Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806005666/wm2002sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806005666/wm2002Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean () = 0.000 Å
- Disorder in main residue
- R factor = 0.020
- wR factor = 0.047
- Data-to-parameter ratio = 11.5
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT301_ALERT_3_B Main Residue Disorder ......................... 32.00 Perc.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ?
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: SHELXTL.
UPd0.60Sb2 | Dx = 10.279 Mg m−3 |
Mr = 545.37 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, P4/nmm | Cell parameters from 1893 reflections |
Hall symbol: -P 4a 2a | θ = 2.2–27.3° |
a = 4.3459 (7) Å | µ = 63.74 mm−1 |
c = 9.330 (3) Å | T = 120 K |
V = 176.21 (7) Å3 | Bar, grey |
Z = 2 | 0.08 × 0.05 × 0.05 mm |
F(000) = 443 |
Bruker SMART APEX CCD diffractometer | 150 independent reflections |
Radiation source: fine-focus sealed tube | 149 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
Detector resolution: 8.3 pixels mm-1 | θmax = 27.3°, θmin = 2.2° |
ω scans | h = −5→5 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | k = −5→5 |
Tmin = 0.043, Tmax = 0.057 | l = −12→11 |
1893 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.020 | w = 1/[σ2(Fo2) + (0.0265P)2 + 0.8733P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.047 | (Δ/σ)max < 0.001 |
S = 1.16 | Δρmax = 1.58 e Å−3 |
150 reflections | Δρmin = −1.79 e Å−3 |
13 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0067 (8) |
Experimental. Data collection is performed with four batch runs at φ = 0.00 ° (450 frames), at φ = 90.00 ° (450 frames), at φ = 180.00 ° (450 frames), and at φ = 270.00 (450 frames). Frame width = 0.40 \& in ω. Data are merged, corrected for decay, and treated with multi-scan absorption corrections. |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
U | 0.2500 | 0.2500 | 0.24033 (6) | 0.0106 (3) | |
Sb1 | 0.7500 | 0.2500 | 0.5000 | 0.0105 (3) | |
Sb2 | 0.2500 | 0.2500 | 0.83816 (13) | 0.0148 (3) | |
Pd | 0.7500 | 0.2500 | 0.0000 | 0.0109 (7) | 0.603 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
U | 0.0087 (3) | 0.0087 (3) | 0.0143 (4) | 0.000 | 0.000 | 0.000 |
Sb1 | 0.0095 (4) | 0.0095 (4) | 0.0127 (6) | 0.000 | 0.000 | 0.000 |
Sb2 | 0.0106 (4) | 0.0106 (4) | 0.0232 (7) | 0.000 | 0.000 | 0.000 |
Pd | 0.0105 (8) | 0.0105 (8) | 0.0116 (12) | 0.000 | 0.000 | 0.000 |
U—Pdi | 3.1224 (7) | Sb2—Pdv | 2.6460 (8) |
U—Pdii | 3.1224 (7) | Sb2—Pdxi | 2.6460 (8) |
U—Pdiii | 3.1224 (7) | Sb2—Pdvii | 2.6460 (8) |
U—Pd | 3.1224 (7) | Sb2—Pdxii | 2.6460 (8) |
U—Sb2iv | 3.1591 (6) | Sb2—Uiv | 3.1591 (6) |
U—Sb2v | 3.1591 (6) | Sb2—Uv | 3.1591 (6) |
U—Sb2vi | 3.1591 (6) | Sb2—Uvii | 3.1591 (6) |
U—Sb2vii | 3.1591 (6) | Sb2—Uvi | 3.1591 (6) |
U—Sb1 | 3.2543 (7) | Pd—Sb2v | 2.6460 (8) |
U—Sb1v | 3.2543 (7) | Pd—Sb2xiii | 2.6460 (8) |
U—Sb1ii | 3.2543 (7) | Pd—Sb2vii | 2.6460 (8) |
U—Sb1vii | 3.2543 (7) | Pd—Sb2xiv | 2.6460 (8) |
Sb1—Sb1viii | 3.0730 (5) | Pd—Pdxv | 3.0730 (5) |
Sb1—Sb1vii | 3.0730 (5) | Pd—Pdi | 3.0730 (5) |
Sb1—Sb1v | 3.0730 (5) | Pd—Pdiii | 3.0730 (5) |
Sb1—Sb1ix | 3.0730 (5) | Pd—Pdxvi | 3.0730 (5) |
Sb1—Uv | 3.2543 (7) | Pd—Ux | 3.1224 (7) |
Sb1—Uvii | 3.2543 (7) | Pd—Ui | 3.1224 (7) |
Sb1—Ux | 3.2543 (7) | Pd—Uiii | 3.1224 (7) |
Pdi—U—Pdii | 58.957 (14) | Pdv—Sb2—Pdxi | 71.00 (2) |
Pdi—U—Pdiii | 88.20 (2) | Pdv—Sb2—Pdvii | 110.41 (5) |
Pdii—U—Pdiii | 58.957 (14) | Pdxi—Sb2—Pdvii | 71.00 (2) |
Pdi—U—Pd | 58.957 (14) | Pdv—Sb2—Pdxii | 71.00 (2) |
Pdii—U—Pd | 88.20 (2) | Pdxi—Sb2—Pdxii | 110.41 (5) |
Pdiii—U—Pd | 58.957 (14) | Pdvii—Sb2—Pdxii | 71.00 (2) |
Pdi—U—Sb2iv | 49.822 (17) | Pdv—Sb2—Uiv | 134.199 (19) |
Pdii—U—Sb2iv | 49.822 (17) | Pdxi—Sb2—Uiv | 134.199 (19) |
Pdiii—U—Sb2iv | 108.19 (3) | Pdvii—Sb2—Uiv | 64.368 (12) |
Pd—U—Sb2iv | 108.19 (3) | Pdxii—Sb2—Uiv | 64.368 (12) |
Pdi—U—Sb2v | 108.19 (3) | Pdv—Sb2—Uv | 64.368 (12) |
Pdii—U—Sb2v | 108.19 (3) | Pdxi—Sb2—Uv | 64.368 (12) |
Pdiii—U—Sb2v | 49.822 (17) | Pdvii—Sb2—Uv | 134.199 (19) |
Pd—U—Sb2v | 49.822 (17) | Pdxii—Sb2—Uv | 134.199 (19) |
Sb2iv—U—Sb2v | 153.19 (5) | Uiv—Sb2—Uv | 153.19 (5) |
Pdi—U—Sb2vi | 108.19 (2) | Pdv—Sb2—Uvii | 134.199 (19) |
Pdii—U—Sb2vi | 49.822 (17) | Pdxi—Sb2—Uvii | 64.368 (12) |
Pdiii—U—Sb2vi | 49.822 (17) | Pdvii—Sb2—Uvii | 64.368 (12) |
Pd—U—Sb2vi | 108.19 (3) | Pdxii—Sb2—Uvii | 134.199 (19) |
Sb2iv—U—Sb2vi | 86.919 (11) | Uiv—Sb2—Uvii | 86.919 (11) |
Sb2v—U—Sb2vi | 86.919 (11) | Uv—Sb2—Uvii | 86.919 (11) |
Pdi—U—Sb2vii | 49.822 (17) | Pdv—Sb2—Uvi | 64.368 (12) |
Pdii—U—Sb2vii | 108.19 (2) | Pdxi—Sb2—Uvi | 134.199 (19) |
Pdiii—U—Sb2vii | 108.19 (3) | Pdvii—Sb2—Uvi | 134.199 (19) |
Pd—U—Sb2vii | 49.822 (17) | Pdxii—Sb2—Uvi | 64.368 (12) |
Sb2iv—U—Sb2vii | 86.919 (11) | Uiv—Sb2—Uvi | 86.919 (11) |
Sb2v—U—Sb2vii | 86.919 (11) | Uvii—Sb2—Uvi | 153.19 (5) |
Sb2vi—U—Sb2vii | 153.19 (5) | Sb2v—Pd—Sb2xiii | 109.00 (2) |
Pdi—U—Sb1 | 122.315 (12) | Sb2v—Pd—Sb2vii | 110.41 (5) |
Pdii—U—Sb1 | 177.789 (14) | Sb2xiii—Pd—Sb2vii | 109.00 (2) |
Pdiii—U—Sb1 | 122.315 (11) | Sb2v—Pd—Sb2xiv | 109.00 (2) |
Pd—U—Sb1 | 94.01 (2) | Sb2xiii—Pd—Sb2xiv | 110.41 (5) |
Sb2iv—U—Sb1 | 129.19 (2) | Sb2vii—Pd—Sb2xiv | 109.00 (2) |
Sb2v—U—Sb1 | 73.34 (2) | Sb2v—Pd—Pdxv | 54.501 (11) |
Sb2vi—U—Sb1 | 129.19 (2) | Sb2xiii—Pd—Pdxv | 125.499 (11) |
Sb2vii—U—Sb1 | 73.34 (2) | Sb2vii—Pd—Pdxv | 125.499 (11) |
Pdi—U—Sb1v | 177.789 (14) | Sb2xiv—Pd—Pdxv | 54.501 (11) |
Pdii—U—Sb1v | 122.315 (12) | Sb2v—Pd—Pdi | 125.499 (11) |
Pdiii—U—Sb1v | 94.01 (2) | Sb2xiii—Pd—Pdi | 54.501 (11) |
Pd—U—Sb1v | 122.315 (11) | Sb2vii—Pd—Pdi | 54.501 (11) |
Sb2iv—U—Sb1v | 129.19 (2) | Sb2xiv—Pd—Pdi | 125.499 (11) |
Sb2v—U—Sb1v | 73.34 (2) | Pdxv—Pd—Pdi | 180.0 |
Sb2vi—U—Sb1v | 73.34 (2) | Sb2v—Pd—Pdiii | 54.501 (11) |
Sb2vii—U—Sb1v | 129.19 (2) | Sb2xiii—Pd—Pdiii | 54.501 (11) |
Sb1—U—Sb1v | 56.347 (14) | Sb2vii—Pd—Pdiii | 125.499 (11) |
Pdi—U—Sb1ii | 122.315 (11) | Sb2xiv—Pd—Pdiii | 125.499 (11) |
Pdii—U—Sb1ii | 94.01 (2) | Pdxv—Pd—Pdiii | 90.0 |
Pdiii—U—Sb1ii | 122.315 (11) | Pdi—Pd—Pdiii | 90.0 |
Pd—U—Sb1ii | 177.789 (14) | Sb2v—Pd—Pdxvi | 125.499 (11) |
Sb2iv—U—Sb1ii | 73.34 (2) | Sb2xiii—Pd—Pdxvi | 125.499 (11) |
Sb2v—U—Sb1ii | 129.19 (2) | Sb2vii—Pd—Pdxvi | 54.501 (11) |
Sb2vi—U—Sb1ii | 73.34 (2) | Sb2xiv—Pd—Pdxvi | 54.501 (11) |
Sb2vii—U—Sb1ii | 129.19 (2) | Pdxv—Pd—Pdxvi | 90.0 |
Sb1—U—Sb1ii | 83.78 (2) | Pdi—Pd—Pdxvi | 90.0 |
Sb1v—U—Sb1ii | 56.347 (14) | Pdiii—Pd—Pdxvi | 180.0 |
Pdi—U—Sb1vii | 94.01 (2) | Sb2v—Pd—U | 65.810 (17) |
Pdii—U—Sb1vii | 122.315 (11) | Sb2xiii—Pd—U | 80.69 (3) |
Pdiii—U—Sb1vii | 177.789 (14) | Sb2vii—Pd—U | 65.810 (17) |
Pd—U—Sb1vii | 122.315 (11) | Sb2xiv—Pd—U | 168.89 (2) |
Sb2iv—U—Sb1vii | 73.34 (2) | Pdxv—Pd—U | 119.479 (7) |
Sb2v—U—Sb1vii | 129.19 (2) | Pdi—Pd—U | 60.521 (7) |
Sb2vi—U—Sb1vii | 129.19 (2) | Pdiii—Pd—U | 60.521 (7) |
Sb2vii—U—Sb1vii | 73.34 (2) | Pdxvi—Pd—U | 119.479 (8) |
Sb1—U—Sb1vii | 56.347 (14) | Sb2v—Pd—Ux | 65.810 (17) |
Sb1v—U—Sb1vii | 83.78 (2) | Sb2xiii—Pd—Ux | 168.89 (2) |
Sb1ii—U—Sb1vii | 56.347 (14) | Sb2vii—Pd—Ux | 65.810 (17) |
Sb1viii—Sb1—Sb1vii | 180.0 | Sb2xiv—Pd—Ux | 80.69 (3) |
Sb1viii—Sb1—Sb1v | 90.0 | Pdxv—Pd—Ux | 60.521 (7) |
Sb1vii—Sb1—Sb1v | 90.0 | Pdi—Pd—Ux | 119.479 (7) |
Sb1viii—Sb1—Sb1ix | 90.0 | Pdiii—Pd—Ux | 119.479 (7) |
Sb1vii—Sb1—Sb1ix | 90.0 | Pdxvi—Pd—Ux | 60.521 (7) |
Sb1v—Sb1—Sb1ix | 180.0 | U—Pd—Ux | 88.20 (2) |
Sb1viii—Sb1—Uv | 61.827 (7) | Sb2v—Pd—Ui | 168.89 (2) |
Sb1vii—Sb1—Uv | 118.173 (7) | Sb2xiii—Pd—Ui | 65.810 (17) |
Sb1v—Sb1—Uv | 61.827 (7) | Sb2vii—Pd—Ui | 80.69 (3) |
Sb1ix—Sb1—Uv | 118.173 (7) | Sb2xiv—Pd—Ui | 65.810 (17) |
Sb1viii—Sb1—Uvii | 118.173 (7) | Pdxv—Pd—Ui | 119.479 (7) |
Sb1vii—Sb1—Uvii | 61.827 (7) | Pdi—Pd—Ui | 60.521 (7) |
Sb1v—Sb1—Uvii | 118.173 (7) | Pdiii—Pd—Ui | 119.479 (7) |
Sb1ix—Sb1—Uvii | 61.827 (7) | Pdxvi—Pd—Ui | 60.521 (7) |
Uv—Sb1—Uvii | 83.78 (2) | U—Pd—Ui | 121.043 (15) |
Sb1viii—Sb1—Ux | 61.827 (7) | Ux—Pd—Ui | 121.043 (14) |
Sb1vii—Sb1—Ux | 118.173 (7) | Sb2v—Pd—Uiii | 80.69 (3) |
Sb1v—Sb1—Ux | 118.173 (7) | Sb2xiii—Pd—Uiii | 65.810 (18) |
Sb1ix—Sb1—Ux | 61.827 (7) | Sb2vii—Pd—Uiii | 168.89 (2) |
Uv—Sb1—Ux | 123.653 (14) | Sb2xiv—Pd—Uiii | 65.810 (18) |
Uvii—Sb1—Ux | 123.653 (14) | Pdxv—Pd—Uiii | 60.521 (7) |
Sb1viii—Sb1—U | 118.173 (7) | Pdi—Pd—Uiii | 119.479 (7) |
Sb1vii—Sb1—U | 61.827 (7) | Pdiii—Pd—Uiii | 60.521 (7) |
Sb1v—Sb1—U | 61.827 (7) | Pdxvi—Pd—Uiii | 119.479 (7) |
Sb1ix—Sb1—U | 118.173 (7) | U—Pd—Uiii | 121.043 (15) |
Uv—Sb1—U | 123.653 (14) | Ux—Pd—Uiii | 121.043 (14) |
Uvii—Sb1—U | 123.653 (14) | Ui—Pd—Uiii | 88.20 (2) |
Ux—Sb1—U | 83.78 (2) |
Symmetry codes: (i) −x+1, −y, −z; (ii) x−1, y, z; (iii) −x+1, −y+1, −z; (iv) −x, −y, −z+1; (v) −x+1, −y+1, −z+1; (vi) −x, −y+1, −z+1; (vii) −x+1, −y, −z+1; (viii) −x+2, −y+1, −z+1; (ix) −x+2, −y, −z+1; (x) x+1, y, z; (xi) x, y, z+1; (xii) x−1, y, z+1; (xiii) x, y, z−1; (xiv) x+1, y, z−1; (xv) −x+2, −y+1, −z; (xvi) −x+2, −y, −z. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register