inorganic compounds
Nonalithium trigallium(III) tris[pyrophosphate(V)] diphosphate(V), Li9Ga3(P2O7)3(PO4)2, has been synthesized by a hydrothermal method and its crystal structure solved from X-ray powder diffraction data using Rietveld analysis. The structure is based on separate layers parallel to (001), consisting of GaO6 octahedra that share corners with PO4 tetrahedra and P2O7 groups. The lithium ions are located in the interstitial space.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806012426/br2004sup1.cif | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S1600536806012426/br2004Isup2.rtv |
Computing details top
Data collection: X'pert Data collector (PANalytical, 2003); cell refinement: GSAS (Larson & Von Dreele, 2000) and EXPGUI (Toby, 2001); program(s) used to refine structure: GSAS and EXPGUI; molecular graphics: DIAMOND (Brandenburg, 2004); software used to prepare material for publication: enCIFer (Allen et al., 2004).
Nonalithium trigallium(III) tris[pyrophosphate(V)] diphosphate(V) top
Crystal data top
Li9Ga3(P2O7)3(PO4)2 | F(000) = 944.0 |
Mr = 983.39 | Dx = 2.933 Mg m−3 |
Trigonal, P3c1 | Cu Kα1, Cu Kα2 radiation, λ = 1.540562, 1.544390 Å |
a = 9.72879 (13) Å | T = 295 K |
c = 13.5827 (3) Å | Particle morphology: laminar |
V = 1113.36 (3) Å3 | white |
Z = 2 | flat_sheet, 10 × 10 mm |
Data collection top
PANalytical X'pert PRO Diffractometer | Data collection mode: reflection |
Radiation source: fine-focus sealed tube, PANalytical X'pert | Scan method: continuous |
Graphite monochromator | 2θmin = 4.963°, 2θmax = 99.939°, 2θstep = 0.008° |
Specimen mounting: packed powder sample container |
Refinement top
Least-squares matrix: full | 65 parameters |
Rp = 0.047 | 1 restraint |
Rwp = 0.061 | 0 constraints |
Rexp = 0.049 | (Δ/σ)max = 0.02 |
R(F2) = 0.11835 | Background function: GSAS Background function number 1 with 30 terms. Shifted Chebyshev function of 1st kind 1: 396.391 2: -390.915 3: 175.085 4: -60.8638 5: 14.8885 6: 5.54921 7: -4.37525 8: 10.8573 9: -19.0968 10: 22.4582 11: -14.0394 12: 2.52708 13: 6.09238 14: -7.46171 15: 3.80752 16: 0.299572 17: 0.855120 18: -3.83141 19: 4.92177 20: -2.26483 21: -0.804778 22: 1.92868 23: -0.408054 24: 0.276157 25: -1.69598 26: 2.24824 27: -3.06344 28: 2.95966 29: -1.95750 30: 1.10098 |
11873 data points | Preferred orientation correction: March-Dollase (March (1932) and Dollase (1986)) AXIS 1 Ratio= 0.73101 h= 1.000 k= 0.000 l= 1.000 Prefered orientation correction range: Min= 0.82553, Max= 1.27264 |
Profile function: CW Profile function number 3 with 19 terms Pseudovoigt profile coefficients as parameterized in Thompson et al. (1987). Asymmetry correction of Finger et al. (1994). #1(GU) = 480.794 #2(GV) = -436.187 #3(GW) = 81.492 #4(GP) = 47.258 #5(LX) = 1.896 #6(LY) = 0.574 #7(S/L) = 0.0005 #8(H/L) = 0.0005 #9(trns) = -4.77 #10(shft)= -3.4119 #11(stec)= 0.15 #12(ptec)= 0.93 #13(sfec)= 0.00 #14(L11) = 0.019 #15(L22) = 0.089 #16(L33) = -0.029 #17(L12) = 0.034 #18(L13) = 0.030 #19(L23) = -0.058 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
P1 | 0.6667 | 0.3333 | 0.6255 (5) | 0.010 (2)* | |
P2 | 0.3192 (4) | 0.0886 (6) | 0.8416 (3) | 0.0071 (11)* | |
Ga1 | 0.5705 (3) | 0.0 | 0.75 | 0.0055 (6)* | |
Li1 | 0.0 | 0.0 | 0.0 | 0.04 (2)* | |
Li2 | 0.6667 | 0.3333 | 0.868 (5) | 0.09 (3)* | |
Li3 | 0.328 (3) | 0.106 (4) | 0.0589 (18) | 0.021 (8)* | |
O1 | 0.6667 | 0.3333 | 0.5125 (12) | 0.011 (5)* | |
O2 | 0.2145 (10) | 0.0 | 0.75 | 0.009 (3)* | |
O3 | 0.6764 (9) | 0.1896 (9) | 0.6630 (7) | 0.008 (3)* | |
O4 | 0.4820 (9) | 0.1094 (8) | 0.8310 (6) | 0.012 (3)* | |
O5 | 0.3228 (10) | 0.2437 (10) | 0.8431 (6) | 0.029 (2)* | |
O6 | 0.2367 (8) | 0.9963 (12) | 0.9331 (5) | 0.007 (2)* |
Geometric parameters (Å, º) top
P1—Li3i | 3.05 (3) | Li2—P2iv | 3.028 (8) |
P1—Li3ii | 3.05 (3) | Li2—P2v | 3.029 (8) |
P1—Li3iii | 3.05 (3) | Li2—Ga1 | 3.30 (3) |
P1—O1 | 1.535 (17) | Li2—Ga1iv | 3.30 (3) |
P1—O3 | 1.535 (7) | Li2—Ga1v | 3.31 (3) |
P1—O3iv | 1.536 (7) | Li2—O1i | 1.97 (6) |
P1—O3v | 1.536 (7) | Li2—O4 | 2.076 (15) |
P2—P2vi | 2.902 (8) | Li2—O4iv | 2.075 (15) |
P2—Li2 | 3.029 (8) | Li2—O4v | 2.077 (15) |
P2—Li3vii | 2.96 (2) | Li3—P1xxiv | 3.05 (3) |
P2—Li3viii | 3.00 (3) | Li3—P2xxv | 2.96 (2) |
P2—Li3ix | 3.22 (3) | Li3—P2viii | 3.22 (3) |
P2—O2 | 1.565 (5) | Li3—P2ix | 3.00 (3) |
P2—O4 | 1.500 (8) | Li3—Ga1xxiv | 3.13 (3) |
P2—O5 | 1.492 (9) | Li3—Li1 | 2.93 (3) |
P2—O6x | 1.509 (9) | Li3—Li3xvi | 3.24 (3) |
Ga1—Li2 | 3.30 (3) | Li3—Li3xvii | 3.24 (3) |
Ga1—Li2vi | 3.30 (3) | Li3—O3xxiv | 2.11 (3) |
Ga1—Li3i | 3.13 (3) | Li3—O5viii | 2.05 (3) |
Ga1—Li3xi | 3.13 (3) | Li3—O6xviii | 1.97 (2) |
Ga1—O3 | 1.990 (8) | Li3—O6xxiii | 1.86 (3) |
Ga1—O3vi | 1.990 (8) | O1—P1 | 1.535 (17) |
Ga1—O4 | 2.001 (7) | O1—Li2xxiv | 1.97 (6) |
Ga1—O4vi | 2.001 (7) | O2—P2 | 1.565 (5) |
Ga1—O5iv | 2.016 (8) | O2—P2vi | 1.565 (5) |
Ga1—O5xii | 2.016 (8) | O3—P1 | 1.535 (7) |
Li1—Li3 | 2.93 (3) | O3—Ga1 | 1.990 (8) |
Li1—Li3xiii | 2.93 (3) | O3—Li3i | 2.11 (3) |
Li1—Li3xiv | 2.93 (3) | O4—P2 | 1.500 (8) |
Li1—Li3xv | 2.93 (3) | O4—Ga1 | 2.001 (7) |
Li1—Li3xvi | 2.93 (3) | O4—Li2 | 2.076 (15) |
Li1—Li3xvii | 2.93 (3) | O5—P2 | 1.492 (9) |
Li1—O6xviii | 2.492 (6) | O5—Ga1v | 2.016 (8) |
Li1—O6xix | 2.492 (6) | O5—Li3ix | 2.05 (3) |
Li1—O6xx | 2.492 (6) | O6—P2xxvi | 1.509 (9) |
Li1—O6xxi | 2.492 (6) | O6—Li1xxvii | 2.492 (6) |
Li1—O6xxii | 2.492 (6) | O6—Li3xxvii | 1.97 (2) |
Li1—O6xxiii | 2.492 (6) | O6—Li3xxviii | 1.86 (3) |
Li2—P2 | 3.029 (8) | ||
O1—P1—O3 | 109.4 (5) | Li3xiv—Li1—Li3xv | 67.1 (4) |
O1—P1—O3iv | 109.4 (5) | Li3xiv—Li1—Li3xvi | 67.1 (4) |
O1—P1—O3v | 109.4 (5) | Li3xiv—Li1—Li3xvii | 180.0 |
O3—P1—O3iv | 109.6 (5) | Li3xv—Li1—Li3xvi | 112.9 (4) |
O3—P1—O3v | 109.6 (5) | Li3xv—Li1—Li3xvii | 112.9 (4) |
O3iv—P1—O3v | 109.5 (5) | Li3xvi—Li1—Li3xvii | 112.9 (4) |
O2—P2—O4 | 110.5 (6) | O1i—Li2—O4 | 103.9 (17) |
O2—P2—O5 | 104.4 (5) | O1i—Li2—O4iv | 103.9 (17) |
O2—P2—O6x | 108.7 (4) | O1i—Li2—O4v | 103.9 (17) |
O4—P2—O5 | 112.1 (5) | O4—Li2—O4iv | 114.4 (13) |
O4—P2—O6x | 111.7 (5) | O4—Li2—O4v | 114.4 (13) |
O5—P2—O6x | 109.1 (5) | O4iv—Li2—O4v | 114.4 (13) |
O3—Ga1—O3xxix | 173.8 (5) | Li1—Li3—O3xxiv | 152.7 (11) |
O3—Ga1—O4 | 89.7 (3) | Li1—Li3—O5viii | 88.9 (10) |
O3—Ga1—O4xxix | 94.6 (3) | Li1—Li3—O6xviii | 57.1 (7) |
O3—Ga1—O5iv | 94.0 (3) | Li1—Li3—O6xxiii | 57.6 (7) |
O3—Ga1—O5xxx | 81.6 (3) | O3xxiv—Li3—O5viii | 78.1 (10) |
O3xxix—Ga1—O4 | 94.6 (3) | O3xxiv—Li3—O6xviii | 149.0 (13) |
O3xxix—Ga1—O4xxix | 89.7 (3) | O3xxiv—Li3—O6xxiii | 107.0 (13) |
O3xxix—Ga1—O5iv | 81.6 (3) | O5viii—Li3—O6xviii | 102.3 (13) |
O3xxix—Ga1—O5xxx | 94.0 (3) | O5viii—Li3—O6xxiii | 116.3 (14) |
O4—Ga1—O4xxix | 91.7 (4) | O6xviii—Li3—O6xxiii | 100.5 (13) |
O4—Ga1—O5iv | 89.7 (3) | P1—O1—Li2xxiv | 179.9802 |
O4—Ga1—O5xxx | 171.3 (3) | P2—O2—P2vi | 136.0 (8) |
O4xxix—Ga1—O5iv | 171.3 (3) | P1—O3—Ga1 | 143.4 (5) |
O4xxix—Ga1—O5xxx | 89.7 (3) | P1—O3—Li3i | 112.5 (10) |
O5iv—Ga1—O5xxx | 90.3 (5) | Ga1—O3—Li3i | 99.5 (9) |
Li3—Li1—Li3xiii | 112.9 (4) | P2—O4—Ga1 | 133.4 (4) |
Li3—Li1—Li3xiv | 112.9 (4) | P2—O4—Li2 | 114.8 (5) |
Li3—Li1—Li3xv | 180.0 | Ga1—O4—Li2 | 108.3 (10) |
Li3—Li1—Li3xvi | 67.1 (4) | P2—O5—Ga1v | 129.7 (5) |
Li3—Li1—Li3xvii | 67.1 (4) | P2—O5—Li3ix | 129.7 (9) |
Li3xiii—Li1—Li3xiv | 112.9 (4) | Ga1v—O5—Li3ix | 100.5 (8) |
Li3xiii—Li1—Li3xv | 67.1 (4) | P2xxvi—O6—Li3xxvii | 115.5 (9) |
Li3xiii—Li1—Li3xvi | 180.0 | P2xxvi—O6—Li3xxviii | 125.9 (10) |
Li3xiii—Li1—Li3xvii | 67.1 (4) | Li3xxvii—O6—Li3xxviii | 115.7 (7) |
Symmetry codes: (i) y−x+1, y, z+1/2; (ii) −y+1, −x+1, z+1/2; (iii) x, x−y, z+1/2; (iv) −y+1, x−y, z; (v) y−x+1, −x+1, z; (vi) x−y, −y, −z+3/2; (vii) x, y, z+1; (viii) y, y−x, −z+1; (ix) x−y, x, −z+1; (x) x, y−1, z; (xi) −x+1, −y, −z+1; (xii) −x+1, y−x, −z+3/2; (xiii) −y, x−y, z; (xiv) y−x, −x, z; (xv) −x, −y, −z; (xvi) y, y−x, −z; (xvii) x−y, x, −z; (xviii) x, y−1, z−1; (xix) −y+1, x−y+1, z−1; (xx) y−x−1, −x, z−1; (xxi) −x, −y+1, −z+1; (xxii) y−1, y−x−1, −z+1; (xxiii) x−y+1, x, −z+1; (xxiv) y−x+1, y, z−1/2; (xxv) x, y, z−1; (xxvi) x, y+1, z; (xxvii) x, y+1, z+1; (xxviii) y, y−x+1, −z+1; (xxix) x−y, −y, −z+5/2; (xxx) −x+1, y−x, −z+5/2. |