research papers
Symmetry reduction in the basic structure of thortveitite-type compound FeInGe2O7–mC22 (C12/m1, No. 12) promoted by the incorporation of yttrium in the formula FeIn1−xYxGe2O7 gives rise to a derivative structure called thortveitite-like AA′Ge2O7–mP44, with symmetry described by the space group P121/m1 (No. 11) for x = 0.50, 0.75 and 0.90. The structure remains unchanged within the structural type of thortveitite when x = 0.25. In order to establish structural models for performing a Rietveld refinement to the derivative structure, symmetry relations between space groups connecting the basic and derivative structures were used. The higher contrast to X-rays of Fe3+, In3+ and Y3+ as well as by the behaviour during the refinements of the isotropic thermal displacements, the values of interatomic distances and calculated bond-valence sums for each atom in the asymmetric unit, were helpful for elucidating the relocation of cations in the different available crystallographic sites generated by the symmetry reduction.
Keywords: thortveitite; symmetry relations between space groups; Rietveld refinement; bond-valence sum.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520618009654/ra5035sup1.cif |
CCDC references: 434316; 434317; 434310
Computing details top
For all structures, program(s) used to refine structure: GSAS-II (Toby & Von Dreele, J. Appl. Cryst. 46, 544-549, 2013).
(Y25) top
Crystal data top
FeGe2In0.75O7Y0.25 | β = 102.519 (3)° |
Mr = 421.36 | V = 266.94 (3) Å3 |
Monoclinic, C2/m | Z = 2 |
a = 6.5501 (12) Å | Cu Kα radiation |
b = 8.5635 (4) Å | T = 300 K |
c = 4.8749 (6) Å |
Refinement top
Least-squares matrix: full | 5455 data points |
Rp = 0.051 | Profile function: Finger-Cox-Jephcoat function parameters U, V, W, X, Y, SH/L: peak variance(Gauss) = Utan(Th)2+Vtan(Th)+W: peak HW(Lorentz) = X/cos(Th)+Ytan(Th); SH/L = S/L+H/L U, V, W in (centideg)2, X & Y in centideg 2.000, -2.000, 5.000, 0.000, 0.000, 0.002, Crystallite size model "isotropic" for Fe In 0.75 Y 0.25 Ge2 O7 (microns) parameters: Size, G/L mix 1.000, 1.000, Mustrain model "generalized" for Fe In 0.75 Y 0.25 Ge2 O7 (106) parameters: S400, S040, S004, S220, S202, S022, S301, S103, S121, G/L mix 161301.868, 10834.480, 54470.004, 28956.494, 106226.688, 1197.624, 195253.716, -13862.079, 17449.390, 1.000, |
Rwp = 0.071 | 50 parameters |
Rexp = 0.032 | Background function: Background function: "chebyschev" function with 24 terms: 669.8(29), -77(12), -4.9(3)e2, 5.3(10)e2, 3.19(11)e3, -3.42(22)e3, -5.78(4)e3, 7.42(4)e3, -6.2(10)e2, -3.15(17)e3, 7.80(7)e3, -6.60(18)e3, 911(24), 1.80(6)e3, -4.37(8)e3, 3.84(12)e3, -4.85(11)e3, 2.90(22)e3, 3.25(9)e3, -1.18(20)e3, -1631(17), -5.5(4)e2, 2.59(16)e3, -1.66(31)e3, |
R(F2) = 0.06202 | Preferred orientation correction: March-Dollase correction coef. = 1.000 axis = [0, 0, 1] |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Fe1 | 0.00000 | 0.3055 (3) | 0.00000 | 0.0247 (11)* | 0.500000 |
In1 | 0.00000 | 0.30550 | 0.00000 | 0.0247* | 0.375000 |
Y1 | 0.00000 | 0.30550 | 0.00000 | 0.0247* | 0.125000 |
Ge1 | 0.2329 (5) | 0.00000 | 0.4110 (7) | 0.0357 (13)* | |
O1 | 0.00000 | 0.00000 | 0.50000 | 0.045 (3)* | |
O2 | 0.401 (2) | 0.00000 | 0.748 (3) | 0.0453* | |
O3 | 0.2400 (13) | 0.1674 (10) | 0.2193 (15) | 0.0453* |
Geometric parameters (Å, º) top
In1—In1i | 3.3311 | Ge1—O3vii | 1.718 (8) |
In1—O2ii | 2.087 (7) | O1—Ge1 | 1.674 (3) |
In1—O2iii | 2.087 (7) | O1—Ge1viii | 1.674 (3) |
In1—O3 | 2.070 (8) | O2—In1ix | 2.087 (7) |
In1—O3iv | 2.070 (8) | O2—In1x | 2.087 (7) |
In1—O3v | 2.210 (7) | O2—Ge1 | 1.769 (11) |
In1—O3vi | 2.210 (7) | O3—In1 | 2.070 (8) |
Fe1—In1i | 3.331 (2) | O3—In1v | 2.210 (7) |
Fe1—O2ii | 2.087 (7) | O3—Ge1 | 1.718 (8) |
Fe1—O2iii | 2.087 (7) | Y1—In1i | 3.3311 |
Fe1—O3 | 2.070 (8) | Y1—O2ii | 2.087 (7) |
Fe1—O3iv | 2.070 (8) | Y1—O2iii | 2.087 (7) |
Fe1—O3v | 2.210 (7) | Y1—O3 | 2.070 (8) |
Fe1—O3vi | 2.210 (7) | Y1—O3iv | 2.070 (8) |
Ge1—O1 | 1.674 (3) | Y1—O3v | 2.210 (7) |
Ge1—O2 | 1.769 (11) | Y1—O3vi | 2.210 (7) |
Ge1—O3 | 1.718 (8) | ||
O2ii—In1—O2iii | 74.1 (5) | In1—O3—Ge1 | 130.6 (5) |
O2ii—In1—O3 | 149.8 (4) | O2ii—Y1—O2iii | 74.1 (5) |
O2iii—In1—O3 | 92.7 (4) | O2ii—Y1—O3 | 149.8 (4) |
O2ii—In1—O3iv | 92.7 (4) | O2iii—Y1—O3 | 92.7 (4) |
O2iii—In1—O3iv | 149.8 (4) | O2ii—Y1—O3iv | 92.7 (4) |
O3—In1—O3iv | 110.3 (5) | O2iii—Y1—O3iv | 149.8 (4) |
O1—Ge1—O2 | 100.2 (5) | O3—Y1—O3iv | 110.3 (5) |
O1—Ge1—O3 | 105.9 (3) | O2ii—Y1—O3v | 78.8 (5) |
O2—Ge1—O3 | 114.9 (3) | O2iii—Y1—O3v | 91.5 (4) |
O1—Ge1—O3vii | 105.9 (3) | O3—Y1—O3v | 74.4 (3) |
O2—Ge1—O3vii | 114.9 (3) | O3iv—Y1—O3v | 112.9 (3) |
O3—Ge1—O3vii | 113.2 (6) | O2ii—Y1—O3vi | 91.5 (4) |
Ge1—O1—Ge1viii | 180 | O2iii—Y1—O3vi | 78.8 (5) |
In1ix—O2—In1x | 105.9 (5) | O3—Y1—O3vi | 112.9 (3) |
In1ix—O2—Ge1 | 126.7 (3) | O3iv—Y1—O3vi | 74.4 (3) |
In1x—O2—Ge1 | 126.7 (3) | O3v—Y1—O3vi | 168.0 (4) |
Symmetry codes: (i) −x, −y+1, −z; (ii) x−1/2, y+1/2, z−1; (iii) −x+1/2, y+1/2, −z+1; (iv) −x, y, −z; (v) −x+1/2, −y+1/2, −z; (vi) x−1/2, −y+1/2, z; (vii) x, −y, z; (viii) −x, y, −z+1; (ix) x+1/2, y−1/2, z+1; (x) −x+1/2, −y+1/2, −z+1. |
(Y50) top
Crystal data top
FeGe2In0.5O7Y0.5 | β = 101.925 (5)° |
Mr = 414.89 | V = 536.95 (7) Å3 |
Monoclinic, P121/m1 | Z = 4 |
a = 6.5986 (10) Å | Cu Kα radiation |
b = 8.5629 (5) Å | T = 300 K |
c = 9.7125 (17) Å |
Refinement top
Least-squares matrix: full | 5455 data points |
Rp = 0.056 | Profile function: Finger-Cox-Jephcoat function parameters U, V, W, X, Y, SH/L: peak variance(Gauss) = Utan(Th)2+Vtan(Th)+W: peak HW(Lorentz) = X/cos(Th)+Ytan(Th); SH/L = S/L+H/L U, V, W in (centideg)2, X & Y in centideg 2.000, -2.000, 5.000, 0.000, 0.000, 0.002, Crystallite size model "isotropic" for Fe In 0.5 Y 0.5 Ge 2 O 7 (microns) parameters: Size, G/L mix 1.000, 1.000, Mustrain model "generalized" for Fe In 0.5 Y 0.5 Ge 2 O 7 (106) parameters: S400, S040, S004, S220, S202, S022, S301, S103, S121, G/L mix 363324.362, 19218.581, 3038.642, 32193.942, 69752.738, -2025.851, 280444.257, -8436.553, 13696.591, 1.000, |
Rwp = 0.075 | 84 parameters |
Rexp = 0.032 | Background function: Background function: "chebyschev" function with 24 terms: 698(4), -45(16), -9.7(4)e2, -2.5(12)e2, -1.74(13)e3, -1.3527(25)e5, 1.2358(4)e5, 2.84050(5)e6, -1.08721(12)e6, -2.505549(20)e7, 4.87275(9)e6, 1.2061868(21)e8, -1.2843476(26)e7, -3.5081609(8)e8, 2.048631(9)e7, 6.4435235(13)e8, -1.931310(13)e7, -7.5322886(25)e8, 9.80186(10)e6, 5.4404485(24)e8, -1.982892(18)e6, -2.2156320(5)e8, -5.523(18)e4, 3.89428(4)e7, |
R(F2) = 0.06176 | Preferred orientation correction: March-Dollase correction coef. = 1.000 axis = [0, 0, 1] |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Fe1 | 0.749 (3) | 0.0506 (8) | 0.7429 (17) | 0.044 (3)* | 0.209205 |
In1 | 0.7486 | 0.0506 | 0.7429 | 0.0438* | 0.290795 |
Y1 | 0.7486 | 0.0506 | 0.7429 | 0.0438* | 0.500000 |
Fe2 | 0.764 (4) | 0.0553 (11) | 0.244 (2) | 0.036 (3)* | 0.790795 |
In2 | 0.764 | 0.0553 | 0.2441 | 0.036* | 0.209205 |
Ge1 | 0.017 (3) | 0.75000 | 0.9489 (19) | 0.020 (6)* | |
Ge2 | 0.544 (3) | 0.75000 | 0.0294 (17) | 0.010 (5)* | |
Ge3 | 0.965 (4) | 0.75000 | 0.460 (2) | 0.058 (9)* | |
Ge4 | 0.506 (4) | 0.75000 | 0.561 (3) | 0.086 (12)* | |
O1 | 0.751 (4) | 0.75000 | −0.057 (5) | 0.042 (4)* | |
O2 | 0.772 (5) | 0.75000 | 0.560 (5) | 0.042* | |
O3 | 0.172 (10) | 0.75000 | 0.119 (4) | 0.042* | |
O4 | 0.410 (6) | 0.75000 | 0.854 (3) | 0.042* | |
O5 | 0.171 (7) | 0.75000 | 0.608 (4) | 0.042* | |
O6 | 0.348 (11) | 0.75000 | 0.392 (5) | 0.042* | |
O7 | 0.019 (9) | 0.9438 (17) | 0.894 (4) | 0.042* | |
O8 | 0.519 (8) | 0.892 (4) | 0.155 (4) | 0.042* | |
O9 | 0.932 (9) | 0.923 (3) | 0.364 (4) | 0.042* | |
O10 | 0.455 (9) | 0.920 (3) | 0.648 (5) | 0.042* |
Geometric parameters (Å, º) top
Fe1—Fe2i | 3.32 (2) | Ge1—O7xi | 1.743 (8) |
Fe1—O1ii | 3.22 (3) | Ge2—O1 | 1.746 (8) |
Fe1—O2iii | 3.15 (3) | Ge2—O4xii | 1.751 (8) |
Fe1—O3iv | 2.17 (2) | Ge2—O8 | 1.750 (8) |
Fe1—O6iv | 2.17 (2) | Ge2—O8xi | 1.750 (8) |
Fe1—O7v | 2.26 (5) | Ge3—O2 | 1.757 (8) |
Fe1—O8vi | 2.25 (3) | Ge3—O5xiii | 1.758 (8) |
Fe1—O9vii | 2.54 (5) | Ge3—O9 | 1.745 (8) |
Fe1—O10iii | 2.26 (5) | Ge3—O9xi | 1.745 (8) |
In1—Fe2i | 3.32 (2) | Ge4—O2 | 1.758 (8) |
In1—O3iv | 2.169 (18) | Ge4—O6 | 1.750 (8) |
In1—O6iv | 2.17 (2) | Ge4—O10 | 1.748 (8) |
In1—O7v | 2.26 (5) | Ge4—O10xi | 1.748 (8) |
In1—O8vi | 2.25 (4) | O1—Ge1xiv | 1.744 (8) |
In1—O9vii | 2.54 (5) | O1—Ge2 | 1.746 (8) |
In1—O10iii | 2.26 (5) | O2—Ge3 | 1.757 (8) |
Y1—Fe2i | 3.32 (2) | O2—Ge4 | 1.758 (8) |
Y1—O3iv | 2.169 (18) | O3—Fe1xv | 2.17 (2) |
Y1—O6iv | 2.17 (2) | O3—Fe1vi | 2.17 (2) |
Y1—O7v | 2.26 (5) | O3—Ge1xii | 1.751 (8) |
Y1—O8vi | 2.25 (4) | O4—Fe2xv | 2.13 (2) |
Y1—O9vii | 2.54 (5) | O4—Fe2vi | 2.13 (2) |
Y1—O10iii | 2.26 (5) | O4—Ge2x | 1.751 (8) |
Fe2—Fe1i | 3.32 (2) | O5—Fe2xv | 2.19 (3) |
Fe2—Fe2viii | 3.335 (19) | O5—Fe2vi | 2.19 (3) |
Fe2—O4iv | 2.13 (2) | O5—Ge3xvi | 1.758 (8) |
Fe2—O5iv | 2.19 (3) | O6—Fe1xv | 2.17 (2) |
Fe2—O7vi | 2.16 (4) | O6—Fe1vi | 2.17 (2) |
Fe2—O8iii | 2.18 (4) | O6—Ge4 | 1.750 (8) |
Fe2—O9iii | 1.83 (3) | O7—Fe1xvii | 2.26 (5) |
Fe2—O10vi | 1.96 (4) | O7—Fe2vi | 2.16 (4) |
In2—Fe1i | 3.320 (18) | O7—Ge1 | 1.743 (8) |
In2—Fe2viii | 3.335 (9) | O8—Fe1vi | 2.25 (3) |
In2—O4iv | 2.133 (17) | O8—Fe2xviii | 2.18 (4) |
In2—O5iv | 2.19 (3) | O8—Ge2 | 1.750 (8) |
In2—O7vi | 2.16 (4) | O9—Fe1vii | 2.54 (5) |
In2—O8iii | 2.18 (4) | O9—Fe2xviii | 1.83 (3) |
In2—O9iii | 1.83 (3) | O9—Ge3 | 1.745 (8) |
In2—O10vi | 1.96 (4) | O10—Fe1xviii | 2.26 (5) |
Ge1—O1ix | 1.744 (8) | O10—Fe2vi | 1.96 (4) |
Ge1—O3x | 1.751 (8) | O10—Ge4 | 1.748 (8) |
Ge1—O7 | 1.743 (8) | ||
O3iv—Y1—O6iv | 76.1 (6) | O1—Ge2—O4xii | 79 (2) |
O3iv—Y1—O7v | 81.8 (12) | O1—Ge2—O8 | 122 (2) |
O6iv—Y1—O7v | 144.0 (18) | O4xii—Ge2—O8 | 125 (2) |
O3iv—Y1—O8vi | 71 (2) | O1—Ge2—O8xi | 122 (2) |
O6iv—Y1—O8vi | 86 (2) | O4xii—Ge2—O8xi | 125 (2) |
O7v—Y1—O8vi | 112.7 (17) | O8—Ge2—O8xi | 88 (3) |
O3iv—Y1—O10iii | 136 (2) | O2—Ge3—O5xiii | 95 (2) |
O6iv—Y1—O10iii | 91.2 (17) | O2—Ge3—O9 | 106 (2) |
O7v—Y1—O10iii | 124.1 (9) | O5xiii—Ge3—O9 | 115 (2) |
O8vi—Y1—O10iii | 66.8 (11) | O2—Ge3—O9xi | 106 (2) |
O4iv—In2—O7vi | 95.0 (15) | O5xiii—Ge3—O9xi | 115 (2) |
O4iv—In2—O9iii | 165.7 (14) | O9—Ge3—O9xi | 116 (3) |
O7vi—In2—O9iii | 90.1 (17) | O2—Ge4—O6 | 113 (4) |
O4iv—In2—O10vi | 76.4 (16) | O2—Ge4—O10 | 107 (2) |
O7vi—In2—O10vi | 171 (2) | O6—Ge4—O10 | 109 (3) |
O9iii—In2—O10vi | 98 (2) | O2—Ge4—O10xi | 107 (2) |
O1ix—Ge1—O3x | 115 (4) | O6—Ge4—O10xi | 109 (3) |
O1ix—Ge1—O7 | 93.5 (19) | O10—Ge4—O10xi | 113 (3) |
O3x—Ge1—O7 | 104 (2) | Ge1xiv—O1—Ge2 | 150 (3) |
O1ix—Ge1—O7xi | 93.5 (19) | Ge3—O2—Ge4 | 148 (4) |
O3x—Ge1—O7xi | 104 (2) | Fe2xviii—O9—Ge3 | 149 (4) |
O7—Ge1—O7xi | 144 (3) |
Symmetry codes: (i) −x+2, −y, −z+1; (ii) x, y−1, z+1; (iii) x, y−1, z; (iv) −x+1, y−1/2, −z+1; (v) x+1, y−1, z; (vi) −x+1, −y+1, −z+1; (vii) −x+2, −y+1, −z+1; (viii) x, −y+3/2, z; (ix) x−1, y, z+1; (x) x, y, z+1; (xi) x, −y+5/2, z; (xii) x, y, z−1; (xiii) x+1, y, z; (xiv) x+1, y, z−1; (xv) −x+1, y+1/2, −z+1; (xvi) x−1, y, z; (xvii) x−1, y+1, z; (xviii) x, y+1, z. |
(Y75) top
Crystal data top
FeGe2In0.25O7Y0.75 | β = 101.218 (3)° |
Mr = 408.41 | V = 540.75 (6) Å3 |
Monoclinic, P121/m1 | Z = 4 |
a = 6.6484 (7) Å | Cu Kα radiation |
b = 8.5648 (4) Å | T = 300 K |
c = 9.6815 (11) Å |
Refinement top
Least-squares matrix: full | 5455 data points |
Rp = 0.054 | Profile function: Finger-Cox-Jephcoat function parameters U, V, W, X, Y, SH/L: peak variance(Gauss) = Utan(Th)2+Vtan(Th)+W: peak HW(Lorentz) = X/cos(Th)+Ytan(Th); SH/L = S/L+H/L U, V, W in (centideg)2, X & Y in centideg 2.000, -2.000, 5.000, 0.000, 0.000, 0.002, Crystallite size model "isotropic" for Fe In 0.25 Y 0.75 Ge 2 O 7 (microns) parameters: Size, G/L mix 1(20)e1, 1.000, Mustrain model "generalized" for Fe In 0.25 Y 0.75 Ge 2 O 7 (106) parameters: S400, S040, S004, S220, S202, S022, S301, S103, S121, G/L mix 108071.203, 14067.607, 3272.259, 16254.503, 24931.495, -284.193, 78003.264, 2546.782, -542.581, 1.000, |
Rwp = 0.075 | 93 parameters |
Rexp = 0.032 | Background function: Background function: "chebyschev" function with 32 terms: 691(4), 49(12), -5.09(5)e3, -3.031(8)e4, 1.8487(22)e5, 1.68572(11)e6, -2.99915(19)e6, -4.145656(7)e7, 2.704722(21)e7, 5.5800223(4)e8, -1.6257405(6)e8, -4.62843601(9)e9, 7.5633787(18)e8, 2.540510150(10)e10, -2.90892201(23)e9, -9.653089526(7)e10, 8.98161040(17)e9, 2.61078082580(26)e11, -2.102414170(6)e10, -5.1007652553(6)e11, 3.581457900(13)e10, 7.2210372140(10)e11, -4.317915902(24)e10, -7.3385632605(12)e11, 3.572028764(27)e10, 5.2188253926(10)e11, -1.924956594(19)e10, -2.4656056517(5)e11, 6.08179886(5)e9, 6.951635866(6)e10, -8.544791(4)e8, -8.85125663(19)e9, |
R(F2) = 0.05021 | Preferred orientation correction: March-Dollase correction coef. = 1.000 axis = [0, 0, 1] |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Fe1 | 0.756 (3) | 0.0451 (6) | 0.7535 (17) | 0.042 (2)* | 0.0500000 |
In1 | 0.7561 | 0.0451 | 0.7535 | 0.0418* | 0.200000 |
Y1 | 0.7561 | 0.0451 | 0.7535 | 0.0418* | 0.750000 |
Fe2 | 0.760 (5) | 0.0552 (9) | 0.252 (3) | 0.028 (3)* | 0.950000 |
In2 | 0.760 | 0.0552 | 0.2519 | 0.0279* | 0.0500000 |
Ge1 | 0.014 (3) | 0.75000 | 0.954 (2) | 0.032 (8)* | |
Ge2 | 0.540 (4) | 0.75000 | 0.0296 (18) | 0.007 (6)* | |
Ge3 | 0.953 (5) | 0.75000 | 0.470 (2) | 0.057 (10)* | |
Ge4 | 0.483 (3) | 0.75000 | 0.562 (2) | 0.028 (8)* | |
O1 | 0.747 (4) | 0.75000 | −0.060 (5) | 0.045 (3)* | |
O2 | 0.746 (4) | 0.75000 | 0.558 (6) | 0.045* | |
O3 | 0.175 (8) | 0.75000 | 0.119 (3) | 0.045* | |
O4 | 0.358 (10) | 0.75000 | 0.873 (5) | 0.045* | |
O5 | 0.152 (9) | 0.75000 | 0.618 (6) | 0.045* | |
O6 | 0.379 (9) | 0.75000 | 0.382 (2) | 0.045* | |
O7 | 0.031 (10) | 0.915 (3) | 0.851 (4) | 0.045* | |
O8 | 0.552 (8) | 0.898 (3) | 0.155 (3) | 0.045* | |
O9 | 0.952 (9) | 0.923 (3) | 0.374 (3) | 0.045* | |
O10 | 0.447 (10) | 0.939 (2) | 0.622 (4) | 0.045* |
Geometric parameters (Å, º) top
Fe1—Fe2i | 3.34 (3) | Ge1—O7xi | 1.742 (8) |
Fe1—O1ii | 3.12 (3) | Ge2—O1 | 1.758 (8) |
Fe1—O2iii | 3.15 (3) | Ge2—O4xii | 1.750 (8) |
Fe1—O3iv | 2.143 (16) | Ge2—O8 | 1.743 (8) |
Fe1—O6iv | 2.270 (19) | Ge2—O8xi | 1.743 (8) |
Fe1—O7v | 2.19 (6) | Ge3—O2 | 1.760 (8) |
Fe1—O8vi | 2.44 (5) | Ge3—O5xiii | 1.751 (8) |
Fe1—O9vii | 2.51 (5) | Ge3—O9 | 1.745 (8) |
Fe1—O10iii | 2.38 (6) | Ge3—O9xi | 1.745 (8) |
In1—Fe2i | 3.34 (3) | Ge4—O2 | 1.755 (8) |
In1—O3iv | 2.143 (15) | Ge4—O6 | 1.746 (8) |
In1—O6iv | 2.270 (17) | Ge4—O10 | 1.751 (8) |
In1—O7v | 2.19 (6) | Ge4—O10xi | 1.751 (8) |
In1—O8vi | 2.44 (5) | O1—Ge1xiv | 1.753 (8) |
In1—O9vii | 2.51 (5) | O1—Ge2 | 1.758 (8) |
In1—O10iii | 2.38 (6) | O2—Ge3 | 1.760 (8) |
Y1—Fe2i | 3.34 (3) | O2—Ge4 | 1.755 (8) |
Y1—O3iv | 2.143 (15) | O3—Fe1xv | 2.143 (16) |
Y1—O6iv | 2.270 (17) | O3—Fe1vi | 2.143 (16) |
Y1—O7v | 2.19 (6) | O3—Ge1xii | 1.745 (8) |
Y1—O8vi | 2.44 (5) | O4—Fe2xv | 2.12 (2) |
Y1—O9vii | 2.51 (5) | O4—Fe2vi | 2.12 (2) |
Y1—O10iii | 2.38 (6) | O4—Ge2x | 1.750 (8) |
Fe2—Fe1i | 3.34 (3) | O5—Fe2xv | 2.10 (3) |
Fe2—Fe2viii | 3.336 (15) | O5—Fe2vi | 2.10 (3) |
Fe2—O4iv | 2.12 (2) | O5—Ge3xvi | 1.751 (8) |
Fe2—O5iv | 2.10 (3) | O6—Fe1xv | 2.270 (19) |
Fe2—O7vi | 1.88 (6) | O6—Fe1vi | 2.270 (19) |
Fe2—O8iii | 2.03 (4) | O6—Ge4 | 1.746 (8) |
Fe2—O9iii | 1.93 (5) | O7—Fe1xvii | 2.19 (6) |
Fe2—O10vi | 2.01 (6) | O7—Fe2vi | 1.88 (6) |
In2—Fe1i | 3.338 (18) | O7—Ge1 | 1.742 (8) |
In2—Fe2viii | 3.336 (8) | O8—Fe1vi | 2.44 (5) |
In2—O4iv | 2.118 (17) | O8—Fe2xviii | 2.03 (4) |
In2—O5iv | 2.10 (3) | O8—Ge2 | 1.743 (8) |
In2—O7vi | 1.88 (5) | O9—Fe1vii | 2.51 (5) |
In2—O8iii | 2.03 (4) | O9—Fe2xviii | 1.93 (5) |
In2—O9iii | 1.93 (4) | O9—Ge3 | 1.745 (8) |
In2—O10vi | 2.01 (5) | O10—Fe1xviii | 2.38 (6) |
Ge1—O1ix | 1.753 (8) | O10—Fe2vi | 2.01 (6) |
Ge1—O3x | 1.745 (8) | O10—Ge4 | 1.751 (8) |
Ge1—O7 | 1.742 (8) | ||
O3iv—Y1—O6iv | 73.5 (4) | O3x—Ge1—O7xi | 115 (2) |
O3iv—Y1—O7v | 95.9 (14) | O7—Ge1—O7xi | 108 (3) |
O6iv—Y1—O7v | 147.8 (18) | O1—Ge2—O4xii | 93 (3) |
O4iv—In2—O5iv | 75.2 (5) | O1—Ge2—O8 | 114 (3) |
O4iv—In2—O7vi | 80 (2) | O4xii—Ge2—O8 | 122 (2) |
O5iv—In2—O7vi | 93 (3) | O1—Ge2—O8xi | 114 (3) |
O4iv—In2—O8iii | 96.6 (14) | O4xii—Ge2—O8xi | 122 (2) |
O5iv—In2—O8iii | 153 (2) | O8—Ge2—O8xi | 93 (3) |
O7vi—In2—O8iii | 110.7 (16) | O2—Ge3—O5xiii | 98 (3) |
O4iv—In2—O9iii | 160 (2) | O2—Ge3—O9 | 110 (3) |
O5iv—In2—O9iii | 91.5 (13) | O5xiii—Ge3—O9 | 111 (2) |
O7vi—In2—O9iii | 86 (2) | O2—Ge3—O9xi | 110 (3) |
O8iii—In2—O9iii | 101.7 (10) | O5xiii—Ge3—O9xi | 111 (2) |
O4iv—In2—O10vi | 96 (2) | O9—Ge3—O9xi | 116 (3) |
O5iv—In2—O10vi | 76 (2) | O2—Ge4—O6 | 100 (3) |
O7vi—In2—O10vi | 169.4 (15) | O2—Ge4—O10 | 102 (2) |
O8iii—In2—O10vi | 79.2 (16) | O6—Ge4—O10 | 106.1 (15) |
O9iii—In2—O10vi | 95.3 (18) | O2—Ge4—O10xi | 102 (2) |
O1ix—Ge1—O3x | 120 (3) | O6—Ge4—O10xi | 106.1 (15) |
O1ix—Ge1—O7 | 98 (3) | O10—Ge4—O10xi | 135 (3) |
O3x—Ge1—O7 | 115 (2) | Ge1xiv—O1—Ge2 | 147 (3) |
O1ix—Ge1—O7xi | 98 (3) | Ge3—O2—Ge4 | 153 (4) |
Symmetry codes: (i) −x+2, −y, −z+1; (ii) x, y−1, z+1; (iii) x, y−1, z; (iv) −x+1, y−1/2, −z+1; (v) x+1, y−1, z; (vi) −x+1, −y+1, −z+1; (vii) −x+2, −y+1, −z+1; (viii) x, −y+3/2, z; (ix) x−1, y, z+1; (x) x, y, z+1; (xi) x, −y+5/2, z; (xii) x, y, z−1; (xiii) x+1, y, z; (xiv) x+1, y, z−1; (xv) −x+1, y+1/2, −z+1; (xvi) x−1, y, z; (xvii) x−1, y+1, z; (xviii) x, y+1, z. |
(Y90) top
Crystal data top
FeGe2In0.1O7Y0.9 | β = 100.899 (2)° |
Mr = 404.52 | V = 541.36 (4) Å3 |
Monoclinic, P121/m1 | Z = 4 |
a = 6.6659 (5) Å | Cu Kα radiation |
b = 8.5545 (3) Å | T = 300 K |
c = 9.6680 (8) Å |
Refinement top
Least-squares matrix: full | 5455 data points |
Rp = 0.053 | Profile function: Finger-Cox-Jephcoat function parameters U, V, W, X, Y, SH/L: peak variance(Gauss) = Utan(Th)2+Vtan(Th)+W: peak HW(Lorentz) = X/cos(Th)+Ytan(Th); SH/L = S/L+H/L U, V, W in (centideg)2, X & Y in centideg 2.000, -2.000, 5.000, 0.000, 0.000, 0.002, Crystallite size model "isotropic" for Fe In 0.10 Y 0.90 Ge 2 O 7 (microns) parameters: Size, G/L mix 1.000, 1.000, Mustrain model "generalized" for Fe In 0.10 Y 0.90 Ge 2 O 7 (106) parameters: S400, S040, S004, S220, S202, S022, S301, S103, S121, G/L mix 24582.801, 10580.820, 2071.679, 7559.181, 9245.186, -470.066, 16767.908, 2602.016, -2305.206, 1.000, |
Rwp = 0.076 | 94 parameters |
Rexp = 0.028 | Background function: Background function: "chebyschev" function with 34 terms: 916(4), 282(14), -4.07(6)e3, -2.877(9)e4, 1.3902(25)e5, 1.32610(11)e6, -4.09034(19)e6, -3.268858(9)e7, 8.151639(25)e7, 4.6106403(3)e8, -1.00723582(8)e9, -4.04323665(10)e9, 7.97281661(17)e9, 2.352511227(12)e10, -4.235044064(26)e10, -9.514506238(9)e10, 1.5662125942(23)e11, 2.7601939015(4)e11, -4.1335033609(12)e11, -5.8550265765(5)e11, 7.8900705436(8)e11, 9.1607173493(10)e11, -1.09197621774(21)e12, -1.05563394588(13)e12, 1.08527814898(30)e12, 8.8443686334(13)e11, -7.5494223724(29)e11, -5.2358178330(10)e11, 3.4893986655(17)e11, 2.0737233362(3)e11, -9.626609758(10)e10, -4.923987886(8)e10, 1.19958581(5)e10, 5.29145728(23)e9, |
R(F2) = 0.06570 | Preferred orientation correction: March-Dollase correction coef. = 1.000 axis = [0, 0, 1] |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Fe1 | 0.744 (2) | 0.0475 (6) | 0.7464 (15) | 0.0328 (18)* | 0.0500000 |
In1 | 0.7438 | 0.0475 | 0.7464 | 0.0328* | 0.0500000 |
Y1 | 0.7438 | 0.0475 | 0.7464 | 0.0328* | 0.900000 |
Fe2 | 0.756 (3) | 0.0506 (9) | 0.245 (2) | 0.031 (3)* | 0.950000 |
In2 | 0.756 | 0.0506 | 0.2453 | 0.0308* | 0.0500000 |
Ge1 | 0.004 (3) | 0.75000 | 0.935 (2) | 0.078 (9)* | |
Ge2 | 0.548 (3) | 0.75000 | 0.0292 (19) | 0.012 (5)* | |
Ge3 | 0.958 (3) | 0.75000 | 0.471 (2) | 0.031 (7)* | |
Ge4 | 0.474 (2) | 0.75000 | 0.5505 (15) | 0.003 (4)* | |
O1 | 0.737 (4) | 0.75000 | −0.077 (4) | 0.035 (3)* | |
O2 | 0.733 (4) | 0.75000 | 0.540 (6) | 0.0346* | |
O3 | 0.128 (10) | 0.75000 | 0.113 (3) | 0.0346* | |
O4 | 0.336 (9) | 0.75000 | 0.891 (6) | 0.0346* | |
O5 | 0.158 (9) | 0.75000 | 0.618 (6) | 0.0346* | |
O6 | 0.383 (10) | 0.75000 | 0.368 (2) | 0.0346* | |
O7 | 0.040 (7) | 0.942 (2) | 0.882 (3) | 0.0346* | |
O8 | 0.552 (10) | 0.914 (4) | 0.137 (4) | 0.0346* | |
O9 | 0.964 (9) | 0.917 (4) | 0.372 (4) | 0.0346* | |
O10 | 0.480 (7) | 0.908 (3) | 0.663 (3) | 0.0346* |
Geometric parameters (Å, º) top
Fe1—O1i | 3.08 (2) | Ge2—O8 | 1.745 (9) |
Fe1—O2ii | 3.22 (3) | Ge2—O8ix | 1.745 (9) |
Fe1—O3iii | 2.269 (17) | Ge3—O2 | 1.750 (9) |
Fe1—O6iii | 2.143 (18) | Ge3—O5xi | 1.754 (9) |
Fe1—O7iv | 2.34 (4) | Ge3—O9 | 1.728 (9) |
Fe1—O8v | 2.47 (6) | Ge3—O9ix | 1.728 (9) |
Fe1—O9vi | 2.45 (6) | Ge4—O2 | 1.747 (9) |
Fe1—O10ii | 2.15 (4) | Ge4—O6 | 1.751 (9) |
In1—O3iii | 2.269 (16) | Ge4—O10 | 1.736 (9) |
In1—O6iii | 2.143 (18) | Ge4—O10ix | 1.736 (9) |
In1—O7iv | 2.34 (4) | O1—Ge1xii | 1.764 (9) |
In1—O8v | 2.47 (6) | O1—Ge2 | 1.769 (9) |
In1—O9vi | 2.45 (5) | O2—Ge3 | 1.750 (9) |
In1—O10ii | 2.15 (4) | O2—Ge4 | 1.747 (9) |
Y1—O3iii | 2.269 (16) | O3—Fe1xiii | 2.269 (17) |
Y1—O6iii | 2.143 (18) | O3—Fe1v | 2.269 (17) |
Y1—O7iv | 2.34 (4) | O3—Ge1x | 1.758 (9) |
Y1—O8v | 2.47 (6) | O4—Fe2xiii | 2.17 (3) |
Y1—O9vi | 2.45 (5) | O4—Fe2v | 2.17 (3) |
Y1—O10ii | 2.15 (4) | O4—Ge2viii | 1.752 (9) |
Fe2—O4iii | 2.17 (3) | O5—Fe2xiii | 2.17 (3) |
Fe2—O5iii | 2.17 (3) | O5—Fe2v | 2.17 (3) |
Fe2—O7v | 2.00 (5) | O5—Ge3xiv | 1.754 (9) |
Fe2—O8ii | 1.94 (4) | O6—Fe1xiii | 2.143 (18) |
Fe2—O9ii | 2.02 (4) | O6—Fe1v | 2.143 (18) |
Fe2—O10v | 1.97 (5) | O6—Ge4 | 1.751 (9) |
In2—O4iii | 2.17 (3) | O7—Fe1xv | 2.34 (4) |
In2—O5iii | 2.17 (3) | O7—Fe2v | 2.00 (5) |
In2—O7v | 2.00 (4) | O7—Ge1 | 1.748 (9) |
In2—O8ii | 1.94 (4) | O8—Fe1v | 2.47 (6) |
In2—O9ii | 2.02 (4) | O8—Fe2xvi | 1.94 (4) |
In2—O10v | 1.97 (4) | O8—Ge2 | 1.745 (9) |
Ge1—O1vii | 1.764 (9) | O9—Fe1vi | 2.45 (6) |
Ge1—O3viii | 1.758 (9) | O9—Fe2xvi | 2.02 (4) |
Ge1—O7 | 1.748 (9) | O9—Ge3 | 1.728 (9) |
Ge1—O7ix | 1.748 (9) | O10—Fe1xvi | 2.15 (4) |
Ge2—O1 | 1.769 (9) | O10—Fe2v | 1.97 (5) |
Ge2—O4x | 1.752 (9) | O10—Ge4 | 1.736 (9) |
O6iii—In1—O10ii | 92.2 (16) | O4x—Ge2—O8 | 112 (2) |
O3iii—Y1—O6iii | 76.2 (5) | O1—Ge2—O8ix | 115 (3) |
O3iii—Y1—O10ii | 147 (2) | O4x—Ge2—O8ix | 112 (2) |
O6iii—Y1—O10ii | 92.2 (16) | O8—Ge2—O8ix | 107 (3) |
O7v—In2—O8ii | 100.1 (17) | O2—Ge3—O5xi | 105 (3) |
O7v—In2—O9ii | 85.4 (19) | O2—Ge3—O9 | 109 (3) |
O8ii—In2—O9ii | 108.4 (9) | O5xi—Ge3—O9 | 111 (2) |
O7v—In2—O10v | 163.9 (15) | O2—Ge3—O9ix | 109 (3) |
O8ii—In2—O10v | 79.3 (18) | O5xi—Ge3—O9ix | 111 (2) |
O9ii—In2—O10v | 110.2 (18) | O9—Ge3—O9ix | 112 (4) |
O1vii—Ge1—O3viii | 110 (3) | O2—Ge4—O6 | 96 (3) |
O1vii—Ge1—O7 | 99.9 (17) | O2—Ge4—O10 | 97.7 (18) |
O3viii—Ge1—O7 | 102.8 (13) | O6—Ge4—O10 | 126.5 (14) |
O1vii—Ge1—O7ix | 99.9 (17) | O2—Ge4—O10ix | 97.7 (18) |
O3viii—Ge1—O7ix | 102.8 (13) | O6—Ge4—O10ix | 126.5 (14) |
O7—Ge1—O7ix | 140 (3) | O10—Ge4—O10ix | 103 (2) |
O1—Ge2—O4x | 97 (3) | Ge1xii—O1—Ge2 | 141 (3) |
O1—Ge2—O8 | 115 (3) | Ge3—O2—Ge4 | 161 (4) |
Symmetry codes: (i) x, y−1, z+1; (ii) x, y−1, z; (iii) −x+1, y−1/2, −z+1; (iv) x+1, y−1, z; (v) −x+1, −y+1, −z+1; (vi) −x+2, −y+1, −z+1; (vii) x−1, y, z+1; (viii) x, y, z+1; (ix) x, −y+5/2, z; (x) x, y, z−1; (xi) x+1, y, z; (xii) x+1, y, z−1; (xiii) −x+1, y+1/2, −z+1; (xiv) x−1, y, z; (xv) x−1, y+1, z; (xvi) x, y+1, z. |