Download citation
Download citation
link to html
The high-pressure structural chemistry of α-zirconium phosphate, α-Zr(HPO4)2·H2O, was studied using in-situ high-pressure diffraction and synchrotron radiation. The layered phosphate was studied under both hydrostatic and non-hydrostatic conditions and Rietveld refinement carried out on the resulting diffraction patterns. It was found that under hydrostatic conditions no uptake of additional water molecules from the pressure-transmitting medium occurred, contrary to what had previously been observed with some zeolite materials and a layered titanium phosphate. Under hydrostatic conditions the sample remained crystalline up to 10 GPa, but under non-hydrostatic conditions the sample amorphized between 7.3 and 9.5 GPa. The calculated bulk modulus, K0 = 15.2 GPa, showed the material to be very compressible with the weak linkages in the structure of the type Zr—O—P.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614011317/zb5035sup1.cif
Contains datablock ZRP_10_publ

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S2052520614011317/zb5035sup2.rtv
Contains datablock ZRP_10_publ

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614011317/zb5035sup3.hkl
Contains datablock ZRP_10_publ

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052520614011317/zb5035sup4.pdf
Rietveld plots for each refinement

Computing details top

Program(s) used to refine structure: GSAS.

(ZRP_10_publ) top
Crystal data top
O9P2Zrc = 13.8705 (15) Å
Mr = 297.16β = 101.296 (9)°
Monoclinic, P21/nV = 558.54 (8) Å3
a = 8.3593 (4) ÅZ = 4
b = 4.9123 (2) ÅT = 298 K
Data collection top
2θmin = 0.004°, 2θmax = 24.996°, 2θstep = 0.008°
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 3 with 19 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. #1(GU) = 0.000 #2(GV) = 242.518 #3(GW) = 0.378 #4(GP) = 0.000 #5(LX) = 1.991 #6(LY) = 0.000 #7(S/L) = 0.0104 #8(H/L) = 0.0005 #9(trns) = 0.00 #10(shft)= 0.0000 #11(stec)= 0.00 #12(ptec)= 1.90 #13(sfec)= 0.00 #14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000 #17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0019 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.00844 parameters
Rwp = 0.0128 restraints
Rexp = 0.069(Δ/σ)max = 6.71
R(F2) = 0.14837Background function: GSAS Background function number 7 with 1 terms. Linear interpolation 1: -0.308080
3125 data pointsPreferred orientation correction: March-Dollase AXIS 1 Ratio= 1.365 Frac 1.000 h= 0.000 k= 0.000 l= 1.000 AXIS 2 Ratio= 1.000 Frac 0.000 h= 0.000 k= 1.000 l= 1.000 AXIS 3 Ratio= 1.000 Frac 0.000 h= 0.000 k= 0.000 l= 1.000 Prefered orientation correction range: Min= 0.39602, Max= 1.58906
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
ZR10.2510 (12)0.244 (2)0.4970 (10)0.0153 (7)*
P20.382 (2)0.747 (6)0.3697 (14)0.01*
P30.1317 (18)0.250 (5)0.3826 (14)0.01*
O40.537 (3)0.896 (5)0.416 (3)0.01*
O50.371 (5)0.465 (6)0.413 (4)0.01*
O60.231 (3)0.859 (6)0.393 (4)0.01*
O70.345 (4)0.751 (10)0.2569 (17)0.01*
O80.255 (4)0.412 (5)0.429 (3)0.01*
O90.119 (5)0.044 (6)0.410 (4)0.01*
O100.169 (4)0.251 (12)0.2695 (17)0.01*
O110.037 (3)0.351 (5)0.383 (3)0.01*
O120.004 (7)0.747 (10)0.257 (4)0.01*
Geometric parameters (Å, º) top
ZR1—P2i3.26 (2)P3—O101.538 (14)
ZR1—P3ii3.21 (3)P3—O111.491 (15)
ZR1—P3iii3.26 (2)O4—ZR1i2.06 (4)
ZR1—O4i2.06 (4)O4—P21.515 (15)
ZR1—O52.00 (4)O5—ZR12.00 (4)
ZR1—O6iv2.37 (3)O5—P21.519 (15)
ZR1—O8iii1.97 (3)O6—ZR1v2.37 (3)
ZR1—O9ii2.10 (4)O6—P21.469 (15)
ZR1—O112.21 (4)O7—P21.534 (14)
P2—ZR1i3.26 (2)O8—ZR1iii1.97 (3)
P2—O41.515 (15)O8—P31.538 (15)
P2—O51.519 (15)O9—ZR1ii2.10 (4)
P2—O61.469 (15)O9—P31.492 (15)
P2—O71.534 (14)O10—P31.538 (14)
P3—ZR1ii3.21 (3)O10—O112.15 (5)
P3—ZR1iii3.26 (2)O11—ZR12.21 (4)
P3—O81.538 (15)O11—P31.491 (15)
P3—O91.492 (15)O11—O102.15 (5)
O4i—ZR1—O592.7 (16)O4—P2—O7114 (3)
O4i—ZR1—O6iv92.4 (13)O5—P2—O698 (2)
O4i—ZR1—O8iii93.3 (16)O5—P2—O7113 (4)
O4i—ZR1—O9ii89.0 (16)O6—P2—O7102 (3)
O4i—ZR1—O11169.9 (15)O8—P3—O9115 (3)
O5—ZR1—O6iv93.5 (16)O8—P3—O10114 (3)
O5—ZR1—O8iii83.1 (18)O8—P3—O11122 (2)
O5—ZR1—O9ii175 (2)O9—P3—O10105 (3)
O5—ZR1—O1183.4 (18)O9—P3—O11107 (2)
O6iv—ZR1—O8iii174 (2)O10—P3—O1190 (2)
O6iv—ZR1—O9ii91.1 (18)ZR1i—O4—P2131 (2)
O6iv—ZR1—O1178.6 (12)ZR1—O5—P2143 (3)
O8iii—ZR1—O9ii92.1 (17)ZR1v—O6—P2117.9 (19)
O8iii—ZR1—O1195.5 (14)ZR1iii—O8—P3136 (2)
O9ii—ZR1—O1195.7 (14)ZR1ii—O9—P3126 (3)
O4—P2—O5113 (3)ZR1—O11—P3124 (3)
O4—P2—O6115 (2)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y, z+1; (iii) x, y+1, z+1; (iv) x, y1, z; (v) x, y+1, z.
 

Follow Acta Cryst. B
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds