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The discovery of a new quaternary intermetallic compound of composition Zr3Mn3Sn4Ga during a survey of the Zr–Mn–Sn–Ga phase diagram is reported. Single-crystal X-ray diffraction reveals that the new compound crystallizes in a hexagonal lattice (space group P63/mmc, No. 194). The analysis of single-crystal X-ray diffraction data indicates that the atomic arrangement is an ordered variant of the high-temperature hexagonal Ti6Sn5 crystal structure. From a simple geometry point of view, the unit cell consists of GaZr3 octahedra chains and Mn chains growing along the sixfold symmetry axis c. The Mn chains are stacked within the ab basal plane in a kagome geometry, with large interatomic distances. The possible slight levels of Sn/Ga and Zr/Mn mixed occupancy based on additional results of electron probe microanalysis and single-crystal neutron diffraction are discussed. It is noteworthy that this compound is the first quaternary intermetallic discovered in this structure and the first Ti6Sn5 derivative bearing a magnetic metal, namely Mn, in the 6g position, which may give rise to interesting physical properties.
Supporting information
CCDC references: 2209554; 2211262; 2211263; 2211264
Cell refinement: SAINT V8.38A (Bruker, 2018) for zrmnsnga_300k, zrmnsnga_100k. Data reduction: SAINT V8.38A (Bruker, 2018) for zrmnsnga_300k, zrmnsnga_100k; DATARED (CFML-v.1) for ZrMnGaSn_neutron1, ZrMnGaSn_neutron2. Program(s) used to solve structure: SHELXS (Sheldrick, 2008) for zrmnsnga_300k, zrmnsnga_100k. Program(s) used to refine structure: SHELXL 2018/3 (Sheldrick, 2015) for zrmnsnga_300k, zrmnsnga_100k; FULLPROF for ZrMnGaSn_neutron1, ZrMnGaSn_neutron2. Molecular graphics: Olex2 1.3 (Dolomanov et al., 2009) for zrmnsnga_300k, zrmnsnga_100k. Software used to prepare material for publication: Olex2 1.3 (Dolomanov et al., 2009) for zrmnsnga_300k, zrmnsnga_100k.
Crystal data top
GaMn3Sn4Zr3 | Dx = 7.900 Mg m−3 |
Mr = 982.96 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63/mmc | Cell parameters from 9785 reflections |
a = 9.2073 (4) Å | θ = 4.4–43.1° |
c = 5.6287 (2) Å | µ = 22.99 mm−1 |
V = 413.24 (4) Å3 | T = 300 K |
Z = 2 | Needle, metallic gray |
F(000) = 852 | 0.11 × 0.10 × 0.09 mm |
Data collection top
Bruker APEX-II CCD diffractometer | 622 reflections with I > 2σ(I) |
φ and ω scans | Rint = 0.033 |
Absorption correction: multi-scan SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1473 before and 0.0451 after correction.
The Ratio of minimum to maximum transmission is 0.6136.
The λ/2 correction factor is Not present. | θmax = 43.2°, θmin = 2.6° |
Tmin = 0.459, Tmax = 0.749 | h = −17→17 |
36702 measured reflections | k = −17→17 |
622 independent reflections | l = −10→10 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0039P)2 + 2.0701P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.015 | (Δ/σ)max < 0.001 |
wR(F2) = 0.033 | Δρmax = 1.26 e Å−3 |
S = 1.36 | Δρmin = −1.43 e Å−3 |
622 reflections | Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
18 parameters | Extinction coefficient: 0.0072 (3) |
0 restraints | |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Sn1(6h) | 0.78917 (3) | 0.57834 (2) | 0.250000 | 0.00638 (5) | |
Sn2(2c) | 0.333333 | 0.666667 | 0.250000 | 0.00726 (6) | |
Zr1(6h) | 0.14705 (4) | 0.29409 (2) | 0.250000 | 0.00518 (6) | |
Ga1(2a) | 0.000000 | 0.000000 | 0.000000 | 0.00595 (9) | |
Mn1(6g) | 0.500000 | 0.000000 | 0.000000 | 0.00660 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn1(6h) | 0.00591 (6) | 0.00809 (8) | 0.00585 (7) | 0.00405 (4) | 0.00000 | 0.00000 |
Sn2(2c) | 0.00545 (8) | 0.00545 (8) | 0.01089 (14) | 0.00273 (4) | 0.00000 | 0.00000 |
Zr1(6h) | 0.00583 (8) | 0.00445 (10) | 0.00480 (10) | 0.00223 (5) | 0.00000 | 0.00000 |
Ga1(2a) | 0.00602 (13) | 0.00602 (13) | 0.0058 (2) | 0.00301 (6) | 0.00000 | 0.00000 |
Mn1(6g) | 0.00603 (11) | 0.00742 (16) | 0.00680 (15) | 0.00371 (8) | −0.00088 (7) | −0.00177 (13) |
Geometric parameters (Å, º) top
Sn1—Zr1i | 2.9865 (2) | Sn2—Mn1xi | 3.0074 (1) |
Sn1—Zr1 | 2.9926 (2) | Sn2—Mn1xii | 3.0074 (1) |
Sn1—Zr1ii | 2.9865 (2) | Sn2—Mn1iv | 3.0074 (1) |
Sn1—Zr1iii | 2.9926 (2) | Zr1—Zr1ii | 3.6633 (2) |
Sn1—Mn1iv | 2.7692 (1) | Zr1—Ga1 | 2.7348 (3) |
Sn1—Mn1v | 2.7692 (1) | Zr1—Ga1ii | 2.7348 (3) |
Sn1—Mn1 | 2.7692 (1) | Zr1—Mn1iv | 3.1582 (2) |
Sn1—Mn1vi | 2.7692 (1) | Zr1—Mn1x | 3.1582 (2) |
Sn2—Zr1vii | 2.9708 (3) | Zr1—Mn1v | 3.1582 (2) |
Sn2—Zr1viii | 2.9708 (3) | Zr1—Mn1xi | 3.1582 (2) |
Sn2—Zr1 | 2.9708 (3) | Ga1—Ga1ii | 2.8144 (1) |
Sn2—Mn1ix | 3.0074 (1) | Ga1—Ga1v | 2.8144 (1) |
Sn2—Mn1x | 3.0074 (1) | Mn1—Mn1xiii | 2.8144 (1) |
Sn2—Mn1v | 3.0074 (1) | Mn1—Mn1iv | 2.8144 (1) |
| | | |
Zr1i—Sn1—Zr1ii | 85.687 (14) | Ga1ii—Zr1—Mn1v | 102.504 (3) |
Zr1ii—Sn1—Zr1 | 75.567 (7) | Ga1—Zr1—Mn1x | 102.504 (3) |
Zr1i—Sn1—Zr1 | 75.567 (7) | Ga1—Zr1—Mn1xi | 102.504 (3) |
Zr1i—Sn1—Zr1iii | 75.567 (7) | Ga1—Zr1—Mn1iv | 132.457 (5) |
Zr1—Sn1—Zr1iii | 140.255 (15) | Ga1ii—Zr1—Mn1iv | 102.504 (3) |
Zr1ii—Sn1—Zr1iii | 75.568 (7) | Ga1ii—Zr1—Mn1xi | 132.457 (5) |
Mn1vi—Sn1—Zr1ii | 66.432 (5) | Ga1—Zr1—Mn1v | 132.457 (5) |
Mn1iv—Sn1—Zr1ii | 136.937 (7) | Ga1ii—Zr1—Mn1x | 132.457 (5) |
Mn1—Sn1—Zr1ii | 136.937 (7) | Mn1v—Zr1—Zr1ii | 54.552 (5) |
Mn1v—Sn1—Zr1ii | 66.432 (5) | Mn1xi—Zr1—Zr1ii | 155.888 (6) |
Mn1—Sn1—Zr1iii | 66.346 (3) | Mn1iv—Zr1—Zr1ii | 103.187 (4) |
Mn1iv—Sn1—Zr1i | 66.432 (5) | Mn1x—Zr1—Zr1ii | 96.007 (4) |
Mn1v—Sn1—Zr1i | 136.937 (7) | Mn1v—Zr1—Mn1x | 52.918 (4) |
Mn1—Sn1—Zr1i | 66.432 (5) | Mn1x—Zr1—Mn1iv | 117.352 (10) |
Mn1iv—Sn1—Zr1iii | 123.680 (2) | Mn1v—Zr1—Mn1iv | 93.578 (7) |
Mn1vi—Sn1—Zr1i | 136.937 (7) | Mn1v—Zr1—Mn1xi | 117.352 (10) |
Mn1v—Sn1—Zr1iii | 123.681 (2) | Mn1x—Zr1—Mn1xi | 93.578 (7) |
Mn1vi—Sn1—Zr1 | 123.680 (2) | Mn1iv—Zr1—Mn1xi | 52.918 (4) |
Mn1v—Sn1—Zr1 | 66.346 (3) | Zr1xiv—Ga1—Zr1xv | 95.904 (5) |
Mn1iv—Sn1—Zr1 | 66.346 (3) | Zr1xvi—Ga1—Zr1xvii | 95.904 (5) |
Mn1—Sn1—Zr1 | 123.680 (2) | Zr1xiv—Ga1—Zr1xvii | 84.096 (5) |
Mn1vi—Sn1—Zr1iii | 66.346 (3) | Zr1xvii—Ga1—Zr1xv | 180.0 |
Mn1—Sn1—Mn1v | 153.928 (9) | Zr1—Ga1—Zr1xvii | 84.096 (5) |
Mn1—Sn1—Mn1vi | 112.447 (4) | Zr1v—Ga1—Zr1xvii | 95.904 (5) |
Mn1iv—Sn1—Mn1vi | 153.928 (9) | Zr1xvi—Ga1—Zr1xv | 84.096 (5) |
Mn1vi—Sn1—Mn1v | 61.081 (3) | Zr1xiv—Ga1—Zr1v | 180.0 |
Mn1iv—Sn1—Mn1 | 61.081 (3) | Zr1—Ga1—Zr1xv | 95.904 (5) |
Mn1iv—Sn1—Mn1v | 112.447 (4) | Zr1xvi—Ga1—Zr1 | 180.0 |
Zr1viii—Sn2—Zr1 | 120.0 | Zr1v—Ga1—Zr1xv | 84.096 (5) |
Zr1viii—Sn2—Zr1vii | 120.0 | Zr1—Ga1—Zr1xiv | 95.904 (5) |
Zr1—Sn2—Zr1vii | 120.0 | Zr1xvi—Ga1—Zr1v | 95.904 (5) |
Zr1viii—Sn2—Mn1xii | 63.8 | Zr1—Ga1—Zr1v | 84.096 (5) |
Zr1vii—Sn2—Mn1iv | 152.102 (1) | Zr1xvi—Ga1—Zr1xiv | 84.096 (5) |
Zr1viii—Sn2—Mn1iv | 63.776 (1) | Zr1—Ga1—Ga1ii | 59.033 (4) |
Zr1vii—Sn2—Mn1xi | 152.102 (1) | Zr1xvi—Ga1—Ga1ii | 120.967 (4) |
Zr1—Sn2—Mn1x | 63.8 | Zr1—Ga1—Ga1v | 120.967 (4) |
Zr1—Sn2—Mn1iv | 63.8 | Zr1xiv—Ga1—Ga1ii | 59.033 (4) |
Zr1viii—Sn2—Mn1v | 152.102 (1) | Zr1xv—Ga1—Ga1v | 120.967 (4) |
Zr1vii—Sn2—Mn1x | 63.8 | Zr1v—Ga1—Ga1ii | 120.967 (4) |
Zr1vii—Sn2—Mn1v | 63.775 (1) | Zr1xiv—Ga1—Ga1v | 120.967 (4) |
Zr1vii—Sn2—Mn1xii | 63.776 (1) | Zr1xvii—Ga1—Ga1ii | 120.967 (4) |
Zr1—Sn2—Mn1ix | 152.102 (1) | Zr1xvii—Ga1—Ga1v | 59.033 (4) |
Zr1—Sn2—Mn1v | 63.8 | Zr1xv—Ga1—Ga1ii | 59.033 (4) |
Zr1vii—Sn2—Mn1ix | 63.8 | Zr1xvi—Ga1—Ga1v | 59.033 (4) |
Zr1viii—Sn2—Mn1x | 152.102 (1) | Zr1v—Ga1—Ga1v | 59.033 (4) |
Zr1viii—Sn2—Mn1xi | 63.776 (1) | Ga1ii—Ga1—Ga1v | 180.0 |
Zr1—Sn2—Mn1xii | 152.102 (1) | Sn1—Mn1—Sn1xviii | 180.0 |
Zr1—Sn2—Mn1xi | 63.8 | Sn1xix—Mn1—Sn1viii | 180.0 |
Zr1viii—Sn2—Mn1ix | 63.8 | Sn1xviii—Mn1—Sn1viii | 104.684 (9) |
Mn1ix—Sn2—Mn1xi | 127.551 (1) | Sn1—Mn1—Sn1xix | 104.684 (9) |
Mn1xi—Sn2—Mn1xii | 99.881 (2) | Sn1xviii—Mn1—Sn1xix | 75.316 (9) |
Mn1xii—Sn2—Mn1x | 99.881 (2) | Sn1—Mn1—Sn1viii | 75.316 (9) |
Mn1v—Sn2—Mn1x | 55.796 (2) | Sn1—Mn1—Sn2iii | 72.617 (3) |
Mn1xi—Sn2—Mn1x | 99.881 (1) | Sn1—Mn1—Sn2xx | 107.383 (3) |
Mn1ix—Sn2—Mn1v | 99.881 (1) | Sn1xix—Mn1—Sn2xx | 72.617 (3) |
Mn1ix—Sn2—Mn1xii | 55.796 (2) | Sn1xviii—Mn1—Sn2iii | 107.383 (3) |
Mn1xi—Sn2—Mn1v | 127.6 | Sn1xviii—Mn1—Sn2xx | 72.617 (3) |
Mn1ix—Sn2—Mn1x | 127.551 (1) | Sn1xix—Mn1—Sn2iii | 107.383 (3) |
Mn1iv—Sn2—Mn1v | 99.881 (2) | Sn1viii—Mn1—Sn2iii | 72.617 (3) |
Mn1iv—Sn2—Mn1x | 127.6 | Sn1viii—Mn1—Sn2xx | 107.383 (3) |
Mn1xii—Sn2—Mn1v | 127.551 (1) | Sn1xviii—Mn1—Zr1iii | 119.780 (4) |
Mn1xi—Sn2—Mn1iv | 55.796 (3) | Sn1xviii—Mn1—Zr1xxi | 60.084 (6) |
Mn1ix—Sn2—Mn1iv | 99.881 (2) | Sn1viii—Mn1—Zr1xxi | 60.220 (3) |
Mn1iv—Sn2—Mn1xii | 127.551 (1) | Sn1viii—Mn1—Zr1iii | 119.917 (6) |
Sn1v—Zr1—Sn1i | 154.313 (14) | Sn1xix—Mn1—Zr1xxi | 119.780 (4) |
Sn1xi—Zr1—Sn1 | 140.255 (15) | Sn1xviii—Mn1—Zr1xx | 60.220 (4) |
Sn1v—Zr1—Sn1 | 94.334 (1) | Sn1—Mn1—Zr1iii | 60.220 (4) |
Sn1v—Zr1—Sn1xi | 94.333 (1) | Sn1viii—Mn1—Zr1xx | 60.083 (6) |
Sn1i—Zr1—Sn1xi | 94.334 (1) | Sn1xix—Mn1—Zr1iii | 60.083 (6) |
Sn1i—Zr1—Sn1 | 94.334 (1) | Sn1—Mn1—Zr1i | 60.084 (6) |
Sn1v—Zr1—Zr1ii | 52.291 (5) | Sn1—Mn1—Zr1xx | 119.780 (3) |
Sn1xi—Zr1—Zr1ii | 146.234 (4) | Sn1xviii—Mn1—Zr1i | 119.916 (6) |
Sn1i—Zr1—Zr1ii | 117.993 (2) | Sn1xix—Mn1—Zr1xx | 119.917 (6) |
Sn1—Zr1—Zr1ii | 52.142 (4) | Sn1viii—Mn1—Zr1i | 119.780 (4) |
Sn1—Zr1—Mn1xi | 104.023 (8) | Sn1—Mn1—Zr1xxi | 119.916 (6) |
Sn1v—Zr1—Mn1xi | 145.707 (6) | Sn1xix—Mn1—Zr1i | 60.220 (4) |
Sn1xi—Zr1—Mn1iv | 104.023 (8) | Sn1xviii—Mn1—Mn1iv | 120.540 (2) |
Sn1i—Zr1—Mn1v | 145.707 (6) | Sn1—Mn1—Mn1iv | 59.460 (2) |
Sn1xi—Zr1—Mn1xi | 53.434 (3) | Sn1viii—Mn1—Mn1xiii | 120.540 (2) |
Sn1xi—Zr1—Mn1v | 104.023 (8) | Sn1xix—Mn1—Mn1iv | 120.540 (2) |
Sn1—Zr1—Mn1iv | 53.434 (3) | Sn1xix—Mn1—Mn1xiii | 59.460 (2) |
Sn1—Zr1—Mn1x | 104.023 (8) | Sn1viii—Mn1—Mn1iv | 59.460 (2) |
Sn1i—Zr1—Mn1xi | 53.484 (3) | Sn1—Mn1—Mn1xiii | 120.540 (2) |
Sn1v—Zr1—Mn1iv | 145.707 (6) | Sn1xviii—Mn1—Mn1xiii | 59.460 (2) |
Sn1—Zr1—Mn1v | 53.434 (3) | Sn2iii—Mn1—Sn2xx | 180.0 |
Sn1i—Zr1—Mn1iv | 53.485 (3) | Sn2xx—Mn1—Zr1iii | 122.451 (5) |
Sn1v—Zr1—Mn1v | 53.485 (3) | Sn2xx—Mn1—Zr1xxi | 122.452 (5) |
Sn1i—Zr1—Mn1x | 145.707 (6) | Sn2iii—Mn1—Zr1iii | 57.549 (5) |
Sn1xi—Zr1—Mn1x | 53.434 (3) | Sn2xx—Mn1—Zr1xx | 57.549 (5) |
Sn1v—Zr1—Mn1x | 53.485 (3) | Sn2iii—Mn1—Zr1xx | 122.451 (5) |
Sn2—Zr1—Sn1i | 102.844 (7) | Sn2iii—Mn1—Zr1xxi | 57.548 (5) |
Sn2—Zr1—Sn1xi | 70.128 (7) | Sn2iii—Mn1—Zr1i | 122.452 (5) |
Sn2—Zr1—Sn1 | 70.127 (7) | Sn2xx—Mn1—Zr1i | 57.548 (5) |
Sn2—Zr1—Sn1v | 102.844 (7) | Zr1i—Mn1—Zr1iii | 70.895 (9) |
Sn2—Zr1—Zr1ii | 108.667 (2) | Zr1i—Mn1—Zr1xx | 109.105 (9) |
Sn2—Zr1—Mn1v | 58.676 (5) | Zr1i—Mn1—Zr1xxi | 180.0 |
Sn2—Zr1—Mn1x | 58.676 (5) | Zr1xxi—Mn1—Zr1iii | 109.105 (9) |
Sn2—Zr1—Mn1iv | 58.676 (5) | Zr1xxi—Mn1—Zr1xx | 70.895 (9) |
Sn2—Zr1—Mn1xi | 58.676 (5) | Zr1iii—Mn1—Zr1xx | 180.0 |
Ga1—Zr1—Sn1xi | 78.905 (6) | Mn1xiii—Mn1—Sn2iii | 62.102 (1) |
Ga1ii—Zr1—Sn1 | 78.906 (6) | Mn1iv—Mn1—Sn2iii | 117.898 (1) |
Ga1ii—Zr1—Sn1i | 79.012 (6) | Mn1xiii—Mn1—Sn2xx | 117.898 (1) |
Ga1ii—Zr1—Sn1xi | 140.839 (10) | Mn1iv—Mn1—Sn2xx | 62.102 (1) |
Ga1—Zr1—Sn1i | 79.012 (6) | Mn1xiii—Mn1—Zr1xxi | 63.541 (2) |
Ga1ii—Zr1—Sn1v | 79.012 (6) | Mn1iv—Mn1—Zr1xx | 63.541 (2) |
Ga1—Zr1—Sn1 | 140.839 (10) | Mn1xiii—Mn1—Zr1i | 116.459 (2) |
Ga1—Zr1—Sn1v | 79.012 (6) | Mn1xiii—Mn1—Zr1iii | 63.541 (2) |
Ga1—Zr1—Sn2 | 149.033 (4) | Mn1iv—Mn1—Zr1iii | 116.459 (2) |
Ga1ii—Zr1—Sn2 | 149.033 (4) | Mn1iv—Mn1—Zr1i | 63.541 (2) |
Ga1ii—Zr1—Zr1ii | 47.952 (2) | Mn1xiii—Mn1—Zr1xx | 116.459 (2) |
Ga1—Zr1—Zr1ii | 96.942 (6) | Mn1iv—Mn1—Zr1xxi | 116.459 (2) |
Ga1—Zr1—Ga1ii | 61.934 (7) | Mn1xiii—Mn1—Mn1iv | 180.0 |
Symmetry codes: (i) y, −x+y, −z; (ii) x−y, x, z+1/2; (iii) x, y, z+1; (iv) −x+1, −y, z−1/2; (v) x−y, x, z−1/2; (vi) −x+y+1, −x+1, z; (vii) −x+y+1, −x+1, −z−1/2; (viii) −y+1, x−y, z; (ix) y+1, −x+y+1, z−1/2; (x) −x+y+1, −x+1, z−1; (xi) x, y, z−1; (xii) −y+1, x−y, z−1; (xiii) −x+1, −y, z+1/2; (xiv) −x+y, −x, −z−1/2; (xv) −y, x−y, z; (xvi) −x, −y, −z−1; (xvii) y, −x+y, −z−1; (xviii) −x+1, −y, −z+1; (xix) y, −x+y, −z+1; (xx) −x+1, −y, −z; (xxi) −y+1, x−y, z+1. |
Crystal data top
GaMn3Sn4Zr3 | Dx = 7.944 Mg m−3 |
Mr = 982.96 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63/mmc | Cell parameters from 9901 reflections |
a = 9.1953 (18) Å | θ = 2.6–43.0° |
c = 5.6118 (11) Å | µ = 23.12 mm−1 |
V = 410.93 (18) Å3 | T = 100 K |
Z = 2 | Needle, metallic gray |
F(000) = 852 | 0.11 × 0.10 × 0.09 mm |
Data collection top
Bruker APEX-II CCD diffractometer | 618 reflections with I > 2σ(I) |
φ and ω scans | Rint = 0.059 |
Absorption correction: multi-scan SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1419 before and 0.0893 after correction.
The Ratio of minimum to maximum transmission is 0.6091.
The λ/2 correction factor is Not present. | θmax = 43.0°, θmin = 2.6° |
Tmin = 0.456, Tmax = 0.749 | h = −17→17 |
27596 measured reflections | k = −17→17 |
618 independent reflections | l = −10→10 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.005P)2 + 4.8232P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.022 | (Δ/σ)max < 0.001 |
wR(F2) = 0.047 | Δρmax = 2.06 e Å−3 |
S = 1.32 | Δρmin = −2.41 e Å−3 |
618 reflections | Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
18 parameters | Extinction coefficient: 0.0061 (3) |
0 restraints | |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Sn1(6h) | 0.78887 (4) | 0.57774 (2) | 0.250000 | 0.00261 (6) | |
Sn2(2c) | 0.333333 | 0.666667 | 0.250000 | 0.00265 (8) | |
Zr1(6h) | 0.14700 (5) | 0.29401 (3) | 0.250000 | 0.00204 (8) | |
Ga1(2a) | 0.000000 | 0.000000 | 0.000000 | 0.00282 (12) | |
Mn1(6g) | 0.500000 | 0.000000 | 0.000000 | 0.00248 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn1(6h) | 0.00224 (8) | 0.00307 (10) | 0.00282 (10) | 0.00153 (5) | 0.00000 | 0.00000 |
Sn2(2c) | 0.00158 (10) | 0.00158 (10) | 0.00480 (17) | 0.00079 (5) | 0.00000 | 0.00000 |
Zr1(6h) | 0.00201 (11) | 0.00128 (14) | 0.00260 (14) | 0.00064 (7) | 0.00000 | 0.00000 |
Ga1(2a) | 0.00262 (17) | 0.00262 (17) | 0.0032 (3) | 0.00131 (8) | 0.00000 | 0.00000 |
Mn1(6g) | 0.00208 (15) | 0.0025 (2) | 0.0030 (2) | 0.00125 (10) | −0.00022 (8) | −0.00044 (17) |
Geometric parameters (Å, º) top
Sn1—Zr1i | 2.9860 (6) | Sn2—Mn1xi | 3.0024 (5) |
Sn1—Zr1 | 2.9860 (5) | Sn2—Mn1xii | 3.0024 (5) |
Sn1—Zr1ii | 2.9859 (6) | Sn2—Mn1vi | 3.0024 (5) |
Sn1—Zr1iii | 2.9860 (6) | Zr1—Zr1ii | 3.6544 (6) |
Sn1—Mn1iv | 2.7633 (4) | Zr1—Ga1 | 2.7295 (6) |
Sn1—Mn1 | 2.7633 (4) | Zr1—Ga1ii | 2.7295 (6) |
Sn1—Mn1v | 2.7633 (4) | Zr1—Mn1vi | 3.1534 (6) |
Sn1—Mn1vi | 2.7633 (4) | Zr1—Mn1x | 3.1534 (6) |
Sn2—Zr1vii | 2.9676 (7) | Zr1—Mn1v | 3.1534 (6) |
Sn2—Zr1viii | 2.9675 (7) | Zr1—Mn1xi | 3.1534 (6) |
Sn2—Zr1 | 2.9676 (7) | Ga1—Ga1ii | 2.8059 (5) |
Sn2—Mn1ix | 3.0024 (5) | Ga1—Ga1v | 2.8059 (5) |
Sn2—Mn1x | 3.0024 (5) | Mn1—Mn1xiii | 2.8059 (5) |
Sn2—Mn1v | 3.0024 (5) | Mn1—Mn1vi | 2.8059 (5) |
| | | |
Zr1i—Sn1—Zr1ii | 85.540 (18) | Ga1ii—Zr1—Mn1v | 102.564 (9) |
Zr1ii—Sn1—Zr1 | 75.458 (10) | Ga1—Zr1—Mn1x | 102.564 (9) |
Zr1i—Sn1—Zr1 | 75.458 (10) | Ga1—Zr1—Mn1xi | 102.564 (9) |
Zr1i—Sn1—Zr1iii | 75.458 (10) | Ga1—Zr1—Mn1vi | 132.446 (7) |
Zr1—Sn1—Zr1iii | 140.00 (2) | Ga1ii—Zr1—Mn1vi | 102.564 (9) |
Zr1ii—Sn1—Zr1iii | 75.458 (10) | Ga1ii—Zr1—Mn1xi | 132.446 (7) |
Mn1vi—Sn1—Zr1ii | 136.832 (10) | Ga1—Zr1—Mn1v | 132.446 (7) |
Mn1iv—Sn1—Zr1ii | 66.394 (7) | Ga1ii—Zr1—Mn1x | 132.446 (7) |
Mn1v—Sn1—Zr1ii | 66.394 (7) | Mn1v—Zr1—Zr1ii | 54.588 (7) |
Mn1—Sn1—Zr1ii | 136.832 (10) | Mn1xi—Zr1—Zr1ii | 155.885 (8) |
Mn1v—Sn1—Zr1iii | 123.621 (6) | Mn1vi—Zr1—Zr1ii | 103.268 (14) |
Mn1iv—Sn1—Zr1i | 136.833 (10) | Mn1x—Zr1—Zr1ii | 95.956 (11) |
Mn1—Sn1—Zr1i | 66.393 (7) | Mn1v—Zr1—Mn1x | 52.835 (14) |
Mn1v—Sn1—Zr1i | 136.833 (10) | Mn1x—Zr1—Mn1vi | 117.310 (14) |
Mn1iv—Sn1—Zr1iii | 66.393 (9) | Mn1v—Zr1—Mn1vi | 93.607 (11) |
Mn1vi—Sn1—Zr1i | 66.393 (7) | Mn1v—Zr1—Mn1xi | 117.310 (14) |
Mn1—Sn1—Zr1iii | 66.394 (9) | Mn1x—Zr1—Mn1xi | 93.607 (11) |
Mn1vi—Sn1—Zr1 | 66.393 (10) | Mn1vi—Zr1—Mn1xi | 52.835 (14) |
Mn1—Sn1—Zr1 | 123.621 (6) | Zr1v—Ga1—Zr1xiv | 84.048 (11) |
Mn1iv—Sn1—Zr1 | 123.621 (6) | Zr1xv—Ga1—Zr1xvi | 95.952 (11) |
Mn1v—Sn1—Zr1 | 66.393 (9) | Zr1v—Ga1—Zr1xvi | 95.952 (11) |
Mn1vi—Sn1—Zr1iii | 123.622 (6) | Zr1xvi—Ga1—Zr1xiv | 180.0 |
Mn1v—Sn1—Mn1 | 154.110 (12) | Zr1xvii—Ga1—Zr1xvi | 84.048 (11) |
Mn1v—Sn1—Mn1vi | 112.589 (13) | Zr1—Ga1—Zr1xvi | 84.047 (11) |
Mn1iv—Sn1—Mn1vi | 154.110 (12) | Zr1xv—Ga1—Zr1xiv | 84.048 (11) |
Mn1vi—Sn1—Mn1 | 61.021 (14) | Zr1v—Ga1—Zr1 | 84.047 (11) |
Mn1iv—Sn1—Mn1v | 61.021 (14) | Zr1xvii—Ga1—Zr1xiv | 95.952 (11) |
Mn1iv—Sn1—Mn1 | 112.589 (13) | Zr1xv—Ga1—Zr1xvii | 84.047 (11) |
Zr1viii—Sn2—Zr1 | 120.0 | Zr1—Ga1—Zr1xiv | 95.953 (11) |
Zr1viii—Sn2—Zr1vii | 120.0 | Zr1xvii—Ga1—Zr1v | 180.0 |
Zr1—Sn2—Zr1vii | 120.0 | Zr1xv—Ga1—Zr1 | 180.0 |
Zr1viii—Sn2—Mn1xii | 63.765 (2) | Zr1xvii—Ga1—Zr1 | 95.953 (11) |
Zr1vii—Sn2—Mn1vi | 152.142 (6) | Zr1xv—Ga1—Zr1v | 95.953 (11) |
Zr1viii—Sn2—Mn1vi | 63.765 (2) | Zr1xvii—Ga1—Ga1ii | 59.069 (8) |
Zr1vii—Sn2—Mn1xi | 152.142 (6) | Zr1xv—Ga1—Ga1ii | 120.931 (8) |
Zr1—Sn2—Mn1x | 63.765 (1) | Zr1xvii—Ga1—Ga1v | 120.931 (8) |
Zr1—Sn2—Mn1vi | 63.765 (1) | Zr1v—Ga1—Ga1ii | 120.931 (8) |
Zr1viii—Sn2—Mn1v | 152.142 (6) | Zr1xiv—Ga1—Ga1v | 120.930 (8) |
Zr1vii—Sn2—Mn1x | 63.764 (2) | Zr1—Ga1—Ga1ii | 59.070 (8) |
Zr1vii—Sn2—Mn1v | 63.764 (1) | Zr1v—Ga1—Ga1v | 59.069 (8) |
Zr1vii—Sn2—Mn1xii | 63.766 (2) | Zr1xvi—Ga1—Ga1ii | 120.930 (8) |
Zr1—Sn2—Mn1ix | 152.142 (6) | Zr1xvi—Ga1—Ga1v | 59.070 (8) |
Zr1—Sn2—Mn1v | 63.765 (1) | Zr1xiv—Ga1—Ga1ii | 59.070 (8) |
Zr1vii—Sn2—Mn1ix | 63.766 (2) | Zr1xv—Ga1—Ga1v | 59.069 (8) |
Zr1viii—Sn2—Mn1x | 152.142 (6) | Zr1—Ga1—Ga1v | 120.931 (8) |
Zr1viii—Sn2—Mn1xi | 63.765 (2) | Ga1ii—Ga1—Ga1v | 180.0 |
Zr1—Sn2—Mn1xii | 152.142 (6) | Sn1—Mn1—Sn1xviii | 104.827 (13) |
Zr1—Sn2—Mn1xi | 63.765 (2) | Sn1viii—Mn1—Sn1xix | 104.827 (12) |
Zr1viii—Sn2—Mn1ix | 63.765 (2) | Sn1xviii—Mn1—Sn1xix | 75.173 (12) |
Mn1ix—Sn2—Mn1xi | 127.530 (4) | Sn1—Mn1—Sn1viii | 75.173 (13) |
Mn1xi—Sn2—Mn1xii | 99.932 (8) | Sn1xviii—Mn1—Sn1viii | 180.0 |
Mn1xii—Sn2—Mn1x | 99.932 (8) | Sn1—Mn1—Sn1xix | 180.0 |
Mn1v—Sn2—Mn1x | 55.715 (13) | Sn1—Mn1—Sn2iii | 72.501 (11) |
Mn1xi—Sn2—Mn1x | 99.932 (8) | Sn1—Mn1—Sn2xx | 107.499 (11) |
Mn1ix—Sn2—Mn1v | 99.932 (8) | Sn1viii—Mn1—Sn2xx | 107.499 (10) |
Mn1ix—Sn2—Mn1xii | 55.715 (13) | Sn1xviii—Mn1—Sn2iii | 107.499 (12) |
Mn1xi—Sn2—Mn1v | 127.530 (3) | Sn1xviii—Mn1—Sn2xx | 72.501 (12) |
Mn1ix—Sn2—Mn1x | 127.530 (4) | Sn1viii—Mn1—Sn2iii | 72.501 (12) |
Mn1vi—Sn2—Mn1v | 99.932 (8) | Sn1xix—Mn1—Sn2iii | 107.498 (11) |
Mn1vi—Sn2—Mn1x | 127.530 (4) | Sn1xix—Mn1—Sn2xx | 72.502 (11) |
Mn1xii—Sn2—Mn1v | 127.530 (4) | Sn1xviii—Mn1—Zr1iii | 60.190 (8) |
Mn1xi—Sn2—Mn1vi | 55.715 (13) | Sn1xviii—Mn1—Zr1xxi | 119.810 (13) |
Mn1ix—Sn2—Mn1vi | 99.932 (8) | Sn1xix—Mn1—Zr1xxi | 60.191 (9) |
Mn1vi—Sn2—Mn1xii | 127.530 (4) | Sn1xix—Mn1—Zr1iii | 119.810 (13) |
Sn1v—Zr1—Sn1xi | 94.336 (1) | Sn1viii—Mn1—Zr1xxi | 60.190 (13) |
Sn1i—Zr1—Sn1 | 94.336 (2) | Sn1xviii—Mn1—Zr1xx | 119.810 (8) |
Sn1v—Zr1—Sn1 | 94.336 (2) | Sn1—Mn1—Zr1iii | 60.190 (13) |
Sn1v—Zr1—Sn1i | 154.460 (18) | Sn1xix—Mn1—Zr1xx | 60.190 (13) |
Sn1xi—Zr1—Sn1i | 94.336 (2) | Sn1viii—Mn1—Zr1iii | 119.810 (8) |
Sn1xi—Zr1—Sn1 | 140.00 (2) | Sn1—Mn1—Zr1i | 60.191 (8) |
Sn1v—Zr1—Zr1ii | 52.271 (10) | Sn1—Mn1—Zr1xx | 119.810 (13) |
Sn1i—Zr1—Zr1ii | 118.054 (6) | Sn1xviii—Mn1—Zr1i | 60.190 (13) |
Sn1xi—Zr1—Zr1ii | 146.209 (8) | Sn1viii—Mn1—Zr1xx | 60.190 (8) |
Sn1—Zr1—Zr1ii | 52.270 (11) | Sn1xix—Mn1—Zr1i | 119.810 (8) |
Sn1—Zr1—Mn1xi | 103.895 (14) | Sn1—Mn1—Zr1xxi | 119.809 (8) |
Sn1v—Zr1—Mn1xi | 145.686 (9) | Sn1viii—Mn1—Zr1i | 119.810 (13) |
Sn1i—Zr1—Mn1vi | 53.417 (5) | Sn1xviii—Mn1—Mn1vi | 120.511 (7) |
Sn1xi—Zr1—Mn1v | 103.896 (14) | Sn1—Mn1—Mn1vi | 59.489 (7) |
Sn1i—Zr1—Mn1xi | 53.417 (4) | Sn1xix—Mn1—Mn1xiii | 59.489 (7) |
Sn1i—Zr1—Mn1v | 145.686 (10) | Sn1viii—Mn1—Mn1vi | 59.489 (7) |
Sn1—Zr1—Mn1vi | 53.416 (6) | Sn1viii—Mn1—Mn1xiii | 120.511 (7) |
Sn1—Zr1—Mn1x | 103.895 (13) | Sn1xix—Mn1—Mn1vi | 120.511 (7) |
Sn1xi—Zr1—Mn1xi | 53.416 (6) | Sn1—Mn1—Mn1xiii | 120.511 (7) |
Sn1v—Zr1—Mn1vi | 145.686 (9) | Sn1xviii—Mn1—Mn1xiii | 59.489 (7) |
Sn1—Zr1—Mn1v | 53.416 (6) | Sn2iii—Mn1—Sn2xx | 180.0 |
Sn1xi—Zr1—Mn1vi | 103.896 (13) | Sn2xx—Mn1—Zr1iii | 122.419 (8) |
Sn1v—Zr1—Mn1v | 53.416 (5) | Sn2xx—Mn1—Zr1xxi | 122.421 (7) |
Sn1xi—Zr1—Mn1x | 53.416 (6) | Sn2iii—Mn1—Zr1iii | 57.581 (7) |
Sn1i—Zr1—Mn1x | 145.686 (10) | Sn2xx—Mn1—Zr1xx | 57.581 (7) |
Sn1v—Zr1—Mn1x | 53.416 (5) | Sn2iii—Mn1—Zr1xx | 122.419 (8) |
Sn2—Zr1—Sn1xi | 70.000 (11) | Sn2iii—Mn1—Zr1xxi | 57.579 (7) |
Sn2—Zr1—Sn1i | 102.770 (9) | Sn2iii—Mn1—Zr1i | 122.421 (7) |
Sn2—Zr1—Sn1 | 69.999 (11) | Sn2xx—Mn1—Zr1i | 57.579 (7) |
Sn2—Zr1—Sn1v | 102.770 (9) | Zr1i—Mn1—Zr1iii | 70.824 (15) |
Sn2—Zr1—Zr1ii | 108.683 (4) | Zr1i—Mn1—Zr1xx | 109.176 (15) |
Sn2—Zr1—Mn1v | 58.655 (7) | Zr1i—Mn1—Zr1xxi | 180.0 |
Sn2—Zr1—Mn1x | 58.655 (7) | Zr1xxi—Mn1—Zr1iii | 109.176 (15) |
Sn2—Zr1—Mn1vi | 58.655 (7) | Zr1xxi—Mn1—Zr1xx | 70.824 (15) |
Sn2—Zr1—Mn1xi | 58.655 (7) | Zr1iii—Mn1—Zr1xx | 180.0 |
Ga1—Zr1—Sn1i | 79.070 (8) | Mn1xiii—Mn1—Sn2iii | 62.142 (7) |
Ga1ii—Zr1—Sn1 | 79.070 (14) | Mn1vi—Mn1—Sn2iii | 117.858 (7) |
Ga1ii—Zr1—Sn1xi | 140.931 (14) | Mn1xiii—Mn1—Sn2xx | 117.858 (7) |
Ga1ii—Zr1—Sn1i | 79.070 (8) | Mn1vi—Mn1—Sn2xx | 62.142 (7) |
Ga1—Zr1—Sn1xi | 79.070 (14) | Mn1xiii—Mn1—Zr1xxi | 63.582 (7) |
Ga1ii—Zr1—Sn1v | 79.070 (8) | Mn1vi—Mn1—Zr1xx | 63.583 (7) |
Ga1—Zr1—Sn1 | 140.931 (14) | Mn1xiii—Mn1—Zr1i | 116.418 (7) |
Ga1—Zr1—Sn1v | 79.070 (8) | Mn1xiii—Mn1—Zr1iii | 63.583 (7) |
Ga1—Zr1—Sn2 | 149.070 (8) | Mn1vi—Mn1—Zr1iii | 116.417 (7) |
Ga1ii—Zr1—Sn2 | 149.070 (8) | Mn1vi—Mn1—Zr1i | 63.582 (7) |
Ga1ii—Zr1—Zr1ii | 47.976 (6) | Mn1xiii—Mn1—Zr1xx | 116.417 (7) |
Ga1—Zr1—Zr1ii | 96.885 (13) | Mn1vi—Mn1—Zr1xxi | 116.418 (7) |
Ga1—Zr1—Ga1ii | 61.861 (17) | Mn1xiii—Mn1—Mn1vi | 180.0 |
Symmetry codes: (i) y, −x+y, −z; (ii) x−y, x, z+1/2; (iii) x, y, z+1; (iv) −x+y+1, −x+1, z; (v) x−y, x, z−1/2; (vi) −x+1, −y, z−1/2; (vii) −x+y+1, −x+1, −z−1/2; (viii) −y+1, x−y, z; (ix) y+1, −x+y+1, z−1/2; (x) −x+y+1, −x+1, z−1; (xi) x, y, z−1; (xii) −y+1, x−y, z−1; (xiii) −x+1, −y, z+1/2; (xiv) −y, x−y, z; (xv) −x, −y, −z−1; (xvi) y, −x+y, −z−1; (xvii) −x+y, −x, −z−1/2; (xviii) y, −x+y, −z+1; (xix) −x+1, −y, −z+1; (xx) −x+1, −y, −z; (xxi) −y+1, x−y, z+1. |
Crystal data top
Hexagonal, P63/mmc | c = 5.63860 Å |
Hall symbol: -P 6c 2c | V = 414.31 Å3 |
a = 9.21110 Å | Constant Wavelength Neutron Diffraction radiation, λ = 1.38300 Å |
Data collection top
Radiation source: nuclear reactor | 50 independent reflections |
300 measured reflections | Rint = 0.075 |
Refinement top
R[F2 > 2σ(F2)] = 0.059 | 9 parameters |
wR(F2) = 0.091 | 0 restraints |
50 reflections | 3 constraints |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sn1(6h) | 0.7885 (5) | 0.5770 (5) | 0.250000 | 0.020 (3)* | |
Sn2(2c) | 0.333333 | 0.666667 | 0.250000 | 0.027 (5)* | |
Zr1(6h) | 0.1473 (4) | 0.2946 (4) | 0.250000 | 0.012 (3)* | 0.935 (12) |
Zr2(6g) | 0.500000 | 0.000000 | 0.000000 | 0.000 (5)* | 0.065 (12) |
Ga1(2a) | 0.000000 | 0.000000 | 0.000000 | 0.017 (4)* | |
Mn1(6g) | 0.500000 | 0.000000 | 0.000000 | 0.000 (5)* | 0.935 (12) |
Mn2(6h) | 0.1473 (4) | 0.2946 (4) | 0.250000 | 0.012 (3)* | 0.065 (12) |
Crystal data top
Hexagonal, P63/mmc | c = 5.63860 Å |
Hall symbol: -P 6c 2c | V = 414.31 Å3 |
a = 9.21110 Å | Constant Wavelength Neutron Diffraction radiation, λ = 1.38300 Å |
Data collection top
Radiation source: nuclear reactor | 50 independent reflections |
300 measured reflections | Rint = 0.075 |
Refinement top
R[F2 > 2σ(F2)] = 0.064 | 7 parameters |
wR(F2) = 0.122 | 5 constraints |
50 reflections | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Sn1(6h) | 0.7884 (7) | 0.5768 (7) | 0.250000 | 0.010 (3)* | |
Sn2(2c) | 0.333333 | 0.666667 | 0.250000 | 0.027630* | |
Zr1(6h) | 0.1475 (5) | 0.2950 (5) | 0.250000 | 0.014 (4)* | |
Ga1(2a) | 0.000000 | 0.000000 | 0.000000 | 0.006 (4)* | |
Mn1(6g) | 0.500000 | 0.000000 | 0.000000 | 0.019 (5)* | |
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