High-pressure structures of α- and δ-ZrMo2O8

Krogh Andersen, A.M.; Carlson, S.

doi:10.1107/S0108768100013215

High-pressure structures of α- and δ-ZrMo₂O₈

In situ high-pressure synchrotron X-ray powder diffraction studies of trigonal α-ZrMo₂O₈, zirconium molybdate, have been performed from ambient conditions to 1.9 GPa, over the α–δ phase transition at 1.06–1.11 GPa. The monoclinic structure of δ-ZrMo₂O₈, stable between 1.1 and 2.5 GPa at 298 K, has been solved by direct methods and refined using the Rietveld method. Significant distortions of the ZrO₆ and MoO₄ polyhedral elements are observed for δ-ZrMo₂O₈, as compared to the ambient conditions of the α-phase, while the packing of anions becomes more symmetric at high pressure.

Keywords: high-pressure diffraction; distortion; framework structures.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100013215/sn0004sup1.cif Contains datablocks global, 0.20GPa, 0.32GPa, 0.42GPa, 0.56GPa, 0.63GPa, 0.72GPa, 0.80GPa, 0.90GPa, 1.18GPa, 1.48GPa, 1.53GPa, 1.64GPa, 1.79GPa, 1.87GPa
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.20GPasup2.rtv Contains datablock 0.20GPa
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.20GPasup3.hkl Contains datablock 0.20GPa
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.32GPasup4.rtv Contains datablock 0.32GPa
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.32GPasup5.hkl Contains datablock 0.32GPa
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.42GPasup6.rtv Contains datablock 0.42GPa
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.42GPasup7.hkl Contains datablock 0.42GPa
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.56GPasup8.rtv Contains datablock 0.56GPa
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.56sup9.hkl Contains datablock 0.56
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.63GPasup10.rtv Supplementary material
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.63GPasup11.hkl Supplementary material
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.72GPasup12.rtv Supplementary material
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.72GPasup13.hkl Supplementary material
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.80GPasup14.rtv Supplementary material
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.80GPasup15.hkl Supplementary material
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn000400.90GPasup16.rtv Supplementary material
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00040.90GPasup17.hkl Supplementary material
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.18GPasup18.rtv Supplementary material
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.18GPasup19.hkl Supplementary material
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.48GPasup20.rtv Supplementary material
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.48GPasup21.hkl Supplementary material
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.53GPasup22.rtv Supplementary material
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.53GPasup23.hkl Supplementary material
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.64GPasup24.rtv Supplementary material
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.64GPasup25.hkl Supplementary material
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.79GPasup26.rtv Supplementary material
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.79GPasup27.hkl Supplementary material
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.87GPasup28.rtv Supplementary material
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768100013215/sn00041.87GPasup29.hkl Supplementary material
	Portable Document Format (PDF) file https://doi.org/10.1107/S0108768100013215/sn0004sup30.pdf Supplementary material

Computing details top

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.

Figures top

(0.20GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	Z = 6
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2273 data points
R_p = 0.005	Profile function: pseudo-Voigt
R_wp = 0.007	50 parameters
R_exp = 0.008	(Δ/σ)_max = 0.01
R(F²) = 0.0338	Background function: Chebychev polynomial
χ² = 0.846

Crystal data top

Mo₂O₈Zr	V = 1042.54 (1) Å³
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.005	χ² = 0.846
R_wp = 0.007	2273 data points
R_exp = 0.008	50 parameters
R(F²) = 0.0338

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(0.32GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	Z = 6
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2276 data points
R_p = 0.006	Profile function: pseudo-Voigt
R_wp = 0.009	54 parameters
R_exp = 0.008	(Δ/σ)_max = 0.01
R(F²) = 0.0327	Background function: Chebychev polynomial
χ² = 1.300

Crystal data top

Mo₂O₈Zr	V = 1041.46 (2) Å³
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.006	χ² = 1.300
R_wp = 0.009	2276 data points
R_exp = 0.008	54 parameters
R(F²) = 0.0327

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(0.42GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	Z = 6
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2273 data points
R_p = 0.007	Profile function: pseudo-Voigt
R_wp = 0.012	22 parameters
R_exp = 0.008	(Δ/σ)_max = 0.01
R(F²) = 0.0420	Background function: Chebychev polynomial
χ² = 1.988

Crystal data top

Mo₂O₈Zr	V = 1033.38 (2) Å³
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.007	χ² = 1.988
R_wp = 0.012	2273 data points
R_exp = 0.008	22 parameters
R(F²) = 0.0420

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(0.56GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	Z = 6
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2276 data points
R_p = 0.008	Profile function: pseudo-Voigt
R_wp = 0.013	54 parameters
R_exp = 0.008	(Δ/σ)_max = 0.01
R(F²) = 0.0464	Background function: Chebychev polynomial
χ² = 2.528

Crystal data top

Mo₂O₈Zr	V = 1027.46 (3) Å³
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.008	χ² = 2.528
R_wp = 0.013	2276 data points
R_exp = 0.008	54 parameters
R(F²) = 0.0464

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(0.63GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	Z = 6
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2269 data points
R_p = 0.007	Profile function: pseudo-Voigt
R_wp = 0.012	54 parameters
R_exp = 0.008	(Δ/σ)_max = 0.01
R(F²) = 0.0484	Background function: Chebychev polynomial
χ² = 2.190

Crystal data top

Mo₂O₈Zr	V = 1020.46 (3) Å³
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.007	χ² = 2.190
R_wp = 0.012	2269 data points
R_exp = 0.008	54 parameters
R(F²) = 0.0484

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(0.72GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	Z = 6
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2273 data points
R_p = 0.007	Profile function: pseudo-Voigt
R_wp = 0.012	54 parameters
R_exp = 0.008	(Δ/σ)_max = 0.01
R(F²) = 0.0433	Background function: Chebychev polynomial
χ² = 2.220

Crystal data top

Mo₂O₈Zr	V = 1018.11 (3) Å³
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.007	χ² = 2.220
R_wp = 0.012	2273 data points
R_exp = 0.008	54 parameters
R(F²) = 0.0433

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(0.80GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	Z = 6
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2273 data points
R_p = 0.006	Profile function: pseudo-Voigt
R_wp = 0.010	54 parameters
R_exp = 0.008	(Δ/σ)_max = 0.01
R(F²) = 0.0362	Background function: Chebychev polynomial
χ² = 1.742

Crystal data top

Mo₂O₈Zr	V = 1012.37 (3) Å³
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.006	χ² = 1.742
R_wp = 0.010	2273 data points
R_exp = 0.008	54 parameters
R(F²) = 0.0362

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(0.90GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	Z = 6
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2273 data points
R_p = 0.006	Profile function: pseudo-Voigt
R_wp = 0.010	54 parameters
R_exp = 0.008	(Δ/σ)_max = 0.01
R(F²) = 0.0339	Background function: Chebychev polynomial
χ² = 1.613

Crystal data top

Mo₂O₈Zr	V = 1005.75 (2) Å³
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.00°, 2θ_max = 22.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.006	χ² = 1.613
R_wp = 0.010	2273 data points
R_exp = 0.008	54 parameters
R(F²) = 0.0339

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(1.18GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	V = 317.53 (2) Å³
M_r = 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)°

Data collection top

Synchrotron diffractometer	2θ_min = 3.20°, 2θ_max = 20.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2011 data points
R_p = 0.009	Profile function: pseudo-Voigt
R_wp = 0.014	53 parameters
R_exp = 0.007	(Δ/σ)_max = 0.01
R(F²) = 0.0664	Background function: Chebychev polynomial
χ² = 4.162

Crystal data top

Mo₂O₈Zr	β = 92.818 (3)°
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.20°, 2θ_max = 20.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.009	χ² = 4.162
R_wp = 0.014	2011 data points
R_exp = 0.007	53 parameters
R(F²) = 0.0664

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(1.48GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	V = 312.98 (2) Å³
M_r = 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)°

Data collection top

Synchrotron diffractometer	2θ_min = 3.20°, 2θ_max = 20.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2011 data points
R_p = 0.007	Profile function: pseudo-Voigt
R_wp = 0.012	53 parameters
R_exp = 0.007	(Δ/σ)_max = 0.01
R(F²) = 0.0536	Background function: Chebychev polynomial
χ² = 3.423

Crystal data top

Mo₂O₈Zr	β = 93.004 (2)°
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.20°, 2θ_max = 20.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.007	χ² = 3.423
R_wp = 0.012	2011 data points
R_exp = 0.007	53 parameters
R(F²) = 0.0536

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(1.53GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	V = 312.16 (2) Å³
M_r = 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)°

Data collection top

Synchrotron diffractometer	2θ_min = 3.20°, 2θ_max = 20.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2015 data points
R_p = 0.007	Profile function: pseudo-Voigt
R_wp = 0.011	53 parameters
R_exp = 0.006	(Δ/σ)_max = 0.01
R(F²) = 0.0485	Background function: Chebychev polynomial
χ² = 3.168

Crystal data top

Mo₂O₈Zr	β = 93.039 (2)°
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.20°, 2θ_max = 20.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.007	χ² = 3.168
R_wp = 0.011	2015 data points
R_exp = 0.006	53 parameters
R(F²) = 0.0485

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(1.64GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	V = 309.42 (2) Å³
M_r = 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)°

Data collection top

Synchrotron diffractometer	2θ_min = 3.20°, 2θ_max = 20.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2011 data points
R_p = 0.006	Profile function: pseudo-Voigt
R_wp = 0.011	53 parameters
R_exp = 0.006	(Δ/σ)_max = 0.01
R(F²) = 0.0460	Background function: Chebychev polynomial
χ² = 2.856

Crystal data top

Mo₂O₈Zr	β = 93.069 (2)°
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.20°, 2θ_max = 20.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.006	χ² = 2.856
R_wp = 0.011	2011 data points
R_exp = 0.006	53 parameters
R(F²) = 0.0460

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(1.79GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	V = 308.25 (2) Å³
M_r = 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)°

Data collection top

Synchrotron diffractometer	2θ_min = 3.20°, 2θ_max = 20.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2011 data points
R_p = 0.006	Profile function: pseudo-Voigt
R_wp = 0.011	53 parameters
R_exp = 0.006	(Δ/σ)_max = 0.01
R(F²) = 0.0405	Background function: Chebychev polynomial
χ² = 2.856

Crystal data top

Mo₂O₈Zr	β = 93.116 (2)°
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.20°, 2θ_max = 20.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.006	χ² = 2.856
R_wp = 0.011	2011 data points
R_exp = 0.006	53 parameters
R(F²) = 0.0405

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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)

(1.87GPa) Zirconium molybdate top

Crystal data top

Mo₂O₈Zr	V = 306.52 (2) Å³
M_r = 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)°

Data collection top

Synchrotron diffractometer	2θ_min = 3.20°, 2θ_max = 20.00°
Specimen mounting: diamond anvil cell

Refinement top

Refinement on F²	2011 data points
R_p = 0.006	Profile function: pseudo-Voigt
R_wp = 0.010	53 parameters
R_exp = 0.006	(Δ/σ)_max = 0.01
R(F²) = 0.0411	Background function: Chebychev polynomial
χ² = 2.722

Crystal data top

Mo₂O₈Zr	β = 93.140 (2)°
M_r = 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

Data collection top

Synchrotron diffractometer	2θ_min = 3.20°, 2θ_max = 20.00°
Specimen mounting: diamond anvil cell

Refinement top

R_p = 0.006	χ² = 2.722
R_wp = 0.010	2011 data points
R_exp = 0.006	53 parameters
R(F²) = 0.0411

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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)*

Geometric parameters (Å, º) top

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
M_r	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 (°)	2θ_min = 3.00 2θ_max = 22.00 2θ_step = ?	2θ_min = 3.00 2θ_max = 22.00 2θ_step = ?	2θ_min = 3.00 2θ_max = 22.00 2θ_step = ?	2θ_min = 3.00 2θ_max = 22.00 2θ_step = ?

Refinement
R factors and goodness of fit	R_p = 0.005, R_wp = 0.007, R_exp = 0.008, R(F²) = 0.0338, χ² = 0.846	R_p = 0.006, R_wp = 0.009, R_exp = 0.008, R(F²) = 0.0327, χ² = 1.300	R_p = 0.007, R_wp = 0.012, R_exp = 0.008, R(F²) = 0.0420, χ² = 1.988	R_p = 0.008, R_wp = 0.013, R_exp = 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
M_r	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 (°)	2θ_min = 3.00 2θ_max = 22.00 2θ_step = ?	2θ_min = 3.00 2θ_max = 22.00 2θ_step = ?	2θ_min = 3.00 2θ_max = 22.00 2θ_step = ?	2θ_min = 3.00 2θ_max = 22.00 2θ_step = ?

Refinement
R factors and goodness of fit	R_p = 0.007, R_wp = 0.012, R_exp = 0.008, R(F²) = 0.0484, χ² = 2.190	R_p = 0.007, R_wp = 0.012, R_exp = 0.008, R(F²) = 0.0433, χ² = 2.220	R_p = 0.006, R_wp = 0.010, R_exp = 0.008, R(F²) = 0.0362, χ² = 1.742	R_p = 0.006, R_wp = 0.010, R_exp = 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
M_r	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 (°)	2θ_min = 3.20 2θ_max = 20.00 2θ_step = ?	2θ_min = 3.20 2θ_max = 20.00 2θ_step = ?	2θ_min = 3.20 2θ_max = 20.00 2θ_step = ?	2θ_min = 3.20 2θ_max = 20.00 2θ_step = ?

Refinement
R factors and goodness of fit	R_p = 0.009, R_wp = 0.014, R_exp = 0.007, R(F²) = 0.0664, χ² = 4.162	R_p = 0.007, R_wp = 0.012, R_exp = 0.007, R(F²) = 0.0536, χ² = 3.423	R_p = 0.007, R_wp = 0.011, R_exp = 0.006, R(F²) = 0.0485, χ² = 3.168	R_p = 0.006, R_wp = 0.011, R_exp = 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
M_r	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 (°)	2θ_min = 3.20 2θ_max = 20.00 2θ_step = ?	2θ_min = 3.20 2θ_max = 20.00 2θ_step = ?

Refinement
R factors and goodness of fit	R_p = 0.006, R_wp = 0.011, R_exp = 0.006, R(F²) = 0.0405, χ² = 2.856	R_p = 0.006, R_wp = 0.010, R_exp = 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.

Format		BIBTeX
		EndNote
		RefMan
		Refer
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Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text