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
Crystal data top
Al2.5B0.5O4.5 | V = 595.7 (3) Å3 |
Mr = 144.9 | Z = 8 |
Orthorhombic, Cmc21 | F(000) = 568 |
Hall symbol: C 2c -2 | Dx = 3.229 Mg m−3 |
a = 5.5494 (15) Å | X-ray radiation, λ = 0.28988 Å |
b = 14.350 (6) Å | T = 293 K |
c = 7.481 (2) Å | × × mm |
Data collection top
449 measured reflections | θmax = 12.2°, θmin = 1.6° |
341 independent reflections | h = −7→7 |
223 reflections with I > 3σ(I) | k = −16→12 |
Rint = 0.051 | l = −8→9 |
Refinement top
Refinement on F | 3 restraints |
R[F2 > 2σ(F2)] = 0.058 | 0 constraints |
wR(F2) = 0.081 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
S = 1.26 | (Δ/σ)max = 0.046 |
341 reflections | Δρmax = 0.86 e Å−3 |
30 parameters | Δρmin = −0.78 e Å−3 |
Crystal data top
Al2.5B0.5O4.5 | V = 595.7 (3) Å3 |
Mr = 144.9 | Z = 8 |
Orthorhombic, Cmc21 | X-ray radiation, λ = 0.28988 Å |
a = 5.5494 (15) Å | T = 293 K |
b = 14.350 (6) Å | × × mm |
c = 7.481 (2) Å | |
Data collection top
449 measured reflections | 223 reflections with I > 3σ(I) |
341 independent reflections | Rint = 0.051 |
Refinement top
R[F2 > 2σ(F2)] = 0.058 | 30 parameters |
wR(F2) = 0.081 | 3 restraints |
S = 1.26 | Δρmax = 0.86 e Å−3 |
341 reflections | Δρmin = −0.78 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Al1 | 0.2510 (6) | 0.1172 (4) | 0.33664 | 0.0111 (6)* | |
Al2 | 0 | 0.2560 (5) | 0.5196 (11) | 0.0111 (6)* | |
Al3 | 0 | 0.4454 (5) | 0.5296 (13) | 0.0111 (6)* | |
Al4 | 0 | 0.3018 (6) | 0.1671 (12) | 0.0111 (6)* | |
B1 | 0 | 0.0167 (19) | 0.060 (2) | 0.012 (5)* | |
O1 | 0 | 0.3241 (14) | 0.710 (2) | 0.0161 (11)* | |
O2 | 0.2528 (15) | 0.1877 (9) | 0.5402 (17) | 0.0161 (11)* | |
O3 | 0 | 0.4528 (12) | 0.909 (2) | 0.0161 (11)* | |
O4 | 0 | 0.0424 (12) | 0.417 (2) | 0.0161 (11)* | |
O5 | 0 | 0.3544 (15) | 0.369 (2) | 0.0161 (11)* | |
O6 | 0 | 0.1925 (15) | 0.262 (2) | 0.0161 (11)* | |
O7 | 0.2141 (14) | 0.0472 (9) | 0.1317 (18) | 0.0161 (11)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
? | ? | ? | ? | ? | ? | ? |
Bond lengths (Å) top
Al1—Al1i | 2.785 (5) | Al2—Al4v | 3.099 (6) |
Al1—Al1ii | 2.764 (5) | Al2—O1 | 1.73 (2) |
Al1—Al2 | 2.789 (8) | Al2—O2 | 1.718 (11) |
Al1—Al2iii | 3.294 (8) | Al2—O2i | 1.718 (11) |
Al1—Al3iv | 3.174 (9) | Al2—O5 | 1.81 (2) |
Al1—Al3iii | 2.827 (8) | Al3—Al4 | 3.405 (13) |
Al1—Al4 | 3.251 (9) | Al3—O3vii | 1.72 (2) |
Al1—Al4v | 3.061 (9) | Al3—O5 | 1.77 (2) |
Al1—O1iii | 1.874 (13) | Al3—O7v | 1.764 (10) |
Al1—O2 | 1.828 (14) | Al3—O7viii | 1.764 (10) |
Al1—O3iii | 1.792 (12) | Al4—O2iii | 1.675 (11) |
Al1—O4 | 1.858 (12) | Al4—O2ix | 1.675 (11) |
Al1—O6 | 1.848 (14) | Al4—O5 | 1.689 (19) |
Al1—O7 | 1.844 (14) | Al4—O6 | 1.72 (2) |
Al2—Al3 | 2.719 (11) | B1—O4x | 1.36 (3) |
Al2—Al4 | 2.718 (12) | B1—O7 | 1.376 (15) |
Al2—Al4vi | 3.099 (6) | B1—O7i | 1.376 (15) |
Symmetry codes: (i) −x, y, z; (ii) −x+1, y, z; (iii) −x+1/2, −y+1/2, z−1/2; (iv) x+1/2, y−1/2, z; (v) −x+1/2, −y+1/2, z+1/2; (vi) −x−1/2, −y+1/2, z+1/2; (vii) −x, −y+1, z−1/2; (viii) x−1/2, −y+1/2, z+1/2; (ix) x−1/2, −y+1/2, z−1/2; (x) −x, −y, z−1/2. |
Experimental details
Crystal data |
Chemical formula | Al2.5B0.5O4.5 |
Mr | 144.9 |
Crystal system, space group | Orthorhombic, Cmc21 |
Temperature (K) | 293 |
a, b, c (Å) | 5.5494 (15), 14.350 (6), 7.481 (2) |
V (Å3) | 595.7 (3) |
Z | 8 |
Radiation type | X-ray, λ = 0.28988 Å |
µ (mm−1) | ? |
Crystal size (mm) | × × |
|
Data collection |
Diffractometer | ? |
Absorption correction | – |
No. of measured, independent and observed [I > 3σ(I)] reflections | 449, 341, 223 |
Rint | 0.051 |
(sin θ/λ)max (Å−1) | 0.730 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.058, 0.081, 1.26 |
No. of reflections | 341 |
No. of parameters | 30 |
No. of restraints | 3 |
Δρmax, Δρmin (e Å−3) | 0.86, −0.78 |