Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768110031459/bp5031sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768110031459/bp5031LGTsup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768110031459/bp5031LGSTsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768110031459/bp5031LGZrTsup4.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108768110031459/bp5031sup5.pdf |
For all structures, data collection: SCAD; cell refinement: REFINE; data reduction: DATRED; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP; software used to prepare material for publication: SHELX.
Ga5.61La3O14Ta0.41 | Dx = 6.117 Mg m−3 |
Mr = 1106.05 | Neutron radiation, λ = 0.99500 Å |
Trigonal, P321 | Cell parameters from 50 reflections |
a = 8.224 (4) Å | θ = 4–44° |
c = 5.126 (1) Å | µ = 0.02 mm−1 |
V = 300.2 (2) Å3 | T = 300 K |
Z = 1 | Cubic, colourless |
F(000) = 150 | 3 × 3 × 3 mm |
Four circle diffractometer | 355 reflections with I > 2σ(I) |
Radiation source: Dhruva reactor | Rint = 0.025 |
Cu monochromator | θmax = 44.0°, θmin = 4.0° |
τ–\2t scans | h = −9→9 |
Absorption correction: integration datred | k = −9→9 |
l = 0→7 | |
374 measured reflections | 2 standard reflections every 25 reflections |
366 independent reflections | intensity decay: <3 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0963P)2 + 1.0255P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.043 | (Δ/σ)max < 0.001 |
wR(F2) = 0.135 | Δρmax = 1.15 e Å−3 |
S = 1.17 | Δρmin = −1.06 e Å−3 |
366 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
40 parameters | Extinction coefficient: 1.93 (17) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −10 (10) |
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) | |
La | 0.4246 (3) | 0.0000 | 0.0000 | 0.0121 (6) | |
Ga1 | 0.0000 | 0.0000 | 0.0000 | 0.0119 (10) | 0.61 (3) |
Ta | 0.0000 | 0.0000 | 0.0000 | 0.0119 (10) | 0.410 (17) |
Ga2 | 0.7608 (3) | 0.0000 | 0.5000 | 0.0132 (6) | |
Ga3 | 0.3333 | 0.6667 | 0.4696 (5) | 0.0098 (6) | |
O1 | 0.3333 | 0.6667 | 0.8193 (6) | 0.0133 (8) | |
O2 | 0.4565 (3) | 0.3097 (4) | 0.6936 (5) | 0.0190 (7) | |
O3 | 0.2193 (4) | 0.0777 (3) | 0.2356 (4) | 0.0165 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
La | 0.0108 (8) | 0.0089 (10) | 0.0160 (9) | 0.0044 (5) | −0.0002 (3) | −0.0004 (6) |
Ga1 | 0.0108 (12) | 0.0108 (12) | 0.0143 (17) | 0.0054 (6) | 0.000 | 0.000 |
Ta | 0.0108 (12) | 0.0108 (12) | 0.0143 (17) | 0.0054 (6) | 0.000 | 0.000 |
Ga2 | 0.0102 (9) | 0.0108 (11) | 0.0188 (10) | 0.0054 (6) | 0.0030 (4) | 0.0059 (8) |
Ga3 | 0.0087 (8) | 0.0087 (8) | 0.0120 (11) | 0.0044 (4) | 0.000 | 0.000 |
O1 | 0.0136 (11) | 0.0136 (11) | 0.0129 (14) | 0.0068 (5) | 0.000 | 0.000 |
O2 | 0.0114 (11) | 0.0219 (12) | 0.0231 (10) | 0.0079 (9) | −0.0013 (8) | −0.0064 (10) |
O3 | 0.0151 (12) | 0.0194 (12) | 0.0197 (11) | 0.0121 (9) | −0.0056 (8) | −0.0088 (8) |
La—O3i | 2.408 (3) | Ga2—O2ii | 1.865 (3) |
La—O3 | 2.408 (3) | Ga2—O2xiv | 1.865 (3) |
La—O2ii | 2.462 (3) | Ga3—O1 | 1.793 (4) |
La—O2iii | 2.462 (3) | Ga3—O2xv | 1.841 (3) |
La—O1iv | 2.6226 (17) | Ga3—O2xvi | 1.841 (3) |
La—O1v | 2.6226 (17) | Ga3—O2xvii | 1.841 (3) |
La—O2vi | 2.890 (3) | Ga3—Laxi | 3.437 (2) |
La—O2vii | 2.890 (3) | Ga3—Laxviii | 3.437 (2) |
La—Ga3viii | 3.437 (2) | Ga3—Laxix | 3.437 (2) |
La—Ga3ix | 3.437 (2) | O1—Laxx | 2.6226 (17) |
Ga1—O3x | 1.992 (2) | O1—Laxxi | 2.6226 (17) |
Ga1—O3 | 1.992 (2) | O1—Laxxii | 2.6226 (17) |
Ga1—O3xi | 1.992 (2) | O2—Ga3iv | 1.841 (3) |
Ga1—O3i | 1.992 (2) | O2—Ga2xix | 1.865 (3) |
Ga1—O3xii | 1.992 (2) | O2—Laxxii | 2.462 (3) |
Ga1—O3xiii | 1.992 (2) | O2—Laxxiii | 2.890 (3) |
Ga2—O3xiv | 1.847 (2) | O3—Ga2xix | 1.847 (2) |
Ga2—O3ii | 1.847 (2) | ||
O3i—La—O3 | 66.98 (12) | O3x—Ga1—O3xii | 83.66 (13) |
O3i—La—O2ii | 139.29 (9) | O3—Ga1—O3xii | 87.06 (10) |
O3—La—O2ii | 108.26 (8) | O3xi—Ga1—O3xii | 87.06 (10) |
O3i—La—O2iii | 108.26 (8) | O3i—Ga1—O3xii | 104.35 (14) |
O3—La—O2iii | 139.29 (9) | O3x—Ga1—O3xiii | 87.06 (10) |
O2ii—La—O2iii | 100.06 (14) | O3—Ga1—O3xiii | 104.35 (14) |
O3i—La—O1iv | 125.62 (8) | O3xi—Ga1—O3xiii | 83.66 (13) |
O3—La—O1iv | 79.16 (7) | O3i—Ga1—O3xiii | 87.06 (10) |
O2ii—La—O1iv | 90.42 (8) | O3xii—Ga1—O3xiii | 164.84 (13) |
O2iii—La—O1iv | 71.88 (9) | O3xiv—Ga2—O3ii | 132.4 (2) |
O3i—La—O1v | 79.16 (7) | O3xiv—Ga2—O2ii | 99.89 (11) |
O3—La—O1v | 125.62 (8) | O3ii—Ga2—O2ii | 109.91 (11) |
O2ii—La—O1v | 71.88 (9) | O3xiv—Ga2—O2xiv | 109.91 (11) |
O2iii—La—O1v | 90.42 (8) | O3ii—Ga2—O2xiv | 99.89 (11) |
O1iv—La—O1v | 152.65 (10) | O2ii—Ga2—O2xiv | 101.2 (2) |
O3i—La—O2vi | 78.77 (9) | O1—Ga3—O2xv | 117.04 (10) |
O3—La—O2vi | 67.11 (8) | O1—Ga3—O2xvi | 117.04 (11) |
O2ii—La—O2vi | 63.51 (10) | O2xv—Ga3—O2xvi | 100.96 (13) |
O2iii—La—O2vi | 153.57 (7) | O1—Ga3—O2xvii | 117.04 (10) |
O1iv—La—O2vi | 125.57 (8) | O2xv—Ga3—O2xvii | 100.96 (13) |
O1v—La—O2vi | 65.40 (7) | O2xvi—Ga3—O2xvii | 100.96 (13) |
O3i—La—O2vii | 67.11 (8) | O1—Ga3—Laxi | 134.45 (4) |
O3—La—O2vii | 78.77 (9) | O2xv—Ga3—Laxi | 43.74 (10) |
O2ii—La—O2vii | 153.57 (7) | O2xvi—Ga3—Laxi | 107.99 (13) |
O2iii—La—O2vii | 63.51 (10) | O2xvii—Ga3—Laxi | 57.23 (11) |
O1iv—La—O2vii | 65.40 (7) | O1—Ga3—Laxviii | 134.45 (4) |
O1v—La—O2vii | 125.57 (8) | O2xv—Ga3—Laxviii | 57.23 (11) |
O2vi—La—O2vii | 139.04 (13) | O2xvi—Ga3—Laxviii | 43.74 (10) |
O3i—La—Ga3viii | 87.59 (7) | O2xvii—Ga3—Laxviii | 107.99 (13) |
O3—La—Ga3viii | 110.05 (7) | Laxi—Ga3—Laxviii | 76.37 (5) |
O2ii—La—Ga3viii | 128.63 (10) | O1—Ga3—Laxix | 134.45 (3) |
O2iii—La—Ga3viii | 31.13 (5) | O2xv—Ga3—Laxix | 107.99 (13) |
O1iv—La—Ga3viii | 65.13 (8) | O2xvi—Ga3—Laxix | 57.23 (11) |
O1v—La—Ga3viii | 109.59 (7) | O2xvii—Ga3—Laxix | 43.74 (10) |
O2vi—La—Ga3viii | 166.09 (8) | Laxi—Ga3—Laxix | 76.37 (5) |
O2vii—La—Ga3viii | 32.38 (5) | Laxviii—Ga3—Laxix | 76.37 (5) |
O3i—La—Ga3ix | 110.05 (7) | Ga3—O1—Laxx | 110.68 (7) |
O3—La—Ga3ix | 87.59 (7) | Ga3—O1—Laxxi | 110.68 (7) |
O2ii—La—Ga3ix | 31.13 (5) | Laxx—O1—Laxxi | 108.24 (7) |
O2iii—La—Ga3ix | 128.63 (10) | Ga3—O1—Laxxii | 110.68 (7) |
O1iv—La—Ga3ix | 109.59 (7) | Laxx—O1—Laxxii | 108.24 (7) |
O1v—La—Ga3ix | 65.13 (8) | Laxxi—O1—Laxxii | 108.24 (7) |
O2vi—La—Ga3ix | 32.38 (5) | Ga3iv—O2—Ga2xix | 119.60 (15) |
O2vii—La—Ga3ix | 166.09 (8) | Ga3iv—O2—Laxxii | 105.13 (12) |
Ga3viii—La—Ga3ix | 159.22 (8) | Ga2xix—O2—Laxxii | 120.59 (13) |
O3x—Ga1—O3 | 164.84 (13) | Ga3iv—O2—Laxxiii | 90.39 (12) |
O3x—Ga1—O3xi | 104.35 (14) | Ga2xix—O2—Laxxiii | 111.39 (14) |
O3—Ga1—O3xi | 87.06 (10) | Laxxii—O2—Laxxiii | 104.85 (9) |
O3x—Ga1—O3i | 87.06 (10) | Ga2xix—O3—Ga1 | 114.59 (13) |
O3—Ga1—O3i | 83.66 (13) | Ga2xix—O3—La | 137.51 (14) |
O3xi—Ga1—O3i | 164.84 (13) | Ga1—O3—La | 104.68 (9) |
Symmetry codes: (i) x−y, −y, −z; (ii) −x+1, −x+y, −z+1; (iii) −y+1, x−y, z−1; (iv) x−y+1, −y+1, −z+1; (v) x, y−1, z−1; (vi) x−y, −y, −z+1; (vii) x, y, z−1; (viii) x−y+1, −y+1, −z; (ix) x, y−1, z; (x) −x, −x+y, −z; (xi) −y, x−y, z; (xii) −x+y, −x, z; (xiii) y, x, −z; (xiv) −y+1, x−y, z; (xv) x−y, −y+1, −z+1; (xvi) −x+1, −x+y+1, −z+1; (xvii) y, x, −z+1; (xviii) x, y+1, z; (xix) −x+y+1, −x+1, z; (xx) x, y+1, z+1; (xxi) −y, x−y, z+1; (xxii) −x+y+1, −x+1, z+1; (xxiii) x, y, z+1. |
Ga5.34La3O14Si0.36Ta0.29 | Dx = 6.000 Mg m−3 |
Mr = 1075.12 | Neutron radiation, λ = 0.99500 Å |
Trigonal, P321 | Cell parameters from 50 reflections |
a = 8.195 (7) Å | θ = 4.0–44° |
c = 5.118 (1) Å | µ = 0.02 mm−1 |
V = 297.7 (4) Å3 | T = 300 K |
Z = 1 | Cubic, colourless |
F(000) = 148 | 3 × 3 × 3 mm |
Four circle diffractometer | 440 reflections with I > 2σ(I) |
Radiation source: dhruva reactor | Rint = 0.022 |
Cu monochromator | θmax = 44.1°, θmin = 4.0° |
τ–\2t scans | h = −11→11 |
Absorption correction: integration Datred | k = −5→10 |
l = −6→7 | |
461 measured reflections | 2 standard reflections every 25 reflections |
454 independent reflections | intensity decay: <3 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0939P)2 + 1.5721P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.045 | (Δ/σ)max = 0.012 |
wR(F2) = 0.134 | Δρmax = 0.83 e Å−3 |
S = 1.14 | Δρmin = −0.83 e Å−3 |
454 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
42 parameters | Extinction coefficient: 2.10 (17) |
2 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 10 (10) |
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) | |
La | 0.4222 (3) | 0.0000 | 0.0000 | 0.0077 (6) | |
Ga1 | 0.0000 | 0.0000 | 0.0000 | 0.0104 (10) | 0.75 (3) |
Ta | 0.0000 | 0.0000 | 0.0000 | 0.0104 (10) | 0.288 (12) |
Ga2 | 0.7640 (3) | 0.0000 | 0.5000 | 0.0081 (6) | |
Si | 0.3333 | 0.6667 | 0.5321 (6) | 0.0067 (7) | 0.18 (2) |
Ga3 | 0.3333 | 0.6667 | 0.5321 (6) | 0.0067 (7) | 0.794 (10) |
O12D | 0.3333 | 0.6667 | 0.1873 (7) | 0.0122 (8) | |
O26G | 0.4609 (3) | 0.3108 (4) | 0.3113 (4) | 0.0161 (6) | |
O36G | 0.2211 (4) | 0.0794 (4) | 0.7633 (4) | 0.0171 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
La | 0.0108 (8) | 0.0070 (9) | 0.0040 (8) | 0.0035 (5) | 0.0006 (3) | 0.0013 (6) |
Ga1 | 0.0137 (13) | 0.0137 (13) | 0.0038 (17) | 0.0068 (6) | 0.000 | 0.000 |
Ta | 0.0137 (13) | 0.0137 (13) | 0.0038 (17) | 0.0068 (6) | 0.000 | 0.000 |
Ga2 | 0.0084 (8) | 0.0089 (10) | 0.0072 (9) | 0.0044 (5) | −0.0027 (4) | −0.0053 (7) |
Si | 0.0076 (9) | 0.0076 (9) | 0.0050 (11) | 0.0038 (4) | 0.000 | 0.000 |
Ga3 | 0.0076 (9) | 0.0076 (9) | 0.0050 (11) | 0.0038 (4) | 0.000 | 0.000 |
O12D | 0.0122 (10) | 0.0122 (10) | 0.0121 (16) | 0.0061 (5) | 0.000 | 0.000 |
O26G | 0.0125 (11) | 0.0212 (12) | 0.0144 (10) | 0.0084 (9) | 0.0055 (8) | 0.0086 (8) |
O36G | 0.0200 (12) | 0.0262 (14) | 0.0115 (11) | 0.0165 (10) | 0.0073 (9) | 0.0140 (8) |
La—O36Gi | 2.384 (3) | Ga2—O26Gxiv | 1.891 (3) |
La—O36Gii | 2.384 (3) | Ga2—O26Giii | 1.891 (3) |
La—O26Giii | 2.479 (3) | Si—O12D | 1.764 (4) |
La—O26Giv | 2.479 (3) | Si—O26Gxv | 1.792 (3) |
La—O12Dv | 2.631 (2) | Si—O26Gxvi | 1.792 (3) |
La—O12Dvi | 2.631 (2) | Si—O26Gxi | 1.792 (3) |
La—O26Gvii | 2.885 (3) | O12D—Laxvii | 2.631 (2) |
La—O26G | 2.885 (3) | O12D—Laxviii | 2.631 (2) |
La—Ga3viii | 3.426 (3) | O12D—Laxix | 2.631 (2) |
La—Ga3ix | 3.426 (3) | O26G—Ga3viii | 1.792 (3) |
Ga1—O36Gx | 1.999 (3) | O26G—Siviii | 1.792 (3) |
Ga1—O36Gxi | 1.999 (3) | O26G—Ga2xix | 1.891 (3) |
Ga1—O36Gii | 1.999 (3) | O26G—Laxix | 2.479 (3) |
Ga1—O36Gxii | 1.999 (3) | O36G—Ga2xix | 1.822 (3) |
Ga1—O36Gxiii | 1.999 (3) | O36G—Taxx | 1.999 (3) |
Ga1—O36Gi | 1.999 (3) | O36G—Ga1xx | 1.999 (3) |
Ga2—O36Giii | 1.822 (3) | O36G—Laxx | 2.384 (3) |
Ga2—O36Gxiv | 1.822 (3) | ||
O36Gi—La—O36Gii | 68.20 (12) | O36Gxi—Ga1—O36Gii | 87.07 (11) |
O36Gi—La—O26Giii | 138.63 (10) | O36Gx—Ga1—O36Gxii | 87.07 (11) |
O36Gii—La—O26Giii | 107.47 (9) | O36Gxi—Ga1—O36Gxii | 83.91 (14) |
O36Gi—La—O26Giv | 107.47 (9) | O36Gii—Ga1—O36Gxii | 165.34 (15) |
O36Gii—La—O26Giv | 138.63 (10) | O36Gx—Ga1—O36Gxiii | 83.91 (14) |
O26Giii—La—O26Giv | 101.25 (14) | O36Gxi—Ga1—O36Gxiii | 87.07 (11) |
O36Gi—La—O12Dv | 78.62 (8) | O36Gii—Ga1—O36Gxiii | 87.07 (11) |
O36Gii—La—O12Dv | 126.76 (9) | O36Gxii—Ga1—O36Gxiii | 103.94 (17) |
O26Giii—La—O12Dv | 72.20 (10) | O36Gx—Ga1—O36Gi | 87.07 (11) |
O26Giv—La—O12Dv | 89.90 (9) | O36Gxi—Ga1—O36Gi | 103.94 (17) |
O36Gi—La—O12Dvi | 126.76 (9) | O36Gii—Ga1—O36Gi | 83.91 (14) |
O36Gii—La—O12Dvi | 78.62 (8) | O36Gxii—Ga1—O36Gi | 87.07 (11) |
O26Giii—La—O12Dvi | 89.90 (9) | O36Gxiii—Ga1—O36Gi | 165.34 (15) |
O26Giv—La—O12Dvi | 72.20 (10) | O36Giii—Ga2—O36Gxiv | 134.7 (2) |
O12Dv—La—O12Dvi | 151.96 (9) | O36Giii—Ga2—O26Gxiv | 100.57 (12) |
O36Gi—La—O26Gvii | 68.00 (9) | O36Gxiv—Ga2—O26Gxiv | 108.50 (11) |
O36Gii—La—O26Gvii | 79.93 (10) | O36Giii—Ga2—O26Giii | 108.50 (11) |
O26Giii—La—O26Gvii | 153.37 (7) | O36Gxiv—Ga2—O26Giii | 100.57 (12) |
O26Giv—La—O26Gvii | 61.77 (11) | O26Gxiv—Ga2—O26Giii | 99.0 (2) |
O12Dv—La—O26Gvii | 124.52 (9) | O12D—Si—O26Gxv | 116.57 (11) |
O12Dvi—La—O26Gvii | 66.05 (8) | O12D—Si—O26Gxvi | 116.57 (11) |
O36Gi—La—O26G | 79.93 (10) | O26Gxv—Si—O26Gxvi | 101.53 (14) |
O36Gii—La—O26G | 68.00 (9) | O12D—Si—O26Gxi | 116.57 (11) |
O26Giii—La—O26G | 61.77 (11) | O26Gxv—Si—O26Gxi | 101.53 (14) |
O26Giv—La—O26G | 153.37 (7) | O26Gxvi—Si—O26Gxi | 101.53 (14) |
O12Dv—La—O26G | 66.05 (8) | Si—O12D—Laxvii | 111.37 (7) |
O12Dvi—La—O26G | 124.52 (9) | Si—O12D—Laxviii | 111.37 (7) |
O26Gvii—La—O26G | 141.24 (13) | Laxvii—O12D—Laxviii | 107.51 (8) |
O36Gi—La—Ga3viii | 110.24 (8) | Si—O12D—Laxix | 111.37 (7) |
O36Gii—La—Ga3viii | 87.82 (8) | Laxvii—O12D—Laxix | 107.51 (8) |
O26Giii—La—Ga3viii | 30.25 (6) | Laxviii—O12D—Laxix | 107.51 (8) |
O26Giv—La—Ga3viii | 128.89 (9) | Ga3viii—O26G—Siviii | 0.00 (17) |
O12Dv—La—Ga3viii | 65.72 (9) | Ga3viii—O26G—Ga2xix | 121.31 (15) |
O12Dvi—La—Ga3viii | 108.73 (9) | Siviii—O26G—Ga2xix | 121.31 (15) |
O26Gvii—La—Ga3viii | 167.39 (8) | Ga3viii—O26G—Laxix | 105.55 (12) |
O26G—La—Ga3viii | 31.52 (5) | Siviii—O26G—Laxix | 105.55 (12) |
O36Gi—La—Ga3ix | 87.82 (8) | Ga2xix—O26G—Laxix | 119.90 (13) |
O36Gii—La—Ga3ix | 110.24 (8) | Ga3viii—O26G—La | 91.15 (12) |
O26Giii—La—Ga3ix | 128.89 (9) | Siviii—O26G—La | 91.15 (12) |
O26Giv—La—Ga3ix | 30.25 (6) | Ga2xix—O26G—La | 109.69 (13) |
O12Dv—La—Ga3ix | 108.73 (9) | Laxix—O26G—La | 104.33 (9) |
O12Dvi—La—Ga3ix | 65.72 (9) | Ga2xix—O36G—Taxx | 114.09 (13) |
O26Gvii—La—Ga3ix | 31.52 (5) | Ga2xix—O36G—Ga1xx | 114.09 (13) |
O26G—La—Ga3ix | 167.39 (8) | Taxx—O36G—Ga1xx | 0.0 |
Ga3viii—La—Ga3ix | 158.56 (7) | Ga2xix—O36G—Laxx | 139.13 (14) |
O36Gx—Ga1—O36Gxi | 165.34 (15) | Taxx—O36G—Laxx | 103.95 (10) |
O36Gx—Ga1—O36Gii | 103.94 (17) | Ga1xx—O36G—Laxx | 103.95 (10) |
Symmetry codes: (i) x, y, z−1; (ii) x−y, −y, −z+1; (iii) −y+1, x−y, z; (iv) −x+1, −x+y, −z; (v) x−y+1, −y+1, −z; (vi) x, y−1, z; (vii) x−y, −y, −z; (viii) x−y+1, −y+1, −z+1; (ix) x, y−1, z−1; (x) −x+y, −x, z−1; (xi) y, x, −z+1; (xii) −y, x−y, z−1; (xiii) −x, −x+y, −z+1; (xiv) −x+1, −x+y, −z+1; (xv) x−y, −y+1, −z+1; (xvi) −x+1, −x+y+1, −z+1; (xvii) −y, x−y, z; (xviii) x, y+1, z; (xix) −x+y+1, −x+1, z; (xx) x, y, z+1. |
Ga5.48La3O14Ta0.03Zr0.50 | Dx = 5.876 Mg m−3 |
Mr = 1073.18 | Neutron radiation, λ = 0.99500 Å |
Trigonal, P321 | Cell parameters from 50 reflections |
a = 8.256 (5) Å | θ = 4–44° |
c = 5.141 (2) Å | µ = 0.01 mm−1 |
V = 303.5 (3) Å3 | T = 300 K |
Z = 1 | Cubic, colourless |
F(000) = 150 | 3 × 3 × 3 mm |
Four circle diffractometer | 341 reflections with I > 2σ(I) |
Radiation source: Dhruva | Rint = 0.0000 |
Cu monochromator | θmax = 44.1°, θmin = 4.0° |
τ–\2t scans | h = −9→10 |
Absorption correction: integration datred | k = −10→11 |
l = −7→7 | |
354 measured reflections | 2 standard reflections every 25 reflections |
354 independent reflections | intensity decay: <3 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0446P)2 + 0.320P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.027 | (Δ/σ)max < 0.001 |
wR(F2) = 0.071 | Δρmax = 0.60 e Å−3 |
S = 1.14 | Δρmin = −0.71 e Å−3 |
354 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
43 parameters | Extinction coefficient: 3.14 (16) |
2 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −10 (10) |
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) | |
La | 0.42582 (18) | 0.0000 | 0.0000 | 0.0096 (4) | |
Ga2 | 0.7583 (2) | 0.0000 | 0.5000 | 0.0103 (4) | 0.977 (8) |
Zr2 | 0.7583 (2) | 0.0000 | 0.5000 | 0.0103 (4) | 0.026 (5) |
Ga1 | 0.0000 | 0.0000 | 0.0000 | 0.0099 (9) | 0.55 (4) |
Zr1 | 0.0000 | 0.0000 | 0.0000 | 0.0099 (9) | 0.42 (5) |
Ta | 0.0000 | 0.0000 | 0.0000 | 0.0099 (9) | 0.027 (3) |
Ga3 | 0.3333 | 0.6667 | 0.5309 (3) | 0.0091 (4) | |
O1 | 0.3333 | 0.6667 | 0.1806 (4) | 0.0118 (5) | |
O2 | 0.4578 (2) | 0.3108 (3) | 0.3051 (3) | 0.0151 (4) | |
O3 | 0.2232 (2) | 0.0796 (2) | 0.7597 (3) | 0.0148 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
La | 0.0114 (5) | 0.0104 (7) | 0.0066 (5) | 0.0052 (3) | 0.0003 (2) | 0.0006 (4) |
Ga2 | 0.0116 (6) | 0.0118 (7) | 0.0075 (6) | 0.0059 (4) | −0.0016 (2) | −0.0033 (5) |
Zr2 | 0.0116 (6) | 0.0118 (7) | 0.0075 (6) | 0.0059 (4) | −0.0016 (2) | −0.0033 (5) |
Ga1 | 0.0117 (10) | 0.0117 (10) | 0.0063 (13) | 0.0059 (5) | 0.000 | 0.000 |
Zr1 | 0.0117 (10) | 0.0117 (10) | 0.0063 (13) | 0.0059 (5) | 0.000 | 0.000 |
Ta | 0.0117 (10) | 0.0117 (10) | 0.0063 (13) | 0.0059 (5) | 0.000 | 0.000 |
Ga3 | 0.0110 (6) | 0.0110 (6) | 0.0051 (7) | 0.0055 (3) | 0.000 | 0.000 |
O1 | 0.0155 (7) | 0.0155 (7) | 0.0044 (9) | 0.0078 (4) | 0.000 | 0.000 |
O2 | 0.0116 (7) | 0.0229 (8) | 0.0101 (6) | 0.0080 (6) | 0.0014 (5) | 0.0064 (6) |
O3 | 0.0163 (8) | 0.0189 (8) | 0.0117 (7) | 0.0106 (6) | 0.0035 (5) | 0.0066 (5) |
La—O3i | 2.420 (2) | Ga3—O2xvi | 1.8438 (19) |
La—O3ii | 2.420 (2) | Ga3—O2xii | 1.8438 (19) |
La—O2iii | 2.454 (2) | Ga3—Zr2xvii | 3.202 (2) |
La—O2iv | 2.454 (2) | Ga3—Zr2xviii | 3.202 (2) |
La—O1v | 2.6301 (17) | Ga3—Zr2xix | 3.202 (2) |
La—O1vi | 2.6301 (17) | Ga3—Laxx | 3.4453 (18) |
La—O2vii | 2.905 (2) | Ga3—Laxxi | 3.4453 (18) |
La—O2 | 2.905 (2) | Ga3—Laxxii | 3.4453 (18) |
La—Ga3viii | 3.4453 (18) | O1—Laxvii | 2.6301 (17) |
La—Ga3ix | 3.4453 (18) | O1—Laxviii | 2.6301 (17) |
Ga2—O3iii | 1.8417 (17) | O1—Laxix | 2.6301 (17) |
Ga2—O3x | 1.8417 (17) | O2—Ga3viii | 1.8438 (19) |
Ga2—O2x | 1.869 (2) | O2—Zr2xix | 1.869 (2) |
Ga2—O2iii | 1.869 (2) | O2—Ga2xix | 1.869 (2) |
Ga1—O3xi | 2.0357 (17) | O2—Laxix | 2.454 (2) |
Ga1—O3xii | 2.0357 (17) | O3—Zr2xix | 1.8417 (17) |
Ga1—O3ii | 2.0357 (17) | O3—Ga2xix | 1.8417 (17) |
Ga1—O3xiii | 2.0357 (17) | O3—Taxxiii | 2.0357 (17) |
Ga1—O3i | 2.0357 (17) | O3—Zr1xxiii | 2.0357 (17) |
Ga1—O3xiv | 2.0357 (17) | O3—Ga1xxiii | 2.0357 (17) |
Ga3—O1 | 1.801 (3) | O3—Laxxiii | 2.420 (2) |
Ga3—O2xv | 1.8438 (19) | ||
O3i—La—O3ii | 68.42 (8) | O2xvi—Ga3—O2xii | 100.74 (9) |
O3i—La—O2iii | 138.94 (6) | O1—Ga3—Zr2xvii | 87.15 (3) |
O3ii—La—O2iii | 107.62 (6) | O2xv—Ga3—Zr2xvii | 30.64 (5) |
O3i—La—O2iv | 107.62 (6) | O2xvi—Ga3—Zr2xvii | 112.42 (7) |
O3ii—La—O2iv | 138.94 (6) | O2xii—Ga3—Zr2xvii | 123.17 (7) |
O2iii—La—O2iv | 100.58 (9) | O1—Ga3—Zr2xviii | 87.15 (3) |
O3i—La—O1v | 78.41 (5) | O2xv—Ga3—Zr2xviii | 123.17 (7) |
O3ii—La—O1v | 125.87 (6) | O2xvi—Ga3—Zr2xviii | 30.64 (5) |
O2iii—La—O1v | 71.88 (6) | O2xii—Ga3—Zr2xviii | 112.42 (7) |
O2iv—La—O1v | 90.78 (5) | Zr2xvii—Ga3—Zr2xviii | 119.755 (5) |
O3i—La—O1vi | 125.87 (6) | O1—Ga3—Zr2xix | 87.15 (3) |
O3ii—La—O1vi | 78.41 (5) | O2xv—Ga3—Zr2xix | 112.42 (7) |
O2iii—La—O1vi | 90.78 (5) | O2xvi—Ga3—Zr2xix | 123.17 (7) |
O2iv—La—O1vi | 71.88 (6) | O2xii—Ga3—Zr2xix | 30.64 (5) |
O1v—La—O1vi | 153.07 (6) | Zr2xvii—Ga3—Zr2xix | 119.755 (5) |
O3i—La—O2vii | 67.30 (6) | Zr2xviii—Ga3—Zr2xix | 119.755 (5) |
O3ii—La—O2vii | 78.78 (6) | O1—Ga3—Laxx | 134.42 (3) |
O2iii—La—O2vii | 153.75 (5) | O2xv—Ga3—Laxx | 57.47 (7) |
O2iv—La—O2vii | 63.36 (6) | O2xvi—Ga3—Laxx | 43.29 (6) |
O1v—La—O2vii | 125.76 (6) | O2xii—Ga3—Laxx | 107.80 (9) |
O1vi—La—O2vii | 65.11 (5) | Zr2xvii—Ga3—Laxx | 73.71 (3) |
O3i—La—O2 | 78.78 (6) | Zr2xviii—Ga3—Laxx | 68.79 (3) |
O3ii—La—O2 | 67.30 (6) | Zr2xix—Ga3—Laxx | 138.29 (5) |
O2iii—La—O2 | 63.36 (6) | O1—Ga3—Laxxi | 134.42 (3) |
O2iv—La—O2 | 153.75 (5) | O2xv—Ga3—Laxxi | 43.29 (6) |
O1v—La—O2 | 65.11 (5) | O2xvi—Ga3—Laxxi | 107.80 (9) |
O1vi—La—O2 | 125.76 (6) | O2xii—Ga3—Laxxi | 57.47 (7) |
O2vii—La—O2 | 138.91 (8) | Zr2xvii—Ga3—Laxxi | 68.79 (3) |
O3i—La—Ga3viii | 109.98 (5) | Zr2xviii—Ga3—Laxxi | 138.29 (5) |
O3ii—La—Ga3viii | 87.27 (5) | Zr2xix—Ga3—Laxxi | 73.71 (3) |
O2iii—La—Ga3viii | 31.01 (3) | Laxx—Ga3—Laxxi | 76.42 (5) |
O2iv—La—Ga3viii | 129.04 (6) | O1—Ga3—Laxxii | 134.42 (3) |
O1v—La—Ga3viii | 65.09 (6) | O2xv—Ga3—Laxxii | 107.80 (9) |
O1vi—La—Ga3viii | 109.78 (6) | O2xvi—Ga3—Laxxii | 57.47 (7) |
O2vii—La—Ga3viii | 165.82 (5) | O2xii—Ga3—Laxxii | 43.29 (6) |
O2—La—Ga3viii | 32.36 (3) | Zr2xvii—Ga3—Laxxii | 138.29 (5) |
O3i—La—Ga3ix | 87.27 (5) | Zr2xviii—Ga3—Laxxii | 73.71 (3) |
O3ii—La—Ga3ix | 109.98 (5) | Zr2xix—Ga3—Laxxii | 68.79 (3) |
O2iii—La—Ga3ix | 129.04 (6) | Laxx—Ga3—Laxxii | 76.42 (5) |
O2iv—La—Ga3ix | 31.01 (3) | Laxxi—Ga3—Laxxii | 76.42 (5) |
O1v—La—Ga3ix | 109.78 (6) | Ga3—O1—Laxvii | 110.67 (4) |
O1vi—La—Ga3ix | 65.09 (6) | Ga3—O1—Laxviii | 110.67 (4) |
O2vii—La—Ga3ix | 32.36 (3) | Laxvii—O1—Laxviii | 108.24 (5) |
O2—La—Ga3ix | 165.82 (5) | Ga3—O1—Laxix | 110.67 (4) |
Ga3viii—La—Ga3ix | 159.52 (5) | Laxvii—O1—Laxix | 108.24 (5) |
O3iii—Ga2—O3x | 132.25 (14) | Laxviii—O1—Laxix | 108.24 (5) |
O3iii—Ga2—O2x | 100.35 (8) | Ga3viii—O2—Zr2xix | 119.17 (10) |
O3x—Ga2—O2x | 109.28 (7) | Ga3viii—O2—Ga2xix | 119.17 (10) |
O3iii—Ga2—O2iii | 109.28 (7) | Zr2xix—O2—Ga2xix | 0.00 (6) |
O3x—Ga2—O2iii | 100.35 (8) | Ga3viii—O2—Laxix | 105.70 (8) |
O2x—Ga2—O2iii | 101.93 (15) | Zr2xix—O2—Laxix | 120.29 (8) |
O3xi—Ga1—O3xii | 165.09 (9) | Ga2xix—O2—Laxix | 120.29 (8) |
O3xi—Ga1—O3ii | 104.22 (10) | Ga3viii—O2—La | 90.17 (8) |
O3xii—Ga1—O3ii | 86.98 (7) | Zr2xix—O2—La | 111.63 (9) |
O3xi—Ga1—O3xiii | 86.98 (7) | Ga2xix—O2—La | 111.63 (9) |
O3xii—Ga1—O3xiii | 83.87 (9) | Laxix—O2—La | 105.07 (6) |
O3ii—Ga1—O3xiii | 165.09 (9) | Zr2xix—O3—Ga2xix | 0.00 (10) |
O3xi—Ga1—O3i | 86.98 (7) | Zr2xix—O3—Taxxiii | 114.03 (8) |
O3xii—Ga1—O3i | 104.22 (10) | Ga2xix—O3—Taxxiii | 114.03 (8) |
O3ii—Ga1—O3i | 83.87 (9) | Zr2xix—O3—Zr1xxiii | 114.03 (8) |
O3xiii—Ga1—O3i | 86.98 (7) | Ga2xix—O3—Zr1xxiii | 114.03 (8) |
O3xi—Ga1—O3xiv | 83.87 (9) | Taxxiii—O3—Zr1xxiii | 0.0 |
O3xii—Ga1—O3xiv | 86.98 (7) | Zr2xix—O3—Ga1xxiii | 114.03 (8) |
O3ii—Ga1—O3xiv | 86.98 (7) | Ga2xix—O3—Ga1xxiii | 114.03 (8) |
O3xiii—Ga1—O3xiv | 104.22 (10) | Taxxiii—O3—Ga1xxiii | 0.0 |
O3i—Ga1—O3xiv | 165.09 (9) | Zr1xxiii—O3—Ga1xxiii | 0.0 |
O1—Ga3—O2xv | 117.21 (7) | Zr2xix—O3—Laxxiii | 138.60 (9) |
O1—Ga3—O2xvi | 117.21 (7) | Ga2xix—O3—Laxxiii | 138.60 (9) |
O2xv—Ga3—O2xvi | 100.74 (9) | Taxxiii—O3—Laxxiii | 103.86 (7) |
O1—Ga3—O2xii | 117.21 (7) | Zr1xxiii—O3—Laxxiii | 103.86 (7) |
O2xv—Ga3—O2xii | 100.74 (9) | Ga1xxiii—O3—Laxxiii | 103.86 (7) |
Symmetry codes: (i) x, y, z−1; (ii) x−y, −y, −z+1; (iii) −y+1, x−y, z; (iv) −x+1, −x+y, −z; (v) x−y+1, −y+1, −z; (vi) x, y−1, z; (vii) x−y, −y, −z; (viii) x−y+1, −y+1, −z+1; (ix) x, y−1, z−1; (x) −x+1, −x+y, −z+1; (xi) −x+y, −x, z−1; (xii) y, x, −z+1; (xiii) −y, x−y, z−1; (xiv) −x, −x+y, −z+1; (xv) x−y, −y+1, −z+1; (xvi) −x+1, −x+y+1, −z+1; (xvii) −y, x−y, z; (xviii) x, y+1, z; (xix) −x+y+1, −x+1, z; (xx) x, y+1, z+1; (xxi) −y, x−y, z+1; (xxii) −x+y+1, −x+1, z+1; (xxiii) x, y, z+1. |