Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807007507/fi2029sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807007507/fi2029Isup2.hkl |
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: SCXmini Benchtop Crystallography System Software (Rigaku, 2006); data reduction: CrystalStructure (Rigaku, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SCXmini Benchtop Crystallography System Software; software used to prepare material for publication: CrystalStructure.
LiNi0.66Fe0.34PO4 | F(000) = 416 |
Mr = 159.63 | Dx = 3.815 Mg m−3 Dm = 3.749 Mg m−3 Dm measured by floatation |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71075 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 50 reflections |
a = 10.0871 (16) Å | θ = 1.0–27.5° |
b = 5.8845 (10) Å | µ = 6.84 mm−1 |
c = 4.6820 (8) Å | T = 150 K |
V = 277.91 (8) Å3 | Block, dark amber-brown |
Z = 4 | 0.19 × 0.18 × 0.14 mm |
Rigaku SCXmini diffractometer | 345 independent reflections |
Radiation source: fine-focus sealed tube | 328 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
Detector resolution: 4900 pixels mm-1 | θmax = 27.5°, θmin = 4.0° |
data collected from ω scans | h = −13→12 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −7→7 |
Tmin = 0.568, Tmax = 0.692 | l = −6→5 |
2026 measured reflections |
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)] = 0.020 | w = 1/[σ2(Fo2) + (0.0162P)2 + 0.3281P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.044 | (Δ/σ)max < 0.001 |
S = 1.18 | Δρmax = 0.37 e Å−3 |
345 reflections | Δρmin = −0.47 e Å−3 |
43 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.055 (4) |
Experimental. high-temperature flux |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ni1 | 0.27649 (4) | 0.2500 | −0.01877 (8) | 0.0034 (2) | 0.66 |
Fe1 | 0.27649 (4) | 0.2500 | −0.01877 (8) | 0.0034 (2) | 0.34 |
P1 | 0.09411 (8) | 0.2500 | 0.41781 (17) | 0.0041 (2) | |
O1 | 0.0988 (2) | 0.2500 | 0.7429 (5) | 0.0058 (5) | |
O2 | 0.4521 (2) | 0.2500 | 0.2019 (5) | 0.0051 (5) | |
O3 | 0.16550 (14) | 0.0433 (3) | 0.2782 (3) | 0.0058 (4) | |
Li1 | 0.0000 | 0.0000 | 0.0000 | 0.0050 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0031 (3) | 0.0022 (3) | 0.0048 (3) | 0.000 | −0.00022 (14) | 0.000 |
Fe1 | 0.0031 (3) | 0.0022 (3) | 0.0048 (3) | 0.000 | −0.00022 (14) | 0.000 |
P1 | 0.0040 (4) | 0.0033 (4) | 0.0049 (4) | 0.000 | 0.0003 (3) | 0.000 |
O1 | 0.0061 (11) | 0.0050 (10) | 0.0063 (11) | 0.000 | −0.0006 (9) | 0.000 |
O2 | 0.0043 (11) | 0.0043 (10) | 0.0067 (11) | 0.000 | 0.0005 (9) | 0.000 |
O3 | 0.0070 (8) | 0.0044 (7) | 0.0060 (7) | 0.0007 (6) | 0.0014 (6) | 0.0001 (5) |
Li1 | 0.006 (3) | 0.005 (2) | 0.004 (3) | −0.004 (2) | −0.0009 (18) | −0.0013 (18) |
Ni1—O2 | 2.051 (2) | O1—Li1vi | 2.1464 (16) |
Ni1—O3i | 2.0557 (15) | O2—P1vii | 1.538 (2) |
Ni1—O3ii | 2.0557 (15) | O2—Li1viii | 2.0844 (15) |
Ni1—O1iii | 2.111 (2) | O2—Li1ix | 2.0844 (15) |
Ni1—O3iv | 2.1599 (15) | O3—Fe1x | 2.0557 (15) |
Ni1—O3 | 2.1600 (15) | O3—Ni1x | 2.0557 (15) |
Ni1—P1 | 2.7501 (10) | O3—Li1 | 2.1327 (15) |
Ni1—Li1 | 3.1544 (5) | Li1—O2v | 2.0844 (15) |
Ni1—Li1iv | 3.1544 (5) | Li1—O2xi | 2.0844 (15) |
P1—O1 | 1.523 (2) | Li1—O3xii | 2.1327 (15) |
P1—O2v | 1.538 (2) | Li1—O1xiii | 2.1464 (16) |
P1—O3iv | 1.5572 (16) | Li1—O1iii | 2.1464 (16) |
P1—O3 | 1.5572 (16) | Li1—P1xii | 2.6253 (7) |
P1—Li1 | 2.6253 (7) | Li1—Li1iv | 2.9423 (5) |
P1—Li1iv | 2.6253 (7) | Li1—Li1xiv | 2.9423 (5) |
O1—Fe1vi | 2.111 (2) | Li1—Ni1xii | 3.1544 (5) |
O1—Ni1vi | 2.111 (2) | Li1—Fe1xii | 3.1544 (5) |
O2—Ni1—O3i | 89.26 (5) | Fe1x—O3—Ni1x | 0.000 (19) |
O2—Ni1—O3ii | 89.26 (5) | P1—O3—Li1 | 89.30 (7) |
O3i—Ni1—O3ii | 114.22 (9) | Fe1x—O3—Li1 | 113.88 (7) |
O2—Ni1—O1iii | 178.34 (8) | Ni1x—O3—Li1 | 113.88 (7) |
O3i—Ni1—O1iii | 89.84 (5) | P1—O3—Ni1 | 94.03 (7) |
O3ii—Ni1—O1iii | 89.84 (5) | Fe1x—O3—Ni1 | 128.53 (7) |
O2—Ni1—O3iv | 97.09 (6) | Ni1x—O3—Ni1 | 128.53 (7) |
O3i—Ni1—O3iv | 156.63 (7) | Li1—O3—Ni1 | 94.59 (6) |
O3ii—Ni1—O3iv | 88.42 (4) | O2v—Li1—O2xi | 180.00 (9) |
O1iii—Ni1—O3iv | 84.28 (6) | O2v—Li1—O3 | 71.82 (7) |
O2—Ni1—O3 | 97.09 (6) | O2xi—Li1—O3 | 108.18 (7) |
O3i—Ni1—O3 | 88.42 (4) | O2v—Li1—O3xii | 108.18 (7) |
O3ii—Ni1—O3 | 156.63 (7) | O2xi—Li1—O3xii | 71.82 (7) |
O1iii—Ni1—O3 | 84.28 (6) | O3—Li1—O3xii | 180.0 |
O3iv—Ni1—O3 | 68.53 (8) | O2v—Li1—O1xiii | 90.04 (6) |
O2—Ni1—P1 | 101.74 (6) | O2xi—Li1—O1xiii | 89.96 (6) |
O3i—Ni1—P1 | 122.29 (4) | O3—Li1—O1xiii | 95.91 (7) |
O3ii—Ni1—P1 | 122.29 (4) | O3xii—Li1—O1xiii | 84.09 (7) |
O1iii—Ni1—P1 | 79.92 (6) | O2v—Li1—O1iii | 89.96 (6) |
O3iv—Ni1—P1 | 34.39 (4) | O2xi—Li1—O1iii | 90.04 (6) |
O3—Ni1—P1 | 34.39 (4) | O3—Li1—O1iii | 84.09 (7) |
O2—Ni1—Li1 | 138.57 (4) | O3xii—Li1—O1iii | 95.91 (7) |
O3i—Ni1—Li1 | 82.70 (4) | O1xiii—Li1—O1iii | 180.00 (10) |
O3ii—Ni1—Li1 | 131.01 (4) | O2v—Li1—P1 | 35.84 (6) |
O1iii—Ni1—Li1 | 42.62 (4) | O2xi—Li1—P1 | 144.16 (6) |
O3iv—Ni1—Li1 | 77.66 (4) | O3—Li1—P1 | 36.38 (4) |
O3—Ni1—Li1 | 42.37 (4) | O3xii—Li1—P1 | 143.62 (4) |
P1—Ni1—Li1 | 52.252 (16) | O1xiii—Li1—P1 | 97.70 (5) |
O2—Ni1—Li1iv | 138.57 (4) | O1iii—Li1—P1 | 82.30 (5) |
O3i—Ni1—Li1iv | 131.01 (4) | O2v—Li1—P1xii | 144.16 (6) |
O3ii—Ni1—Li1iv | 82.70 (4) | O2xi—Li1—P1xii | 35.84 (6) |
O1iii—Ni1—Li1iv | 42.62 (4) | O3—Li1—P1xii | 143.62 (4) |
O3iv—Ni1—Li1iv | 42.37 (4) | O3xii—Li1—P1xii | 36.38 (4) |
O3—Ni1—Li1iv | 77.66 (4) | O1xiii—Li1—P1xii | 82.30 (5) |
P1—Ni1—Li1iv | 52.252 (16) | O1iii—Li1—P1xii | 97.70 (5) |
Li1—Ni1—Li1iv | 55.597 (13) | P1—Li1—P1xii | 180.0 |
O1—P1—O2v | 113.17 (13) | O2v—Li1—Li1iv | 45.11 (4) |
O1—P1—O3iv | 113.90 (8) | O2xi—Li1—Li1iv | 134.89 (4) |
O2v—P1—O3iv | 106.12 (8) | O3—Li1—Li1iv | 83.13 (4) |
O1—P1—O3 | 113.90 (8) | O3xii—Li1—Li1iv | 96.87 (4) |
O2v—P1—O3 | 106.12 (8) | O1xiii—Li1—Li1iv | 133.27 (4) |
O3iv—P1—O3 | 102.69 (12) | O1iii—Li1—Li1iv | 46.73 (4) |
O1—P1—Li1 | 139.12 (5) | P1—Li1—Li1iv | 55.919 (11) |
O2v—P1—Li1 | 52.53 (6) | P1xii—Li1—Li1iv | 124.081 (12) |
O3iv—P1—Li1 | 106.98 (7) | O2v—Li1—Li1xiv | 134.89 (4) |
O3—P1—Li1 | 54.32 (6) | O2xi—Li1—Li1xiv | 45.11 (4) |
O1—P1—Li1iv | 139.12 (5) | O3—Li1—Li1xiv | 96.87 (4) |
O2v—P1—Li1iv | 52.53 (6) | O3xii—Li1—Li1xiv | 83.13 (4) |
O3iv—P1—Li1iv | 54.32 (6) | O1xiii—Li1—Li1xiv | 46.73 (4) |
O3—P1—Li1iv | 106.98 (7) | O1iii—Li1—Li1xiv | 133.27 (4) |
Li1—P1—Li1iv | 68.16 (2) | P1—Li1—Li1xiv | 124.082 (11) |
O1—P1—Ni1 | 136.23 (9) | P1xii—Li1—Li1xiv | 55.918 (11) |
O2v—P1—Ni1 | 110.61 (9) | Li1iv—Li1—Li1xiv | 180.0 |
O3iv—P1—Ni1 | 51.58 (6) | O2v—Li1—Ni1xii | 96.07 (5) |
O3—P1—Ni1 | 51.58 (6) | O2xi—Li1—Ni1xii | 83.93 (5) |
Li1—P1—Ni1 | 71.82 (2) | O3—Li1—Ni1xii | 136.96 (4) |
Li1iv—P1—Ni1 | 71.82 (2) | O3xii—Li1—Ni1xii | 43.04 (4) |
P1—O1—Fe1vi | 123.70 (13) | O1xiii—Li1—Ni1xii | 41.77 (6) |
P1—O1—Ni1vi | 123.70 (13) | O1iii—Li1—Ni1xii | 138.23 (6) |
Fe1vi—O1—Ni1vi | 0.000 (18) | P1—Li1—Ni1xii | 124.08 (2) |
P1—O1—Li1xv | 123.10 (8) | P1xii—Li1—Ni1xii | 55.92 (2) |
Fe1vi—O1—Li1xv | 95.61 (8) | Li1iv—Li1—Ni1xii | 117.799 (7) |
Ni1vi—O1—Li1xv | 95.61 (8) | Li1xiv—Li1—Ni1xii | 62.201 (7) |
P1—O1—Li1vi | 123.10 (8) | O2v—Li1—Fe1xii | 96.07 (5) |
Fe1vi—O1—Li1vi | 95.61 (8) | O2xi—Li1—Fe1xii | 83.93 (5) |
Ni1vi—O1—Li1vi | 95.61 (8) | O3—Li1—Fe1xii | 136.96 (4) |
Li1xv—O1—Li1vi | 86.53 (8) | O3xii—Li1—Fe1xii | 43.04 (4) |
P1vii—O2—Ni1 | 128.37 (13) | O1xiii—Li1—Fe1xii | 41.77 (6) |
P1vii—O2—Li1viii | 91.63 (8) | O1iii—Li1—Fe1xii | 138.23 (6) |
Ni1—O2—Li1viii | 122.50 (7) | P1—Li1—Fe1xii | 124.08 (2) |
P1vii—O2—Li1ix | 91.63 (8) | P1xii—Li1—Fe1xii | 55.92 (2) |
Ni1—O2—Li1ix | 122.50 (7) | Li1iv—Li1—Fe1xii | 117.799 (7) |
Li1viii—O2—Li1ix | 89.79 (8) | Li1xiv—Li1—Fe1xii | 62.201 (7) |
P1—O3—Fe1x | 126.39 (9) | Ni1xii—Li1—Fe1xii | 0.000 (16) |
P1—O3—Ni1x | 126.39 (9) |
Symmetry codes: (i) −x+1/2, −y, z−1/2; (ii) −x+1/2, y+1/2, z−1/2; (iii) x, y, z−1; (iv) x, −y+1/2, z; (v) x−1/2, −y+1/2, −z+1/2; (vi) x, y, z+1; (vii) x+1/2, −y+1/2, −z+1/2; (viii) −x+1/2, y+1/2, z+1/2; (ix) −x+1/2, −y, z+1/2; (x) −x+1/2, y−1/2, z+1/2; (xi) −x+1/2, y−1/2, z−1/2; (xii) −x, −y, −z; (xiii) −x, −y, −z+1; (xiv) x, −y−1/2, z; (xv) x, −y+1/2, z+1. |