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 |
Key indicators
- Powder X-ray study
- T = 295 K
- Mean (P-O) = 0.010 Å
- R factor = 0.000
- wR factor = 0.000
- Data-to-parameter ratio = 11.8
checkCIF/PLATON results
No syntax errors found
Alert level C REFI023_ALERT_1_C _refine_diff_density_max is missing Maximum value of final difference map (e A-3). The following tests will not be performed DIFMN_01,DIFMX_01,DIFMX_02 REFI024_ALERT_1_C _refine_diff_density_min is missing Minimum value of final difference map (e A-3). The following tests will not be performed DIFMN_01,DIFMN_02,DIFMN_03 RADNW01_ALERT_1_C The radiation wavelength lies outside the expected range for the supplied radiation type. Expected range 1.54175-1.54180 Wavelength given = 1.54439 PLAT799_ALERT_4_C Numeric Label on Displacement Par. Record ...... ?
Alert level G RADNT01_ALERT_1_G Extra text has been found in the _diffrn_radiation_type field. Radiation given as Cu K\a~1~ Cu K\a~2~ Radiation identified as Cu K\a
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
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. |