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Fast detectors employed at third-generation synchrotrons have reduced collection times significantly and require the optimization of commercial as well as customized software packages for data reduction and analysis. In this paper a procedure to collect, process and analyze single-crystal data sets collected at high pressure at the Extreme Conditions beamline (P02.2) at PETRA III, DESY, is presented. A new data image format called `Esperanto' is introduced that is supported by the commercial software package CrysAlisPro (Agilent Technologies UK Ltd). The new format acts as a vehicle to transform the most common area-detector data formats via a translator software. Such a conversion tool has been developed and converts tiff data collected on a Perkin Elmer detector, as well as data collected on a MAR345/555, to be imported into the CrysAlisPro software. In order to demonstrate the validity of the new approach, a complete structure refinement of boron-mullite (Al5BO9) collected at a pressure of 19.4 (2) GPa is presented. Details pertaining to the data collections and refinements of B-mullite are presented.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0909049513018621/fv5010sup1.cif
Contains datablocks global, I

Computing details top

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
(I) top
Crystal data top
Al2.5B0.5O4.5V = 595.7 (3) Å3
Mr = 144.9Z = 8
Orthorhombic, Cmc21F(000) = 568
Hall symbol: C 2c -2Dx = 3.229 Mg m3
a = 5.5494 (15) ÅX-ray radiation, λ = 0.28988 Å
b = 14.350 (6) ÅT = 293 K
c = 7.481 (2) Å × × mm
Data collection top
449 measured reflectionsθmax = 12.2°, θmin = 1.6°
341 independent reflectionsh = 77
223 reflections with I > 3σ(I)k = 1612
Rint = 0.051l = 89
Refinement top
Refinement on F3 restraints
R[F2 > 2σ(F2)] = 0.0580 constraints
wR(F2) = 0.081Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2)
S = 1.26(Δ/σ)max = 0.046
341 reflectionsΔρmax = 0.86 e Å3
30 parametersΔρmin = 0.78 e Å3
Crystal data top
Al2.5B0.5O4.5V = 595.7 (3) Å3
Mr = 144.9Z = 8
Orthorhombic, Cmc21X-ray radiation, λ = 0.28988 Å
a = 5.5494 (15) ÅT = 293 K
b = 14.350 (6) Å × × mm
c = 7.481 (2) Å
Data collection top
449 measured reflections223 reflections with I > 3σ(I)
341 independent reflectionsRint = 0.051
Refinement top
R[F2 > 2σ(F2)] = 0.05830 parameters
wR(F2) = 0.0813 restraints
S = 1.26Δρmax = 0.86 e Å3
341 reflectionsΔρmin = 0.78 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Al10.2510 (6)0.1172 (4)0.336640.0111 (6)*
Al200.2560 (5)0.5196 (11)0.0111 (6)*
Al300.4454 (5)0.5296 (13)0.0111 (6)*
Al400.3018 (6)0.1671 (12)0.0111 (6)*
B100.0167 (19)0.060 (2)0.012 (5)*
O100.3241 (14)0.710 (2)0.0161 (11)*
O20.2528 (15)0.1877 (9)0.5402 (17)0.0161 (11)*
O300.4528 (12)0.909 (2)0.0161 (11)*
O400.0424 (12)0.417 (2)0.0161 (11)*
O500.3544 (15)0.369 (2)0.0161 (11)*
O600.1925 (15)0.262 (2)0.0161 (11)*
O70.2141 (14)0.0472 (9)0.1317 (18)0.0161 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
Bond lengths (Å) top
Al1—Al1i2.785 (5)Al2—Al4v3.099 (6)
Al1—Al1ii2.764 (5)Al2—O11.73 (2)
Al1—Al22.789 (8)Al2—O21.718 (11)
Al1—Al2iii3.294 (8)Al2—O2i1.718 (11)
Al1—Al3iv3.174 (9)Al2—O51.81 (2)
Al1—Al3iii2.827 (8)Al3—Al43.405 (13)
Al1—Al43.251 (9)Al3—O3vii1.72 (2)
Al1—Al4v3.061 (9)Al3—O51.77 (2)
Al1—O1iii1.874 (13)Al3—O7v1.764 (10)
Al1—O21.828 (14)Al3—O7viii1.764 (10)
Al1—O3iii1.792 (12)Al4—O2iii1.675 (11)
Al1—O41.858 (12)Al4—O2ix1.675 (11)
Al1—O61.848 (14)Al4—O51.689 (19)
Al1—O71.844 (14)Al4—O61.72 (2)
Al2—Al32.719 (11)B1—O4x1.36 (3)
Al2—Al42.718 (12)B1—O71.376 (15)
Al2—Al4vi3.099 (6)B1—O7i1.376 (15)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z; (iii) x+1/2, y+1/2, z1/2; (iv) x+1/2, y1/2, z; (v) x+1/2, y+1/2, z+1/2; (vi) x1/2, y+1/2, z+1/2; (vii) x, y+1, z1/2; (viii) x1/2, y+1/2, z+1/2; (ix) x1/2, y+1/2, z1/2; (x) x, y, z1/2.

Experimental details

Crystal data
Chemical formulaAl2.5B0.5O4.5
Mr144.9
Crystal system, space groupOrthorhombic, Cmc21
Temperature (K)293
a, b, c (Å)5.5494 (15), 14.350 (6), 7.481 (2)
V3)595.7 (3)
Z8
Radiation typeX-ray, λ = 0.28988 Å
µ (mm1)?
Crystal size (mm) × ×
Data collection
Diffractometer?
Absorption correction
No. of measured, independent and
observed [I > 3σ(I)] reflections
449, 341, 223
Rint0.051
(sin θ/λ)max1)0.730
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.058, 0.081, 1.26
No. of reflections341
No. of parameters30
No. of restraints3
Δρmax, Δρmin (e Å3)0.86, 0.78

 

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