Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052519213017442/pi5015sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052519213017442/pi5015Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2052519213017442/pi5015sup3.pdf |
Data collection: CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46); cell refinement: CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46); data reduction: CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46); program(s) used to refine structure: Volkov et al., (2006); molecular graphics: Volkov et al., (2006); software used to prepare material for publication: Volkov et al., (2006).
H12Li4O12P2 | Mo Kα radiation, λ = 0.7107 Å |
Mr = 293.80 | Cell parameters from 41589 reflections |
Cubic, Ia3 | θ = 3.2–72.5° |
a = 12.700 (3) Å | µ = 0.48 mm−1 |
V = 2048.4 (8) Å3 | T = 85 K |
Z = 8.0 | Parallelepiped, colourless |
F(000) = 1200 | 0.35 × 0.22 × 0.21 mm |
Dx = 1.905 Mg m−3 |
Xcalibur, Onyx diffractometer | 3497 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 3178 reflections with > 3σ(I) |
Graphite monochromator | Rint = 0.039 |
Detector resolution: 8.1956 pixels mm-1 | θmax = 72.5°, θmin = 3.2° |
ω and π scans | h = −33→34 |
Absorption correction: analytical CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) | k = −34→32 |
Tmin = 0.885, Tmax = 0.919 | l = −27→31 |
103877 measured reflections |
Refinement on F | 0 restraints |
Least-squares matrix: full | w1 = [Fo*sqrt(w2) + sqrt(Fo2w22 + sqrt(w22))]2
where w2 = q/[s2(Fo2) + (0.00 P)2 + 2.50 P + 0.00 + 0.00 sin(th)] where P = (0.3333 Fo2 + 0.6667 Fc2) q = 1.0 |
R[F2 > 2σ(F2)] = 0.014 | (Δ/σ)max = 0.00001 |
wR(F2) = 0.013 | Δρmax = 0.32 e Å−3 |
S = 1.72 | Δρmin = −0.17 e Å−3 |
2884 reflections | Extinction correction: Becker-Coppens type 1 Gaussian isotropic, Becker, P.J. & Coppens, P. (1974) Acta Cryst., A30, 129-153. |
95 parameters | Extinction coefficient: 0.418 (18) |
H12Li4O12P2 | Z = 8.0 |
Mr = 293.80 | Mo Kα radiation |
Cubic, Ia3 | µ = 0.48 mm−1 |
a = 12.700 (3) Å | T = 85 K |
V = 2048.4 (8) Å3 | 0.35 × 0.22 × 0.21 mm |
Xcalibur, Onyx diffractometer | 3497 independent reflections |
Absorption correction: analytical CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) | 3178 reflections with > 3σ(I) |
Tmin = 0.885, Tmax = 0.919 | Rint = 0.039 |
103877 measured reflections |
R[F2 > 2σ(F2)] = 0.014 | 95 parameters |
wR(F2) = 0.013 | 0 restraints |
S = 1.72 | Δρmax = 0.32 e Å−3 |
2884 reflections | Δρmin = −0.17 e Å−3 |
x | y | z | Uiso*/Ueq | ||
P | 0.200353 (3) | 0.200353 (3) | 0.200353 (3) | 0.004 | |
O | 0.174504 (9) | 0.264039 (8) | 0.101346 (8) | 0.006 | |
O(W) | 0.431732 (11) | 0.149707 (10) | 0.051172 (10) | 0.008 | |
LI(1) | 0.25 | 0.34863 (4) | 0 | 0.01 | |
LI(2) | 0.5 | 0 | 0 | 0.011 | |
H(1) | 0.405447 | 0.19426 | −0.00944 | 0.026 (2) | |
H(2) | 0.366639 | 0.123312 | 0.091399 | 0.024 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
P | 0.003899 (19) | 0.003899 (19) | 0.003899 (19) | −0.000086 (6) | −0.000086 (6) | −0.000086 (6) |
O | 0.00747 (3) | 0.00639 (3) | 0.00513 (3) | 0.00026 (2) | −0.00052 (2) | 0.001072 (19) |
O(W) | 0.00742 (4) | 0.00807 (4) | 0.00721 (4) | 0.00006 (2) | −0.00002 (2) | 0.00034 (3) |
LI(1) | 0.01037 (17) | 0.00940 (17) | 0.00885 (16) | 0 | 0.00072 (13) | 0 |
LI(2) | 0.01128 (13) | 0.01128 (13) | 0.01128 (13) | 0.00010 (15) | −0.00010 (15) | 0.00010 (15) |
P—Pi | 2.1842 (1) | O(W)—H(1) | 1.0120 (1) |
P—O | 1.5307 (1) | O(W)—H(2) | 1.0280 (1) |
Pi—P—O | 107.039 (5) | Oii—P—Oiii | 111.790 (4) |
O—P—Oii | 111.790 (4) | H(1)—O(W)—H(2) | 107.162 (12) |
O—P—Oiii | 111.790 (4) |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+1/2; (ii) z, x, y; (iii) y, z, x. |
Experimental details
Crystal data | |
Chemical formula | H12Li4O12P2 |
Mr | 293.80 |
Crystal system, space group | Cubic, Ia3 |
Temperature (K) | 85 |
a (Å) | 12.700 (3) |
V (Å3) | 2048.4 (8) |
Z | 8.0 |
Radiation type | Mo Kα |
µ (mm−1) | 0.48 |
Crystal size (mm) | 0.35 × 0.22 × 0.21 |
Data collection | |
Diffractometer | Xcalibur, Onyx diffractometer |
Absorption correction | Analytical CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) |
Tmin, Tmax | 0.885, 0.919 |
No. of measured, independent and observed [ > 3σ(I)] reflections | 103877, 3497, 3178 |
Rint | 0.039 |
(sin θ/λ)max (Å−1) | 1.342 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.014, 0.013, 1.72 |
No. of reflections | 2884 |
No. of parameters | 95 |
Δρmax, Δρmin (e Å−3) | 0.32, −0.17 |
Computer programs: CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46), CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46), Volkov et al., (2006).
P—Pi | 2.1842 (1) | O(W)—H(1) | 1.0120 (1) |
P—O | 1.5307 (1) | O(W)—H(2) | 1.0280 (1) |
Pi—P—O | 107.039 (5) | Oii—P—Oiii | 111.790 (4) |
O—P—Oii | 111.790 (4) | H(1)—O(W)—H(2) | 107.162 (12) |
O—P—Oiii | 111.790 (4) |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+1/2; (ii) z, x, y; (iii) y, z, x. |