 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Al1 | 0.00217 (4) | 0.00217 (4) | 0.00217 (4) | 0.00001 (2) | 0.00001 (2) | 0.00001 (2) |
Mg1 | 0.00485 (7) | 0.00485 (7) | 0.00298 (8) | 0.00096 (5) | 0.0000 | 0.0000 |
Si1 | 0.00180 (2) | 0.00180 (2) | 0.00153 (2) | 0.0000 | 0.0000 | 0.0000 |
O1 | 0.00321 (4) | 0.00375 (4) | 0.00261 (4) | 0.00040 (2) | −0.00057 (2) | 0.00009 (2) |
Al1—O1i | 1.8848 (3) | Mg1—O1v | 2.3326 (4) |
Al1—O1ii | 1.8848 (3) | Mg1—O1xvi | 2.3326 (4) |
Al1—O1iii | 1.8848 (3) | Mg1—O1xvii | 2.3326 (4) |
Al1—O1iv | 1.8848 (3) | Mg1—Si1 | 2.8601 (1) |
Al1—O1v | 1.8848 (3) | Mg1—Si1v | 2.8601 (1) |
Al1—O1vi | 1.8848 (3) | Mg1—Al1xviii | 3.1977 (1) |
Al1—Mg1vii | 3.1977 (1) | Mg1—Al1xix | 3.1977 (1) |
Al1—Mg1viii | 3.1977 (1) | Si1—O1xx | 1.6354 (4) |
Al1—Mg1ix | 3.1977 (1) | Si1—O1xiii | 1.6354 (4) |
Al1—Mg1x | 3.1977 (1) | Si1—O1xxi | 1.6354 (4) |
Al1—Mg1xi | 3.1977 (1) | Si1—O1xii | 1.6354 (4) |
Al1—Mg1 | 3.1977 (1) | Si1—Mg1xvi | 2.8601 (1) |
Mg1—O1xii | 2.1960 (4) | O1—Si1xxii | 1.6354 (4) |
Mg1—O1xiii | 2.1960 (4) | O1—Al1vi | 1.8848 (3) |
Mg1—O1iii | 2.1960 (4) | O1—Mg1xxii | 2.1960 (4) |
Mg1—O1xiv | 2.1960 (4) | O1—Mg1xvi | 2.3326 (4) |
Mg1—O1xv | 2.3326 (4) | ||
O1i—Al1—O1ii | 180.0 (2) | O1xiii—Mg1—O1v | 93.640 (10) |
O1i—Al1—O1iii | 87.70 (2) | O1iii—Mg1—O1v | 70.370 (10) |
O1ii—Al1—O1iii | 92.30 (2) | O1xiv—Mg1—O1v | 124.330 (10) |
O1i—Al1—O1iv | 92.30 (2) | O1xv—Mg1—O1v | 164.080 (10) |
O1ii—Al1—O1iv | 87.70 (2) | O1xii—Mg1—O1xvi | 124.330 (10) |
O1iii—Al1—O1iv | 180.0 (2) | O1xiii—Mg1—O1xvi | 70.370 (10) |
O1i—Al1—O1v | 87.70 (2) | O1iii—Mg1—O1xvi | 93.640 (10) |
O1ii—Al1—O1v | 92.30 (2) | O1xiv—Mg1—O1xvi | 73.070 (10) |
O1iii—Al1—O1v | 87.70 (2) | O1xv—Mg1—O1xvi | 109.490 (10) |
O1iv—Al1—O1v | 92.30 (2) | O1v—Mg1—O1xvi | 72.830 (10) |
O1i—Al1—O1vi | 92.30 (2) | O1xii—Mg1—O1xvii | 70.370 (10) |
O1ii—Al1—O1vi | 87.70 (2) | O1xiii—Mg1—O1xvii | 124.330 (10) |
O1iii—Al1—O1vi | 92.30 (2) | O1iii—Mg1—O1xvii | 73.070 (10) |
O1iv—Al1—O1vi | 87.70 (2) | O1xiv—Mg1—O1xvii | 93.640 (10) |
O1v—Al1—O1vi | 180.0 (2) | O1xv—Mg1—O1xvii | 72.830 (10) |
O1i—Al1—Mg1vii | 87.690 (10) | O1v—Mg1—O1xvii | 109.490 (10) |
O1ii—Al1—Mg1vii | 92.310 (10) | O1xvi—Mg1—O1xvii | 164.080 (10) |
O1iii—Al1—Mg1vii | 137.990 (10) | O1xii—Mg1—Si1 | 34.700 (10) |
O1iv—Al1—Mg1vii | 42.010 (10) | O1xiii—Mg1—Si1 | 34.700 (10) |
O1v—Al1—Mg1vii | 133.770 (10) | O1iii—Mg1—Si1 | 145.300 (10) |
O1vi—Al1—Mg1vii | 46.230 (10) | O1xiv—Mg1—Si1 | 145.300 (10) |
O1i—Al1—Mg1viii | 133.770 (10) | O1xv—Mg1—Si1 | 82.040 (9) |
O1ii—Al1—Mg1viii | 46.230 (10) | O1v—Mg1—Si1 | 82.040 (9) |
O1iii—Al1—Mg1viii | 87.690 (10) | O1xvi—Mg1—Si1 | 97.960 (8) |
O1iv—Al1—Mg1viii | 92.310 (10) | O1xvii—Mg1—Si1 | 97.960 (8) |
O1v—Al1—Mg1viii | 137.990 (10) | O1xii—Mg1—Si1v | 145.300 (10) |
O1vi—Al1—Mg1viii | 42.010 (10) | O1xiii—Mg1—Si1v | 145.300 (10) |
Mg1vii—Al1—Mg1viii | 66.4220 (10) | O1iii—Mg1—Si1v | 34.700 (10) |
O1i—Al1—Mg1ix | 46.230 (10) | O1xiv—Mg1—Si1v | 34.700 (10) |
O1ii—Al1—Mg1ix | 133.770 (10) | O1xv—Mg1—Si1v | 97.960 (9) |
O1iii—Al1—Mg1ix | 92.310 (10) | O1v—Mg1—Si1v | 97.960 (9) |
O1iv—Al1—Mg1ix | 87.690 (10) | O1xvi—Mg1—Si1v | 82.040 (9) |
O1v—Al1—Mg1ix | 42.010 (10) | O1xvii—Mg1—Si1v | 82.040 (9) |
O1vi—Al1—Mg1ix | 137.990 (10) | Si1—Mg1—Si1v | 180.0 |
Mg1vii—Al1—Mg1ix | 113.5780 (10) | O1xii—Mg1—Al1xviii | 35.060 (10) |
Mg1viii—Al1—Mg1ix | 180.000 | O1xiii—Mg1—Al1xviii | 94.780 (10) |
O1i—Al1—Mg1x | 137.990 (10) | O1iii—Mg1—Al1xviii | 97.530 (10) |
O1ii—Al1—Mg1x | 42.010 (10) | O1xiv—Mg1—Al1xviii | 127.180 (10) |
O1iii—Al1—Mg1x | 133.770 (10) | O1xv—Mg1—Al1xviii | 78.112 (9) |
O1iv—Al1—Mg1x | 46.230 (10) | O1v—Mg1—Al1xviii | 94.702 (9) |
O1v—Al1—Mg1x | 87.690 (10) | O1xvi—Mg1—Al1xviii | 159.386 (9) |
O1vi—Al1—Mg1x | 92.310 (10) | O1xvii—Mg1—Al1xviii | 35.707 (9) |
Mg1vii—Al1—Mg1x | 66.4220 (10) | Si1—Mg1—Al1xviii | 63.4350 (10) |
Mg1viii—Al1—Mg1x | 66.4220 (10) | Si1v—Mg1—Al1xviii | 116.5650 (10) |
Mg1ix—Al1—Mg1x | 113.5780 (10) | O1xii—Mg1—Al1xix | 94.780 (10) |
O1i—Al1—Mg1xi | 42.010 (10) | O1xiii—Mg1—Al1xix | 35.060 (10) |
O1ii—Al1—Mg1xi | 137.990 (10) | O1iii—Mg1—Al1xix | 127.180 (10) |
O1iii—Al1—Mg1xi | 46.230 (10) | O1xiv—Mg1—Al1xix | 97.530 (10) |
O1iv—Al1—Mg1xi | 133.770 (10) | O1xv—Mg1—Al1xix | 94.702 (9) |
O1v—Al1—Mg1xi | 92.310 (10) | O1v—Mg1—Al1xix | 78.112 (9) |
O1vi—Al1—Mg1xi | 87.690 (10) | O1xvi—Mg1—Al1xix | 35.707 (9) |
Mg1vii—Al1—Mg1xi | 113.5780 (10) | O1xvii—Mg1—Al1xix | 159.386 (9) |
Mg1viii—Al1—Mg1xi | 113.5780 (10) | Si1—Mg1—Al1xix | 63.4350 (10) |
Mg1ix—Al1—Mg1xi | 66.4220 (10) | Si1v—Mg1—Al1xix | 116.5650 (10) |
Mg1x—Al1—Mg1xi | 180.000 | Al1xviii—Mg1—Al1xix | 126.870 (2) |
O1i—Al1—Mg1 | 92.310 (10) | O1xx—Si1—O1xiii | 114.57 (2) |
O1ii—Al1—Mg1 | 87.690 (10) | O1xx—Si1—O1xxi | 99.69 (2) |
O1iii—Al1—Mg1 | 42.010 (10) | O1xiii—Si1—O1xxi | 114.57 (2) |
O1iv—Al1—Mg1 | 137.990 (10) | O1xx—Si1—O1xii | 114.57 (2) |
O1v—Al1—Mg1 | 46.230 (10) | O1xiii—Si1—O1xii | 99.69 (2) |
O1vi—Al1—Mg1 | 133.770 (10) | O1xxi—Si1—O1xii | 114.57 (2) |
Mg1vii—Al1—Mg1 | 180.000 | O1xx—Si1—Mg1 | 130.150 (10) |
Mg1viii—Al1—Mg1 | 113.5780 (10) | O1xiii—Si1—Mg1 | 49.850 (10) |
Mg1ix—Al1—Mg1 | 66.4220 (10) | O1xxi—Si1—Mg1 | 130.150 (10) |
Mg1x—Al1—Mg1 | 113.5780 (10) | O1xii—Si1—Mg1 | 49.850 (10) |
Mg1xi—Al1—Mg1 | 66.4220 (10) | O1xx—Si1—Mg1xvi | 49.850 (10) |
O1xii—Mg1—O1xiii | 69.390 (10) | O1xiii—Si1—Mg1xvi | 130.150 (10) |
O1xii—Mg1—O1iii | 114.1670 (10) | O1xxi—Si1—Mg1xvi | 49.850 (10) |
O1xiii—Mg1—O1iii | 160.490 (10) | O1xii—Si1—Mg1xvi | 130.150 (10) |
O1xii—Mg1—O1xiv | 160.490 (10) | Mg1—Si1—Mg1xvi | 180.000 |
O1xiii—Mg1—O1xiv | 114.170 (10) | Si1xxii—O1—Al1vi | 130.43 (2) |
O1iii—Mg1—O1xiv | 69.390 (10) | Si1xxii—O1—Mg1xxii | 95.45 (2) |
O1xii—Mg1—O1xv | 93.640 (10) | Al1vi—O1—Mg1xxii | 102.93 (2) |
O1xiii—Mg1—O1xv | 73.070 (10) | Si1xxii—O1—Mg1xvi | 122.99 (2) |
O1iii—Mg1—O1xv | 124.330 (10) | Al1vi—O1—Mg1xvi | 98.07 (2) |
O1xiv—Mg1—O1xv | 70.370 (10) | Mg1xxii—O1—Mg1xvi | 101.31 (2) |
O1xii—Mg1—O1v | 73.070 (10) |
Symmetry codes: (i) z−1/2, −x, y; (ii) −z+1/2, x, −y; (iii) y, z−1/2, −x; (iv) −y, −z+1/2, x; (v) −x, y, z−1/2; (vi) x, −y, −z+1/2; (vii) −x, −y, −z; (viii) z−1/4, −y+1/4, −x−1/4; (ix) −z+1/4, y−1/4, x+1/4; (x) −x−1/4, z−1/4, −y+1/4; (xi) x+1/4, −z+1/4, y−1/4; (xii) −z+3/4, −y+1/4, x+1/4; (xiii) z−3/4, y+1/4, x+1/4; (xiv) −y, −z+1, −x; (xv) x, −y+1/2, z−1/2; (xvi) y−1/4, −x+1/4, −z+3/4; (xvii) −y+1/4, x+1/4, −z+3/4; (xviii) −y+1/4, −x+1/4, −z+1/4; (xix) x−1/4, z+1/4, −y+1/4; (xx) y, −z+1, −x+1/2; (xxi) −y, z−1/2, −x+1/2; (xxii) z−1/4, −y+1/4, −x+3/4. |