Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100013215/sn0004sup1.cif | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.20GPasup2.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.20GPasup3.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.32GPasup4.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.32GPasup5.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.42GPasup6.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.42GPasup7.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.56GPasup8.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.56sup9.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.63GPasup10.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.63GPasup11.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.72GPasup12.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.72GPasup13.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.80GPasup14.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.80GPasup15.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn000400.90GPasup16.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.90GPasup17.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.18GPasup18.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.18GPasup19.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.48GPasup20.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.48GPasup21.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.53GPasup22.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.53GPasup23.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.64GPasup24.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.64GPasup25.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.79GPasup26.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.79GPasup27.hkl | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.87GPasup28.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.87GPasup29.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108768100013215/sn0004sup30.pdf |
Program(s) used to refine structure: GSAS for 0.20GPa, 0.32GPa, 0.42GPa, 0.56GPa, 0.63GPa, 0.72GPa, 0.80GPa, 1.18GPa, 1.48GPa, 1.53GPa, 1.64GPa, 1.79GPa, 1.87GPa.
Mo2O8Zr | Z = 6 |
Mr = 411.10 | Synchrotron radiation, λ = 0.42496 Å |
Trigonal, P31c | T = 298 K |
a = 10.13792 (6) Å | light pink |
c = 11.71279 (15) Å | ?, ? × ? × ? mm |
V = 1042.54 (1) Å3 |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2273 data points |
Rp = 0.005 | Profile function: pseudo-Voigt |
Rwp = 0.007 | 50 parameters |
Rexp = 0.008 | (Δ/σ)max = 0.01 |
R(F2) = 0.0338 | Background function: Chebychev polynomial |
χ2 = 0.846 |
Mo2O8Zr | V = 1042.54 (1) Å3 |
Mr = 411.10 | Z = 6 |
Trigonal, P31c | Synchrotron radiation, λ = 0.42496 Å |
a = 10.13792 (6) Å | T = 298 K |
c = 11.71279 (15) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.005 | χ2 = 0.846 |
Rwp = 0.007 | 2273 data points |
Rexp = 0.008 | 50 parameters |
R(F2) = 0.0338 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0 | 0 | 0 | 0.0063 (15)* | |
Zr2 | 0.33333 | 0.66667 | 0.9796 (4) | 0.0063 (15)* | |
Mo1 | 0.3303 (12) | 0.3386 (12) | 0.14700 (14) | 0.0157 (8)* | |
O1 | 0.157 (4) | 0.145 (5) | 0.106 (3) | 0.004 (2)* | |
O2 | 0.322 (4) | 0.496 (4) | 0.091 (2) | 0.004 (2)* | |
O3 | 0.529 (3) | 0.360 (4) | 0.122 (2) | 0.004 (2)* | |
O4 | 0.318 (5) | 0.340 (6) | 0.2889 (6) | 0.004 (2)* |
Zr1—O1 | 1.97 (4) | Zr2—O2 | 2.11 (3) |
Zr1—O1 | 1.97 (4) | Zr2—O3 | 1.94 (3) |
Zr1—O1 | 1.97 (4) | Zr2—O3 | 1.94 (3) |
Zr1—O1 | 1.97 (4) | Zr2—O3 | 1.94 (3) |
Zr1—O1 | 1.97 (4) | Mo—O1 | 1.92 (4) |
Zr1—O1 | 1.97 (4) | Mo—O2 | 1.78 (3) |
Zr2—O2 | 2.11 (3) | Mo—O3 | 1.94 (4) |
Zr2—O2 | 2.11 (3) | Mo—O4 | 1.667 (8) |
O1—Zr1—O1 | 85 (2) | O2—Zr2—O3 | 90.9 (13) |
O1—Zr1—O1 | 85 (2) | O2—Zr2—O3 | 90.9 (13) |
O1—Zr1—O1 | 85 (2) | O2—Zr2—O3 | 90.9 (13) |
O1—Zr1—O1 | 85 (2) | O2—Zr2—O3 | 175.8 (12) |
O1—Zr1—O1 | 85 (2) | O2—Zr2—O3 | 175.8 (12) |
O1—Zr1—O1 | 85 (2) | O2—Zr2—O3 | 175.8 (12) |
O1—Zr1—O1 | 95 (2) | O2—Zr2—O3 | 96.6 (11) |
O1—Zr1—O1 | 95 (2) | O2—Zr2—O3 | 96.6 (11) |
O1—Zr1—O1 | 95 (2) | O2—Zr2—O3 | 96.6 (11) |
O1—Zr1—O1 | 95 (2) | O3—Zr2—O3 | 86.8 (14) |
O1—Zr1—O1 | 95 (2) | O3—Zr2—O3 | 86.8 (14) |
O1—Zr1—O1 | 95 (2) | O3—Zr2—O3 | 86.8 (14) |
O1—Zr1—O1 | 180 (5) | O1—Mo—O2 | 113.5 (17) |
O1—Zr1—O1 | 180 (5) | O1—Mo—O3 | 115.8 (16) |
O1—Zr1—O1 | 180 (5) | O1—Mo—O4 | 103 (2) |
O2—Zr2—O2 | 85.8 (13) | O2—Mo—O3 | 111.0 (16) |
O2—Zr2—O2 | 85.8 (13) | O2—Mo—O4 | 109 (2) |
O2—Zr2—O2 | 85.8 (13) | O3—Mo—O4 | 103 (2) |
Mo2O8Zr | Z = 6 |
Mr = 411.10 | Synchrotron radiation, λ = 0.42496 Å |
Trigonal, P31c | T = 298 K |
a = 10.14778 (9) Å | light pink |
c = 11.6780 (2) Å | ?, ? × ? × ? mm |
V = 1041.46 (2) Å3 |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2276 data points |
Rp = 0.006 | Profile function: pseudo-Voigt |
Rwp = 0.009 | 54 parameters |
Rexp = 0.008 | (Δ/σ)max = 0.01 |
R(F2) = 0.0327 | Background function: Chebychev polynomial |
χ2 = 1.300 |
Mo2O8Zr | V = 1041.46 (2) Å3 |
Mr = 411.10 | Z = 6 |
Trigonal, P31c | Synchrotron radiation, λ = 0.42496 Å |
a = 10.14778 (9) Å | T = 298 K |
c = 11.6780 (2) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.006 | χ2 = 1.300 |
Rwp = 0.009 | 2276 data points |
Rexp = 0.008 | 54 parameters |
R(F2) = 0.0327 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.0021 (14)* | |
Zr2 | 0.33333 | 0.66667 | 0.9752 (4) | 0.0021 (14)* | |
Mo1 | 0.3298 (13) | 0.3375 (13) | 0.14778 (16) | 0.0137 (8)* | |
O1 | 0.160 (6) | 0.150 (6) | 0.097 (2) | 0.005 (2)* | |
O2 | 0.334 (7) | 0.506 (5) | 0.0923 (19) | 0.005 (2)* | |
O3 | 0.523 (3) | 0.352 (4) | 0.1299 (14) | 0.005 (2)* | |
O4 | 0.317 (5) | 0.345 (5) | 0.2909 (7) | 0.005 (2)* |
Zr1—O1 | 1.94 (4) | Zr2—O2 | 2.12 (3) |
Zr1—O1 | 1.94 (4) | Zr2—O3 | 1.99 (3) |
Zr1—O1 | 1.94 (4) | Zr2—O3 | 1.99 (3) |
Zr1—O1 | 1.94 (4) | Zr2—O3 | 1.99 (3) |
Zr1—O1 | 1.94 (4) | Mo—O1 | 1.91 (5) |
Zr1—O1 | 1.94 (4) | Mo—O2 | 1.82 (4) |
Zr2—O2 | 2.12 (3) | Mo—O3 | 1.90 (4) |
Zr2—O2 | 2.12 (3) | Mo—O4 | 1.681 (9) |
O1—Zr1—O1 | 89 (2) | O2—Zr2—O3 | 92.4 (18) |
O1—Zr1—O1 | 89 (2) | O2—Zr2—O3 | 174.8 (19) |
O1—Zr1—O1 | 89 (2) | O2—Zr2—O3 | 174.8 (19) |
O1—Zr1—O1 | 89 (2) | O2—Zr2—O3 | 174.8 (19) |
O1—Zr1—O1 | 89 (2) | O2—Zr2—O3 | 98.9 (15) |
O1—Zr1—O1 | 89 (2) | O2—Zr2—O3 | 98.9 (15) |
O1—Zr1—O1 | 91 (2) | O2—Zr2—O3 | 98.9 (15) |
O1—Zr1—O1 | 91 (2) | O3—Zr2—O3 | 85.9 (11) |
O1—Zr1—O1 | 91 (2) | O3—Zr2—O3 | 85.9 (11) |
O1—Zr1—O1 | 91 (2) | O3—Zr2—O3 | 85.9 (11) |
O1—Zr1—O1 | 91 (2) | O1—Mo—O2 | 114 (2) |
O1—Zr1—O1 | 91 (2) | O1—Mo—O3 | 115.0 (19) |
O1—Zr1—O1 | 180 (3) | O1—Mo—O4 | 107.5 (19) |
O1—Zr1—O1 | 180 (3) | O2—Mo—O3 | 111 (2) |
O1—Zr1—O1 | 180 (3) | O2—Mo—O4 | 106.1 (19) |
O2—Zr2—O2 | 83 (2) | O3—Mo—O4 | 102 (2) |
O2—Zr2—O2 | 83 (2) | Zr1—O1—Mo | 160.9 (19) |
O2—Zr2—O2 | 83 (2) | Zr2—O2—Mo | 160.7 (16) |
O2—Zr2—O3 | 92.4 (18) | Zr2—O3—Mo | 146.9 (10) |
O2—Zr2—O3 | 92.4 (18) |
Mo2O8Zr | Z = 6 |
Mr = 411.10 | Synchrotron radiation, λ = 0.42496 Å |
Trigonal, P31c | T = 298 K |
a = 10.13896 (8) Å | light pink |
c = 11.60753 (19) Å | ?, ? × ? × ? mm |
V = 1033.38 (2) Å3 |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2273 data points |
Rp = 0.007 | Profile function: pseudo-Voigt |
Rwp = 0.012 | 22 parameters |
Rexp = 0.008 | (Δ/σ)max = 0.01 |
R(F2) = 0.0420 | Background function: Chebychev polynomial |
χ2 = 1.988 |
Mo2O8Zr | V = 1033.38 (2) Å3 |
Mr = 411.10 | Z = 6 |
Trigonal, P31c | Synchrotron radiation, λ = 0.42496 Å |
a = 10.13896 (8) Å | T = 298 K |
c = 11.60753 (19) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.007 | χ2 = 1.988 |
Rwp = 0.012 | 2273 data points |
Rexp = 0.008 | 22 parameters |
R(F2) = 0.0420 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.0026 (14)* | |
Zr2 | 0.33333 | 0.66667 | 0.9748 (5) | 0.0026 (14)* | |
Mo1 | 0.3297 (14) | 0.3364 (14) | 0.15039 (17) | 0.0126 (8)* | |
O1 | 0.166 (7) | 0.161 (6) | 0.0800 (19) | 0.003 (2)* | |
O2 | 0.341 (9) | 0.515 (5) | 0.0902 (19) | 0.003 (2)* | |
O3 | 0.531 (3) | 0.345 (5) | 0.1332 (14) | 0.003 (2)* | |
O4 | 0.320 (5) | 0.346 (5) | 0.2840 (8) | 0.003 (2)* |
Zr1—O1 | 1.89 (5) | Zr2—O2 | 2.06 (4) |
Zr1—O1 | 1.89 (5) | Zr2—O3 | 1.90 (3) |
Zr1—O1 | 1.89 (5) | Zr2—O3 | 1.90 (3) |
Zr1—O1 | 1.89 (5) | Zr2—O3 | 1.90 (3) |
Zr1—O1 | 1.89 (5) | Mo—O1 | 1.92 (5) |
Zr1—O1 | 1.89 (5) | Mo—O2 | 1.90 (5) |
Zr2—O2 | 2.06 (4) | Mo—O3 | 2.01 (4) |
Zr2—O2 | 2.06 (4) | Mo—O4 | 1.654 (11) |
O1—Zr1—O1 | 82 (3) | O2—Zr2—O3 | 95 (2) |
O1—Zr1—O1 | 82 (3) | O2—Zr2—O3 | 95 (2) |
O1—Zr1—O1 | 82 (3) | O2—Zr2—O3 | 95 (2) |
O1—Zr1—O1 | 82 (3) | O2—Zr2—O3 | 175 (2) |
O1—Zr1—O1 | 82 (3) | O2—Zr2—O3 | 175 (2) |
O1—Zr1—O1 | 82 (3) | O2—Zr2—O3 | 175 (2) |
O1—Zr1—O1 | 98 (3) | O2—Zr2—O3 | 101 (2) |
O1—Zr1—O1 | 98 (3) | O2—Zr2—O3 | 101 (2) |
O1—Zr1—O1 | 98 (3) | O2—Zr2—O3 | 101 (2) |
O1—Zr1—O1 | 98 (3) | O3—Zr2—O3 | 81.7 (15) |
O1—Zr1—O1 | 98 (3) | O3—Zr2—O3 | 81.7 (15) |
O1—Zr1—O1 | 98 (3) | O3—Zr2—O3 | 81.7 (15) |
O1—Zr1—O1 | 180 (10) | O1—Mo—O2 | 111 (2) |
O1—Zr1—O1 | 180 (10) | O1—Mo—O3 | 112 (2) |
O1—Zr1—O1 | 180 (10) | O1—Mo—O4 | 116 (2) |
O2—Zr2—O2 | 83 (2) | O2—Mo—O3 | 110 (2) |
O2—Zr2—O2 | 83 (2) | O2—Mo—O4 | 106.1 (19) |
O2—Zr2—O2 | 83 (2) | O3—Mo—O4 | 101.6 (19) |
Mo2O8Zr | Z = 6 |
Mr = 411.10 | Synchrotron radiation, λ = 0.42496 Å |
Trigonal, P31c | T = 298 K |
a = 10.14226 (12) Å | light pink |
c = 11.5334 (3) Å | ?, ? × ? × ? mm |
V = 1027.46 (3) Å3 |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2276 data points |
Rp = 0.008 | Profile function: pseudo-Voigt |
Rwp = 0.013 | 54 parameters |
Rexp = 0.008 | (Δ/σ)max = 0.01 |
R(F2) = 0.0464 | Background function: Chebychev polynomial |
χ2 = 2.528 |
Mo2O8Zr | V = 1027.46 (3) Å3 |
Mr = 411.10 | Z = 6 |
Trigonal, P31c | Synchrotron radiation, λ = 0.42496 Å |
a = 10.14226 (12) Å | T = 298 K |
c = 11.5334 (3) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.008 | χ2 = 2.528 |
Rwp = 0.013 | 2276 data points |
Rexp = 0.008 | 54 parameters |
R(F2) = 0.0464 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.0057 (16)* | |
Zr2 | 0.33333 | 0.66667 | 0.9742 (6) | 0.0057 (16)* | |
Mo1 | 0.3293 (16) | 0.3366 (16) | 0.1512 (2) | 0.0117 (11)* | |
O1 | 0.165 (8) | 0.163 (7) | 0.078 (2) | 0.002 (3)* | |
O2 | 0.342 (11) | 0.517 (6) | 0.092 (2) | 0.002 (3)* | |
O3 | 0.531 (4) | 0.342 (6) | 0.1338 (18) | 0.002 (3)* | |
O4 | 0.318 (5) | 0.345 (6) | 0.2844 (11) | 0.002 (3)* |
Zr1—O1 | 1.90 (6) | Zr2—O2 | 2.06 (6) |
Zr1—O1 | 1.90 (6) | Zr2—O3 | 1.88 (4) |
Zr1—O1 | 1.90 (6) | Zr2—O3 | 1.88 (4) |
Zr1—O1 | 1.90 (6) | Zr2—O3 | 1.88 (4) |
Zr1—O1 | 1.90 (6) | Mo—O1 | 1.91 (6) |
Zr1—O1 | 1.90 (6) | Mo—O2 | 1.90 (6) |
Zr2—O2 | 2.06 (6) | Mo—O3 | 2.03 (5) |
Zr2—O2 | 2.06 (6) | Mo—O4 | 1.550 (13) |
O1—Zr1—O1 | 81 (3) | O2—Zr2—O3 | 96 (3) |
O1—Zr1—O1 | 81 (3) | O2—Zr2—O3 | 96 (3) |
O1—Zr1—O1 | 81 (3) | O2—Zr2—O3 | 96 (3) |
O1—Zr1—O1 | 81 (3) | O2—Zr2—O3 | 176 (3) |
O1—Zr1—O1 | 81 (3) | O2—Zr2—O3 | 176 (3) |
O1—Zr1—O1 | 81 (3) | O2—Zr2—O3 | 176 (3) |
O1—Zr1—O1 | 99 (3) | O2—Zr2—O3 | 101 (2) |
O1—Zr1—O1 | 99 (3) | O2—Zr2—O3 | 101 (2) |
O1—Zr1—O1 | 99 (3) | O2—Zr2—O3 | 101 (2) |
O1—Zr1—O1 | 99 (3) | O3—Zr2—O3 | 81 (2) |
O1—Zr1—O1 | 99 (3) | O3—Zr2—O3 | 81 (2) |
O1—Zr1—O1 | 99 (3) | O3—Zr2—O3 | 81 (2) |
O1—Zr1—O1 | 180 (15) | O1—Mo—O2 | 110 (3) |
O1—Zr1—O1 | 180 (15) | O1—Mo—O3 | 112 (3) |
O1—Zr1—O1 | 180 (15) | O1—Mo—O4 | 116 (2) |
O2—Zr2—O2 | 82 (3) | O2—Mo—O3 | 111 (3) |
O2—Zr2—O2 | 82 (3) | O2—Mo—O4 | 106 (2) |
O2—Zr2—O2 | 82 (3) | O3—Mo—O4 | 102 (2) |
Mo2O8Zr | Z = 6 |
Mr = 411.10 | Synchrotron radiation, λ = 0.42496 Å |
Trigonal, P31c | T = 298 K |
a = 10.13168 (11) Å | light pink |
c = 11.4790 (3) Å | ?, ? × ? × ? mm |
V = 1020.46 (3) Å3 |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2269 data points |
Rp = 0.007 | Profile function: pseudo-Voigt |
Rwp = 0.012 | 54 parameters |
Rexp = 0.008 | (Δ/σ)max = 0.01 |
R(F2) = 0.0484 | Background function: Chebychev polynomial |
χ2 = 2.190 |
Mo2O8Zr | V = 1020.46 (3) Å3 |
Mr = 411.10 | Z = 6 |
Trigonal, P31c | Synchrotron radiation, λ = 0.42496 Å |
a = 10.13168 (11) Å | T = 298 K |
c = 11.4790 (3) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.007 | χ2 = 2.190 |
Rwp = 0.012 | 2269 data points |
Rexp = 0.008 | 54 parameters |
R(F2) = 0.0484 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.0023 (14)* | |
Zr2 | 0.33333 | 0.66667 | 0.9739 (5) | 0.0023 (14)* | |
Mo1 | 0.3296 (16) | 0.3369 (15) | 0.1515 (2) | 0.0132 (10)* | |
O1 | 0.164 (7) | 0.163 (6) | 0.081 (2) | 0.003 (3)* | |
O2 | 0.345 (10) | 0.518 (6) | 0.094 (2) | 0.003 (3)* | |
O3 | 0.531 (3) | 0.340 (6) | 0.1354 (16) | 0.003 (3)* | |
O4 | 0.316 (5) | 0.344 (6) | 0.2868 (10) | 0.003 (3)* |
Zr1—O1 | 1.90 (5) | Zr2—O2 | 2.08 (4) |
Zr1—O1 | 1.90 (5) | Zr2—O3 | 1.89 (3) |
Zr1—O1 | 1.90 (5) | Zr2—O3 | 1.89 (3) |
Zr1—O1 | 1.90 (5) | Zr2—O3 | 1.89 (3) |
Zr1—O1 | 1.90 (5) | Mo—O1 | 1.90 (6) |
Zr1—O1 | 1.90 (5) | Mo—O2 | 1.88 (5) |
Zr2—O2 | 2.08 (4) | Mo—O3 | 2.03 (5) |
Zr2—O2 | 2.08 (4) | Mo—O4 | 1.567 (13) |
O1—Zr1—O1 | 82 (3) | O2—Zr2—O3 | 96 (2) |
O1—Zr1—O1 | 82 (3) | O2—Zr2—O3 | 96 (2) |
O1—Zr1—O1 | 82 (3) | O2—Zr2—O3 | 96 (2) |
O1—Zr1—O1 | 82 (3) | O2—Zr2—O3 | 176 (3) |
O1—Zr1—O1 | 82 (3) | O2—Zr2—O3 | 176 (3) |
O1—Zr1—O1 | 82 (3) | O2—Zr2—O3 | 176 (3) |
O1—Zr1—O1 | 98 (3) | O2—Zr2—O3 | 101 (2) |
O1—Zr1—O1 | 98 (3) | O2—Zr2—O3 | 101 (2) |
O1—Zr1—O1 | 98 (3) | O2—Zr2—O3 | 101 (2) |
O1—Zr1—O1 | 98 (3) | O3—Zr2—O3 | 81 (2) |
O1—Zr1—O1 | 98 (3) | O3—Zr2—O3 | 81 (2) |
O1—Zr1—O1 | 98 (3) | O3—Zr2—O3 | 81 (2) |
O1—Zr1—O1 | 180 (9) | O1—Mo—O2 | 111 (2) |
O1—Zr1—O1 | 180 (9) | O1—Mo—O3 | 112 (3) |
O1—Zr1—O1 | 180 (9) | O1—Mo—O4 | 114 (2) |
O2—Zr2—O2 | 81 (2) | O2—Mo—O3 | 112 (3) |
O2—Zr2—O2 | 81 (2) | O2—Mo—O4 | 106 (2) |
O2—Zr2—O2 | 81 (2) | O3—Mo—O4 | 102 (2) |
Mo2O8Zr | Z = 6 |
Mr = 411.10 | Synchrotron radiation, λ = 0.42496 Å |
Trigonal, P31c | T = 298 K |
a = 10.13750 (11) Å | light pink |
c = 11.4395 (3) Å | ?, ? × ? × ? mm |
V = 1018.11 (3) Å3 |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2273 data points |
Rp = 0.007 | Profile function: pseudo-Voigt |
Rwp = 0.012 | 54 parameters |
Rexp = 0.008 | (Δ/σ)max = 0.01 |
R(F2) = 0.0433 | Background function: Chebychev polynomial |
χ2 = 2.220 |
Mo2O8Zr | V = 1018.11 (3) Å3 |
Mr = 411.10 | Z = 6 |
Trigonal, P31c | Synchrotron radiation, λ = 0.42496 Å |
a = 10.13750 (11) Å | T = 298 K |
c = 11.4395 (3) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.007 | χ2 = 2.220 |
Rwp = 0.012 | 2273 data points |
Rexp = 0.008 | 54 parameters |
R(F2) = 0.0433 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.0025 (14)* | |
Zr2 | 0.33333 | 0.66667 | 0.9728 (6) | 0.0025 (14)* | |
Mo1 | 0.3295 (16) | 0.3369 (15) | 0.1519 (2) | 0.0130 (9)* | |
O1 | 0.166 (7) | 0.161 (7) | 0.080 (2) | 0.010 (3)* | |
O2 | 0.340 (12) | 0.516 (7) | 0.095 (2) | 0.010 (3)* | |
O3 | 0.531 (3) | 0.341 (6) | 0.1329 (16) | 0.010 (3)* | |
O4 | 0.315 (5) | 0.343 (6) | 0.2873 (10) | 0.010 (3)* |
Zr1—O1 | 1.89 (6) | Zr2—O2 | 2.09 (6) |
Zr1—O1 | 1.89 (6) | Zr2—O3 | 1.86 (3) |
Zr1—O1 | 1.89 (6) | Zr2—O3 | 1.86 (3) |
Zr1—O1 | 1.89 (6) | Zr2—O3 | 1.86 (3) |
Zr1—O1 | 1.89 (6) | Mo—O1 | 1.91 (6) |
Zr1—O1 | 1.89 (6) | Mo—O2 | 1.88 (7) |
Zr2—O2 | 2.09 (6) | Mo—O3 | 2.04 (5) |
Zr2—O2 | 2.09 (6) | Mo—O4 | 1.563 (13) |
O1—Zr1—O1 | 81 (3) | O2—Zr2—O3 | 97 (3) |
O1—Zr1—O1 | 81 (3) | O2—Zr2—O3 | 97 (3) |
O1—Zr1—O1 | 81 (3) | O2—Zr2—O3 | 97 (3) |
O1—Zr1—O1 | 81 (3) | O2—Zr2—O3 | 177 (3) |
O1—Zr1—O1 | 81 (3) | O2—Zr2—O3 | 177 (3) |
O1—Zr1—O1 | 81 (3) | O2—Zr2—O3 | 177 (3) |
O1—Zr1—O1 | 99 (3) | O2—Zr2—O3 | 101 (2) |
O1—Zr1—O1 | 99 (3) | O2—Zr2—O3 | 101 (2) |
O1—Zr1—O1 | 99 (3) | O2—Zr2—O3 | 101 (2) |
O1—Zr1—O1 | 99 (3) | O3—Zr2—O3 | 82 (2) |
O1—Zr1—O1 | 99 (3) | O3—Zr2—O3 | 82 (2) |
O1—Zr1—O1 | 99 (3) | O3—Zr2—O3 | 82 (2) |
O1—Zr1—O1 | 180 (16) | O1—Mo—O2 | 111 (3) |
O1—Zr1—O1 | 180 (16) | O1—Mo—O3 | 111 (3) |
O1—Zr1—O1 | 180 (16) | O1—Mo—O4 | 114 (2) |
O2—Zr2—O2 | 80 (3) | O2—Mo—O3 | 112 (4) |
O2—Zr2—O2 | 80 (3) | O2—Mo—O4 | 105 (2) |
O2—Zr2—O2 | 80 (3) | O3—Mo—O4 | 103 (2) |
Mo2O8Zr | Z = 6 |
Mr = 411.10 | Synchrotron radiation, λ = 0.42496 Å |
Trigonal, P31c | T = 298 K |
a = 10.13183 (10) Å | light pink |
c = 11.3877 (3) Å | ?, ? × ? × ? mm |
V = 1012.37 (3) Å3 |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2273 data points |
Rp = 0.006 | Profile function: pseudo-Voigt |
Rwp = 0.010 | 54 parameters |
Rexp = 0.008 | (Δ/σ)max = 0.01 |
R(F2) = 0.0362 | Background function: Chebychev polynomial |
χ2 = 1.742 |
Mo2O8Zr | V = 1012.37 (3) Å3 |
Mr = 411.10 | Z = 6 |
Trigonal, P31c | Synchrotron radiation, λ = 0.42496 Å |
a = 10.13183 (10) Å | T = 298 K |
c = 11.3877 (3) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.006 | χ2 = 1.742 |
Rwp = 0.010 | 2273 data points |
Rexp = 0.008 | 54 parameters |
R(F2) = 0.0362 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.0027 (14)* | |
Zr2 | 0.33333 | 0.66667 | 0.9720 (5) | 0.0027 (14)* | |
Mo1 | 0.3289 (13) | 0.3371 (12) | 0.1524 (3) | 0.0147 (8)* | |
O1 | 0.170 (6) | 0.162 (6) | 0.0798 (18) | 0.009 (2)* | |
O2 | 0.343 (9) | 0.516 (5) | 0.0981 (19) | 0.009 (2)* | |
O3 | 0.532 (3) | 0.340 (5) | 0.1361 (15) | 0.009 (2)* | |
O4 | 0.314 (4) | 0.341 (5) | 0.2865 (10) | 0.009 (2)* |
Zr1—O1 | 1.91 (5) | Zr2—O2 | 2.14 (4) |
Zr1—O1 | 1.91 (5) | Zr2—O3 | 1.87 (3) |
Zr1—O1 | 1.91 (5) | Zr2—O3 | 1.87 (3) |
Zr1—O1 | 1.91 (5) | Zr2—O3 | 1.87 (3) |
Zr1—O1 | 1.91 (5) | Mo—O1 | 1.89 (5) |
Zr1—O1 | 1.91 (5) | Mo—O2 | 1.85 (5) |
Zr2—O2 | 2.14 (4) | Mo—O3 | 2.05 (4) |
Zr2—O2 | 2.14 (4) | Mo—O4 | 1.542 (11) |
O1—Zr1—O1 | 81 (2) | O2—Zr2—O3 | 97 (2) |
O1—Zr1—O1 | 81 (2) | O2—Zr2—O3 | 97 (2) |
O1—Zr1—O1 | 81 (2) | O2—Zr2—O3 | 97 (2) |
O1—Zr1—O1 | 81 (2) | O2—Zr2—O3 | 176 (2) |
O1—Zr1—O1 | 81 (2) | O2—Zr2—O3 | 176 (2) |
O1—Zr1—O1 | 81 (2) | O2—Zr2—O3 | 176 (2) |
O1—Zr1—O1 | 99 (2) | O2—Zr2—O3 | 102 (2) |
O1—Zr1—O1 | 99 (2) | O2—Zr2—O3 | 102 (2) |
O1—Zr1—O1 | 99 (2) | O2—Zr2—O3 | 102 (2) |
O1—Zr1—O1 | 99 (2) | O3—Zr2—O3 | 81.3 (18) |
O1—Zr1—O1 | 99 (2) | O3—Zr2—O3 | 81.3 (18) |
O1—Zr1—O1 | 99 (2) | O3—Zr2—O3 | 81.3 (18) |
O1—Zr1—O1 | 180 (14) | O1—Mo—O2 | 112 (2) |
O1—Zr1—O1 | 180 (14) | O1—Mo—O3 | 110 (2) |
O1—Zr1—O1 | 180 (14) | O1—Mo—O4 | 114 (2) |
O2—Zr2—O2 | 80 (2) | O2—Mo—O3 | 112 (3) |
O2—Zr2—O2 | 80 (2) | O2—Mo—O4 | 105 (2) |
O2—Zr2—O2 | 80 (2) | O3—Mo—O4 | 102 (2) |
Mo2O8Zr | Z = 6 |
Mr = 411.10 | Synchrotron radiation, λ = 0.42496 Å |
Trigonal, P31c | T = 298 K |
a = 10.1264 (1) Å | light pink |
c = 11.3252 (2) Å | ?, ? × ? × ? mm |
V = 1005.75 (2) Å3 |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2273 data points |
Rp = 0.006 | Profile function: pseudo-Voigt |
Rwp = 0.010 | 54 parameters |
Rexp = 0.008 | (Δ/σ)max = 0.01 |
R(F2) = 0.0339 | Background function: Chebychev polynomial |
χ2 = 1.613 |
Mo2O8Zr | V = 1005.75 (2) Å3 |
Mr = 411.10 | Z = 6 |
Trigonal, P31c | Synchrotron radiation, λ = 0.42496 Å |
a = 10.1264 (1) Å | T = 298 K |
c = 11.3252 (2) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.00°, 2θmax = 22.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.006 | χ2 = 1.613 |
Rwp = 0.010 | 2273 data points |
Rexp = 0.008 | 54 parameters |
R(F2) = 0.0339 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.0039 (17)* | |
Zr2 | 0.33333 | 0.66667 | 0.9718 (5) | 0.0039 (17)* | |
Mo1 | 0.3283 (12) | 0.3380 (11) | 0.1542 (3) | 0.0148 (9)* | |
O1 | 0.170 (5) | 0.164 (5) | 0.0831 (18) | 0.001 (2)* | |
O2 | 0.344 (7) | 0.519 (4) | 0.1045 (17) | 0.001 (2)* | |
O3 | 0.527 (3) | 0.336 (5) | 0.1409 (15) | 0.001 (2)* | |
O4 | 0.315 (4) | 0.337 (5) | 0.2884 (9) | 0.001 (2)* |
Zr1—O1 | 1.94 (4) | Zr2—O2 | 2.16 (3) |
Zr1—O1 | 1.94 (4) | Zr2—O3 | 1.91 (3) |
Zr1—O1 | 1.94 (4) | Zr2—O3 | 1.91 (3) |
Zr1—O1 | 1.94 (4) | Zr2—O3 | 1.91 (3) |
Zr1—O1 | 1.94 (4) | Mo—O1 | 1.87 (4) |
Zr1—O1 | 1.94 (4) | Mo—O2 | 1.85 (4) |
Zr2—O2 | 2.16 (3) | Mo—O3 | 2.03 (4) |
Zr2—O2 | 2.16 (3) | Mo—O4 | 1.525 (11) |
O1—Zr1—O1 | 82 (2) | O2—Zr2—O3 | 99.5 (18) |
O1—Zr1—O1 | 82 (2) | O2—Zr2—O3 | 99.5 (18) |
O1—Zr1—O1 | 82 (2) | O2—Zr2—O3 | 99.5 (18) |
O1—Zr1—O1 | 82 (2) | O2—Zr2—O3 | 176.1 (18) |
O1—Zr1—O1 | 82 (2) | O2—Zr2—O3 | 176.1 (18) |
O1—Zr1—O1 | 82 (2) | O2—Zr2—O3 | 176.1 (18) |
O1—Zr1—O1 | 98 (2) | O2—Zr2—O3 | 103 (2) |
O1—Zr1—O1 | 98 (2) | O2—Zr2—O3 | 103 (2) |
O1—Zr1—O1 | 98 (2) | O2—Zr2—O3 | 103 (2) |
O1—Zr1—O1 | 98 (2) | O3—Zr2—O3 | 80.5 (17) |
O1—Zr1—O1 | 98 (2) | O3—Zr2—O3 | 80.5 (17) |
O1—Zr1—O1 | 98 (2) | O3—Zr2—O3 | 80.5 (17) |
O1—Zr1—O1 | 180 (3) | O1—Mo—O2 | 114 (2) |
O1—Zr1—O1 | 180 (3) | O1—Mo—O3 | 110 (2) |
O1—Zr1—O1 | 180 (3) | O1—Mo—O4 | 113 (2) |
O2—Zr2—O2 | 76.8 (18) | O2—Mo—O3 | 114 (2) |
O2—Zr2—O2 | 76.8 (18) | O2—Mo—O4 | 105.8 (19) |
O2—Zr2—O2 | 76.8 (18) | O3—Mo—O4 | 99.2 (19) |
Mo2O8Zr | V = 317.53 (2) Å3 |
Mr = 411.10 | Z = 2 |
Monoclinic, C2/m | Synchrotron radiation, λ = 0.42496 Å |
a = 9.8821 (3) Å | T = 298 K |
b = 5.9699 (2) Å | light pink |
c = 5.3888 (2) Å | ?, ? × ? × ? mm |
β = 92.818 (3)° |
Synchrotron diffractometer | 2θmin = 3.20°, 2θmax = 20.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2011 data points |
Rp = 0.009 | Profile function: pseudo-Voigt |
Rwp = 0.014 | 53 parameters |
Rexp = 0.007 | (Δ/σ)max = 0.01 |
R(F2) = 0.0664 | Background function: Chebychev polynomial |
χ2 = 4.162 |
Mo2O8Zr | β = 92.818 (3)° |
Mr = 411.10 | V = 317.53 (2) Å3 |
Monoclinic, C2/m | Z = 2 |
a = 9.8821 (3) Å | Synchrotron radiation, λ = 0.42496 Å |
b = 5.9699 (2) Å | T = 298 K |
c = 5.3888 (2) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.20°, 2θmax = 20.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.009 | χ2 = 4.162 |
Rwp = 0.014 | 2011 data points |
Rexp = 0.007 | 53 parameters |
R(F2) = 0.0664 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.025 (3)* | |
Mo1 | 0.3297 (5) | 0.0 | 0.3090 (8) | 0.0063 (17)* | |
O1 | 0.1136 (14) | −0.256 (3) | 0.857 (3) | 0.005 (3)* | |
O2 | 0.1281 (15) | 0.0 | 0.239 (3) | 0.005 (3)* | |
O3 | 0.3793 (15) | 0.0 | 0.582 (3) | 0.005 (3)* |
Zr—O1 | 2.016 (16) | Zr—O2 | 1.756 (16) |
Zr—O1 | 2.016 (16) | Mo—O1 | 1.867 (17) |
Zr—O1 | 2.016 (16) | Mo—O1 | 1.867 (17) |
Zr—O1 | 2.016 (16) | Mo—O2 | 2.012 (16) |
Zr—O2 | 1.756 (16) | Mo—O3 | 1.530 (17) |
O1—Zr—O1 | 87.0 (6) | O1—Zr—O2 | 96.5 (5) |
O1—Zr—O1 | 87.0 (6) | O1—Zr—O2 | 96.5 (5) |
O1—Zr—O1 | 93.0 (6) | O1—Zr—O2 | 96.5 (5) |
O1—Zr—O1 | 93.0 (6) | O2—Zr—O2 | 180 (1) |
O1—Zr—O1 | 180 (1) | O1—Mo—O1 | 109.2 (7) |
O1—Zr—O1 | 180 (1) | O1—Mo—O2 | 103.3 (5) |
O1—Zr—O2 | 83.5 (5) | O1—Mo—O2 | 103.3 (5) |
O1—Zr—O2 | 83.5 (5) | O1—Mo—O3 | 111.7 (6) |
O1—Zr—O2 | 83.5 (5) | O1—Mo—O3 | 111.7 (6) |
O1—Zr—O2 | 83.5 (5) | O2—Mo—O3 | 117.0 (7) |
O1—Zr—O2 | 96.5 (5) |
Mo2O8Zr | V = 312.98 (2) Å3 |
Mr = 411.10 | Z = 2 |
Monoclinic, C2/m | Synchrotron radiation, λ = 0.42496 Å |
a = 9.8358 (3) Å | T = 298 K |
b = 5.98562 (18) Å | light pink |
c = 5.32344 (19) Å | ?, ? × ? × ? mm |
β = 93.004 (2)° |
Synchrotron diffractometer | 2θmin = 3.20°, 2θmax = 20.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2011 data points |
Rp = 0.007 | Profile function: pseudo-Voigt |
Rwp = 0.012 | 53 parameters |
Rexp = 0.007 | (Δ/σ)max = 0.01 |
R(F2) = 0.0536 | Background function: Chebychev polynomial |
χ2 = 3.423 |
Mo2O8Zr | β = 93.004 (2)° |
Mr = 411.10 | V = 312.98 (2) Å3 |
Monoclinic, C2/m | Z = 2 |
a = 9.8358 (3) Å | Synchrotron radiation, λ = 0.42496 Å |
b = 5.98562 (18) Å | T = 298 K |
c = 5.32344 (19) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.20°, 2θmax = 20.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.007 | χ2 = 3.423 |
Rwp = 0.012 | 2011 data points |
Rexp = 0.007 | 53 parameters |
R(F2) = 0.0536 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.023 (3)* | |
Mo1 | 0.3305 (5) | 0.0 | 0.3111 (7) | 0.0070 (16)* | |
O1 | 0.1125 (13) | −0.247 (3) | 0.853 (2) | 0.009 (3)* | |
O2 | 0.1312 (13) | 0.0 | 0.254 (2) | 0.009 (3)* | |
O3 | 0.3735 (13) | 0.0 | 0.601 (3) | 0.009 (3)* |
Zr—O1 | 2.024 (11) | Zr—O2 | 1.820 (12) |
Zr—O1 | 2.024 (11) | Mo—O1 | 1.852 (12) |
Zr—O1 | 2.024 (11) | Mo—O1 | 1.852 (12) |
Zr—O1 | 2.024 (11) | Mo—O2 | 1.967 (14) |
Zr—O2 | 1.820 (12) | Mo—O3 | 1.586 (16) |
O1—Zr—O1 | 86.1 (5) | O1—Zr—O2 | 95.2 (4) |
O1—Zr—O1 | 86.1 (5) | O1—Zr—O2 | 95.2 (4) |
O1—Zr—O1 | 93.9 (5) | O1—Zr—O2 | 95.2 (4) |
O1—Zr—O1 | 93.9 (5) | O2—Zr—O2 | 180 (3) |
O1—Zr—O1 | 180 (2) | O1—Mo—O1 | 109.7 (5) |
O1—Zr—O1 | 180 (2) | O1—Mo—O2 | 104.8 (4) |
O1—Zr—O2 | 84.8 (4) | O1—Mo—O2 | 104.8 (4) |
O1—Zr—O2 | 84.8 (4) | O1—Mo—O3 | 112.8 (4) |
O1—Zr—O2 | 84.8 (4) | O1—Mo—O3 | 112.8 (4) |
O1—Zr—O2 | 84.8 (4) | O2—Mo—O3 | 111.5 (6) |
O1—Zr—O2 | 95.2 (4) |
Mo2O8Zr | V = 312.16 (2) Å3 |
Mr = 411.10 | Z = 2 |
Monoclinic, C2/m | Synchrotron radiation, λ = 0.42496 Å |
a = 9.8256 (3) Å | T = 298 K |
b = 5.98980 (18) Å | light pink |
c = 5.31146 (19) Å | ?, ? × ? × ? mm |
β = 93.039 (2)° |
Synchrotron diffractometer | 2θmin = 3.20°, 2θmax = 20.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2015 data points |
Rp = 0.007 | Profile function: pseudo-Voigt |
Rwp = 0.011 | 53 parameters |
Rexp = 0.006 | (Δ/σ)max = 0.01 |
R(F2) = 0.0485 | Background function: Chebychev polynomial |
χ2 = 3.168 |
Mo2O8Zr | β = 93.039 (2)° |
Mr = 411.10 | V = 312.16 (2) Å3 |
Monoclinic, C2/m | Z = 2 |
a = 9.8256 (3) Å | Synchrotron radiation, λ = 0.42496 Å |
b = 5.98980 (18) Å | T = 298 K |
c = 5.31146 (19) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.20°, 2θmax = 20.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.007 | χ2 = 3.168 |
Rwp = 0.011 | 2015 data points |
Rexp = 0.006 | 53 parameters |
R(F2) = 0.0485 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.022 (3)* | |
Mo1 | 0.3308 (5) | 0.0 | 0.3123 (7) | 0.0033 (17)* | |
O1 | 0.1112 (14) | −0.248 (3) | 0.850 (3) | 0.009 (3)* | |
O2 | 0.1301 (14) | 0.0 | 0.256 (2) | 0.009 (3)* | |
O3 | 0.3752 (13) | 0.0 | 0.612 (3) | 0.009 (3)* |
Zr—O1 | 2.026 (15) | Zr—O2 | 1.816 (12) |
Zr—O1 | 2.026 (15) | Mo—O1 | 1.848 (16) |
Zr—O1 | 2.026 (15) | Mo—O1 | 1.848 (16) |
Zr—O1 | 2.026 (15) | Mo—O2 | 1.980 (14) |
Zr—O2 | 1.816 (12) | Mo—O3 | 1.629 (16) |
O1—Zr—O1 | 85.7 (6) | O1—Zr—O2 | 94.5 (4) |
O1—Zr—O1 | 85.7 (6) | O1—Zr—O2 | 94.5 (4) |
O1—Zr—O1 | 94.3 (6) | O1—Zr—O2 | 94.5 (4) |
O1—Zr—O1 | 94.3 (6) | O2—Zr—O2 | 180 (2) |
O1—Zr—O1 | 180 (2) | O1—Mo—O1 | 109.6 (6) |
O1—Zr—O1 | 180 (2) | O1—Mo—O2 | 105.2 (4) |
O1—Zr—O2 | 85.5 (4) | O1—Mo—O2 | 105.2 (4) |
O1—Zr—O2 | 85.5 (4) | O1—Mo—O3 | 112.6 (4) |
O1—Zr—O2 | 85.5 (4) | O1—Mo—O3 | 112.6 (4) |
O1—Zr—O2 | 85.5 (4) | O2—Mo—O3 | 111.2 (6) |
O1—Zr—O2 | 94.5 (4) |
Mo2O8Zr | V = 309.42 (2) Å3 |
Mr = 411.10 | Z = 2 |
Monoclinic, C2/m | Synchrotron radiation, λ = 0.42496 Å |
a = 9.7966 (3) Å | T = 298 K |
b = 5.98422 (17) Å | light pink |
c = 5.28547 (18) Å | ?, ? × ? × ? mm |
β = 93.069 (2)° |
Synchrotron diffractometer | 2θmin = 3.20°, 2θmax = 20.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2011 data points |
Rp = 0.006 | Profile function: pseudo-Voigt |
Rwp = 0.011 | 53 parameters |
Rexp = 0.006 | (Δ/σ)max = 0.01 |
R(F2) = 0.0460 | Background function: Chebychev polynomial |
χ2 = 2.856 |
Mo2O8Zr | β = 93.069 (2)° |
Mr = 411.10 | V = 309.42 (2) Å3 |
Monoclinic, C2/m | Z = 2 |
a = 9.7966 (3) Å | Synchrotron radiation, λ = 0.42496 Å |
b = 5.98422 (17) Å | T = 298 K |
c = 5.28547 (18) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.20°, 2θmax = 20.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.006 | χ2 = 2.856 |
Rwp = 0.011 | 2011 data points |
Rexp = 0.006 | 53 parameters |
R(F2) = 0.0460 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.017 (3)* | |
Mo1 | 0.3300 (5) | 0.0 | 0.3119 (7) | 0.0098 (16)* | |
O1 | 0.1121 (12) | −0.246 (2) | 0.849 (2) | 0.002 (3)* | |
O2 | 0.1336 (13) | 0.0 | 0.258 (2) | 0.002 (3)* | |
O3 | 0.3730 (12) | 0.0 | 0.609 (2) | 0.002 (3)* |
Zr—O1 | 2.023 (11) | Zr—O2 | 1.834 (12) |
Zr—O1 | 2.023 (11) | Mo—O1 | 1.846 (12) |
Zr—O1 | 2.023 (11) | Mo—O1 | 1.846 (12) |
Zr—O1 | 2.023 (11) | Mo—O2 | 1.934 (11) |
Zr—O2 | 1.834 (12) | Mo—O3 | 1.606 (11) |
O1—Zr—O1 | 86.6 (4) | O1—Zr—O2 | 94.8 (4) |
O1—Zr—O1 | 86.6 (4) | O1—Zr—O2 | 94.8 (4) |
O1—Zr—O1 | 93.4 (4) | O1—Zr—O2 | 94.8 (4) |
O1—Zr—O1 | 93.4 (4) | O2—Zr—O2 | 180 (2) |
O1—Zr—O1 | 180 (2) | O1—Mo—O1 | 110.9 (5) |
O1—Zr—O1 | 180 (2) | O1—Mo—O2 | 105.3 (4) |
O1—Zr—O2 | 85.2 (4) | O1—Mo—O2 | 105.3 (4) |
O1—Zr—O2 | 85.2 (4) | O1—Mo—O3 | 112.0 (4) |
O1—Zr—O2 | 85.2 (4) | O1—Mo—O3 | 112.0 (4) |
O1—Zr—O2 | 85.2 (4) | O2—Mo—O3 | 111.0 (5) |
O1—Zr—O2 | 94.8 (4) |
Mo2O8Zr | V = 308.25 (2) Å3 |
Mr = 411.10 | Z = 2 |
Monoclinic, C2/m | Synchrotron radiation, λ = 0.42496 Å |
a = 9.7834 (3) Å | T = 298 K |
b = 5.99225 (17) Å | light pink |
c = 5.26578 (18) Å | ?, ? × ? × ? mm |
β = 93.116 (2)° |
Synchrotron diffractometer | 2θmin = 3.20°, 2θmax = 20.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2011 data points |
Rp = 0.006 | Profile function: pseudo-Voigt |
Rwp = 0.011 | 53 parameters |
Rexp = 0.006 | (Δ/σ)max = 0.01 |
R(F2) = 0.0405 | Background function: Chebychev polynomial |
χ2 = 2.856 |
Mo2O8Zr | β = 93.116 (2)° |
Mr = 411.10 | V = 308.25 (2) Å3 |
Monoclinic, C2/m | Z = 2 |
a = 9.7834 (3) Å | Synchrotron radiation, λ = 0.42496 Å |
b = 5.99225 (17) Å | T = 298 K |
c = 5.26578 (18) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.20°, 2θmax = 20.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.006 | χ2 = 2.856 |
Rwp = 0.011 | 2011 data points |
Rexp = 0.006 | 53 parameters |
R(F2) = 0.0405 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.010 (3)* | |
Mo1 | 0.3306 (5) | 0.0 | 0.3131 (8) | 0.0140 (17)* | |
O1 | 0.1132 (11) | −0.243 (2) | 0.849 (2) | 0.001 (3)* | |
O2 | 0.1338 (14) | 0.0 | 0.258 (2) | 0.001 (3)* | |
O3 | 0.3709 (12) | 0.0 | 0.613 (2) | 0.001 (3)* |
Zr—O1 | 2.022 (11) | Zr—O2 | 1.828 (12) |
Zr—O1 | 2.022 (11) | Mo—O1 | 1.853 (12) |
Zr—O1 | 2.022 (11) | Mo—O1 | 1.853 (12) |
Zr—O1 | 2.022 (11) | Mo—O2 | 1.937 (14) |
Zr—O2 | 1.828 (12) | Mo—O3 | 1.608 (11) |
O1—Zr—O1 | 87.4 (4) | O1—Zr—O2 | 95.1 (4) |
O1—Zr—O1 | 87.4 (4) | O1—Zr—O2 | 95.1 (4) |
O1—Zr—O1 | 92.6 (4) | O1—Zr—O2 | 95.1 (4) |
O1—Zr—O1 | 92.6 (4) | O2—Zr—O2 | 180 (3) |
O1—Zr—O1 | 180 (1) | O1—Mo—O1 | 111.8 (5) |
O1—Zr—O1 | 180 (1) | O1—Mo—O2 | 104.5 (4) |
O1—Zr—O2 | 84.9 (4) | O1—Mo—O2 | 104.5 (4) |
O1—Zr—O2 | 84.9 (4) | O1—Mo—O3 | 112.6 (4) |
O1—Zr—O2 | 84.9 (4) | O1—Mo—O3 | 112.6 (4) |
O1—Zr—O2 | 84.9 (4) | O2—Mo—O3 | 110.1 (6) |
O1—Zr—O2 | 95.1 (4) |
Mo2O8Zr | V = 306.52 (2) Å3 |
Mr = 411.10 | Z = 2 |
Monoclinic, C2/m | Synchrotron radiation, λ = 0.42496 Å |
a = 9.7643 (3) Å | T = 298 K |
b = 5.99021 (18) Å | light pink |
c = 5.24841 (19) Å | ?, ? × ? × ? mm |
β = 93.140 (2)° |
Synchrotron diffractometer | 2θmin = 3.20°, 2θmax = 20.00° |
Specimen mounting: diamond anvil cell |
Refinement on F2 | 2011 data points |
Rp = 0.006 | Profile function: pseudo-Voigt |
Rwp = 0.010 | 53 parameters |
Rexp = 0.006 | (Δ/σ)max = 0.01 |
R(F2) = 0.0411 | Background function: Chebychev polynomial |
χ2 = 2.722 |
Mo2O8Zr | β = 93.140 (2)° |
Mr = 411.10 | V = 306.52 (2) Å3 |
Monoclinic, C2/m | Z = 2 |
a = 9.7643 (3) Å | Synchrotron radiation, λ = 0.42496 Å |
b = 5.99021 (18) Å | T = 298 K |
c = 5.24841 (19) Å | ?, ? × ? × ? mm |
Synchrotron diffractometer | 2θmin = 3.20°, 2θmax = 20.00° |
Specimen mounting: diamond anvil cell |
Rp = 0.006 | χ2 = 2.722 |
Rwp = 0.010 | 2011 data points |
Rexp = 0.006 | 53 parameters |
R(F2) = 0.0411 |
x | y | z | Uiso*/Ueq | ||
Zr1 | 0.0 | 0.0 | 0.0 | 0.010 (3)* | |
Mo1 | 0.3310 (6) | 0.0 | 0.3148 (9) | 0.0153 (18)* | |
O1 | 0.1139 (11) | −0.246 (3) | 0.857 (3) | 0.005 (3)* | |
O2 | 0.1337 (15) | 0.0 | 0.260 (2) | 0.005 (3)* | |
O3 | 0.3710 (13) | 0.0 | 0.614 (3) | 0.005 (3)* |
Zr—O1 | 2.020 (12) | Zr—O2 | 1.829 (12) |
Zr—O1 | 2.020 (12) | Mo—O1 | 1.857 (13) |
Zr—O1 | 2.020 (12) | Mo—O1 | 1.857 (13) |
Zr—O1 | 2.020 (12) | Mo—O2 | 1.938 (14) |
Zr—O2 | 1.829 (12) | Mo—O3 | 1.598 (16) |
O1—Zr—O1 | 85.8 (5) | O1—Zr—O2 | 96.0 (5) |
O1—Zr—O1 | 85.8 (5) | O1—Zr—O2 | 96.0 (5) |
O1—Zr—O1 | 94.2 (5) | O1—Zr—O2 | 96.0 (5) |
O1—Zr—O1 | 94.2 (5) | O2—Zr—O2 | 180 (2) |
O1—Zr—O1 | 180 (2) | O1—Mo—O1 | 109.4 (6) |
O1—Zr—O1 | 180 (2) | O1—Mo—O2 | 104.0 (4) |
O1—Zr—O2 | 84.0 (4) | O1—Mo—O2 | 104.0 (4) |
O1—Zr—O2 | 84.0 (4) | O1—Mo—O3 | 114.3 (5) |
O1—Zr—O2 | 84.0 (4) | O1—Mo—O3 | 114.3 (5) |
O1—Zr—O2 | 84.0 (4) | O2—Mo—O3 | 109.9 (6) |
O1—Zr—O2 | 96.0 (5) |
Experimental details
(0.20GPa) | (0.32GPa) | (0.42GPa) | (0.56GPa) | |
Crystal data | ||||
Chemical formula | Mo2O8Zr | Mo2O8Zr | Mo2O8Zr | Mo2O8Zr |
Mr | 411.10 | 411.10 | 411.10 | 411.10 |
Crystal system, space group | Trigonal, P31c | Trigonal, P31c | Trigonal, P31c | Trigonal, P31c |
Temperature (K) | 298 | 298 | 298 | 298 |
a, b, c (Å) | 10.13792 (6), 10.13792 (6), 11.71279 (15) | 10.14778 (9), 10.14778 (9), 11.6780 (2) | 10.13896 (8), 10.13896 (8), 11.60753 (19) | 10.14226 (12), 10.14226 (12), 11.5334 (3) |
α, β, γ (°) | 90, 90, 120 | 90, 90, 120 | 90, 90, 120 | 90, 90, 120 |
V (Å3) | 1042.54 (1) | 1041.46 (2) | 1033.38 (2) | 1027.46 (3) |
Z | 6 | 6 | 6 | 6 |
Radiation type | Synchrotron, λ = 0.42496 Å | Synchrotron, λ = 0.42496 Å | Synchrotron, λ = 0.42496 Å | Synchrotron, λ = 0.42496 Å |
Specimen shape, size (mm) | ?, ? × ? × ? | ?, ? × ? × ? | ?, ? × ? × ? | ?, ? × ? × ? |
Data collection | ||||
Diffractometer | Synchrotron diffractometer | Synchrotron diffractometer | Synchrotron diffractometer | Synchrotron diffractometer |
Specimen mounting | Diamond anvil cell | Diamond anvil cell | Diamond anvil cell | Diamond anvil cell |
Data collection mode | ? | ? | ? | ? |
Scan method | ? | ? | ? | ? |
2θ values (°) | 2θmin = 3.00 2θmax = 22.00 2θstep = ? | 2θmin = 3.00 2θmax = 22.00 2θstep = ? | 2θmin = 3.00 2θmax = 22.00 2θstep = ? | 2θmin = 3.00 2θmax = 22.00 2θstep = ? |
Refinement | ||||
R factors and goodness of fit | Rp = 0.005, Rwp = 0.007, Rexp = 0.008, R(F2) = 0.0338, χ2 = 0.846 | Rp = 0.006, Rwp = 0.009, Rexp = 0.008, R(F2) = 0.0327, χ2 = 1.300 | Rp = 0.007, Rwp = 0.012, Rexp = 0.008, R(F2) = 0.0420, χ2 = 1.988 | Rp = 0.008, Rwp = 0.013, Rexp = 0.008, R(F2) = 0.0464, χ2 = 2.528 |
No. of data points | 2273 | 2276 | 2273 | 2276 |
No. of parameters | 50 | 54 | 22 | 54 |
No. of restraints | ? | ? | ? | ? |
(0.63GPa) | (0.72GPa) | (0.80GPa) | (0.90GPa) | |
Crystal data | ||||
Chemical formula | Mo2O8Zr | Mo2O8Zr | Mo2O8Zr | Mo2O8Zr |
Mr | 411.10 | 411.10 | 411.10 | 411.10 |
Crystal system, space group | Trigonal, P31c | Trigonal, P31c | Trigonal, P31c | Trigonal, P31c |
Temperature (K) | 298 | 298 | 298 | 298 |
a, b, c (Å) | 10.13168 (11), 10.13168 (11), 11.4790 (3) | 10.13750 (11), 10.13750 (11), 11.4395 (3) | 10.13183 (10), 10.13183 (10), 11.3877 (3) | 10.1264 (1), 10.1264 (1), 11.3252 (2) |
α, β, γ (°) | 90, 90, 120 | 90, 90, 120 | 90, 90, 120 | 90, 90, 120 |
V (Å3) | 1020.46 (3) | 1018.11 (3) | 1012.37 (3) | 1005.75 (2) |
Z | 6 | 6 | 6 | 6 |
Radiation type | Synchrotron, λ = 0.42496 Å | Synchrotron, λ = 0.42496 Å | Synchrotron, λ = 0.42496 Å | Synchrotron, λ = 0.42496 Å |
Specimen shape, size (mm) | ?, ? × ? × ? | ?, ? × ? × ? | ?, ? × ? × ? | ?, ? × ? × ? |
Data collection | ||||
Diffractometer | Synchrotron diffractometer | Synchrotron diffractometer | Synchrotron diffractometer | Synchrotron diffractometer |
Specimen mounting | Diamond anvil cell | Diamond anvil cell | Diamond anvil cell | Diamond anvil cell |
Data collection mode | ? | ? | ? | ? |
Scan method | ? | ? | ? | ? |
2θ values (°) | 2θmin = 3.00 2θmax = 22.00 2θstep = ? | 2θmin = 3.00 2θmax = 22.00 2θstep = ? | 2θmin = 3.00 2θmax = 22.00 2θstep = ? | 2θmin = 3.00 2θmax = 22.00 2θstep = ? |
Refinement | ||||
R factors and goodness of fit | Rp = 0.007, Rwp = 0.012, Rexp = 0.008, R(F2) = 0.0484, χ2 = 2.190 | Rp = 0.007, Rwp = 0.012, Rexp = 0.008, R(F2) = 0.0433, χ2 = 2.220 | Rp = 0.006, Rwp = 0.010, Rexp = 0.008, R(F2) = 0.0362, χ2 = 1.742 | Rp = 0.006, Rwp = 0.010, Rexp = 0.008, R(F2) = 0.0339, χ2 = 1.613 |
No. of data points | 2269 | 2273 | 2273 | 2273 |
No. of parameters | 54 | 54 | 54 | 54 |
No. of restraints | ? | ? | ? | ? |
(1.18GPa) | (1.48GPa) | (1.53GPa) | (1.64GPa) | |
Crystal data | ||||
Chemical formula | Mo2O8Zr | Mo2O8Zr | Mo2O8Zr | Mo2O8Zr |
Mr | 411.10 | 411.10 | 411.10 | 411.10 |
Crystal system, space group | Monoclinic, C2/m | Monoclinic, C2/m | Monoclinic, C2/m | Monoclinic, C2/m |
Temperature (K) | 298 | 298 | 298 | 298 |
a, b, c (Å) | 9.8821 (3), 5.9699 (2), 5.3888 (2) | 9.8358 (3), 5.98562 (18), 5.32344 (19) | 9.8256 (3), 5.98980 (18), 5.31146 (19) | 9.7966 (3), 5.98422 (17), 5.28547 (18) |
α, β, γ (°) | 90, 92.818 (3), 90 | 90, 93.004 (2), 90 | 90, 93.039 (2), 90 | 90, 93.069 (2), 90 |
V (Å3) | 317.53 (2) | 312.98 (2) | 312.16 (2) | 309.42 (2) |
Z | 2 | 2 | 2 | 2 |
Radiation type | Synchrotron, λ = 0.42496 Å | Synchrotron, λ = 0.42496 Å | Synchrotron, λ = 0.42496 Å | Synchrotron, λ = 0.42496 Å |
Specimen shape, size (mm) | ?, ? × ? × ? | ?, ? × ? × ? | ?, ? × ? × ? | ?, ? × ? × ? |
Data collection | ||||
Diffractometer | Synchrotron diffractometer | Synchrotron diffractometer | Synchrotron diffractometer | Synchrotron diffractometer |
Specimen mounting | Diamond anvil cell | Diamond anvil cell | Diamond anvil cell | Diamond anvil cell |
Data collection mode | ? | ? | ? | ? |
Scan method | ? | ? | ? | ? |
2θ values (°) | 2θmin = 3.20 2θmax = 20.00 2θstep = ? | 2θmin = 3.20 2θmax = 20.00 2θstep = ? | 2θmin = 3.20 2θmax = 20.00 2θstep = ? | 2θmin = 3.20 2θmax = 20.00 2θstep = ? |
Refinement | ||||
R factors and goodness of fit | Rp = 0.009, Rwp = 0.014, Rexp = 0.007, R(F2) = 0.0664, χ2 = 4.162 | Rp = 0.007, Rwp = 0.012, Rexp = 0.007, R(F2) = 0.0536, χ2 = 3.423 | Rp = 0.007, Rwp = 0.011, Rexp = 0.006, R(F2) = 0.0485, χ2 = 3.168 | Rp = 0.006, Rwp = 0.011, Rexp = 0.006, R(F2) = 0.0460, χ2 = 2.856 |
No. of data points | 2011 | 2011 | 2015 | 2011 |
No. of parameters | 53 | 53 | 53 | 53 |
No. of restraints | ? | ? | ? | ? |
(1.79GPa) | (1.87GPa) | |
Crystal data | ||
Chemical formula | Mo2O8Zr | Mo2O8Zr |
Mr | 411.10 | 411.10 |
Crystal system, space group | Monoclinic, C2/m | Monoclinic, C2/m |
Temperature (K) | 298 | 298 |
a, b, c (Å) | 9.7834 (3), 5.99225 (17), 5.26578 (18) | 9.7643 (3), 5.99021 (18), 5.24841 (19) |
α, β, γ (°) | 90, 93.116 (2), 90 | 90, 93.140 (2), 90 |
V (Å3) | 308.25 (2) | 306.52 (2) |
Z | 2 | 2 |
Radiation type | Synchrotron, λ = 0.42496 Å | Synchrotron, λ = 0.42496 Å |
Specimen shape, size (mm) | ?, ? × ? × ? | ?, ? × ? × ? |
Data collection | ||
Diffractometer | Synchrotron diffractometer | Synchrotron diffractometer |
Specimen mounting | Diamond anvil cell | Diamond anvil cell |
Data collection mode | ? | ? |
Scan method | ? | ? |
2θ values (°) | 2θmin = 3.20 2θmax = 20.00 2θstep = ? | 2θmin = 3.20 2θmax = 20.00 2θstep = ? |
Refinement | ||
R factors and goodness of fit | Rp = 0.006, Rwp = 0.011, Rexp = 0.006, R(F2) = 0.0405, χ2 = 2.856 | Rp = 0.006, Rwp = 0.010, Rexp = 0.006, R(F2) = 0.0411, χ2 = 2.722 |
No. of data points | 2011 | 2011 |
No. of parameters | 53 | 53 |
No. of restraints | ? | ? |
Computer programs: GSAS.