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Single crystals of uranium palladium dianti­monide, UPd0.603 (6)Sb2, were grown from an Sb flux. The title compound crystallizes in space group P4/nmm, adopting the ZrCuSi2 structure type, but with a partial occupancy of the Pd site. All atoms are located on special positions with site symmetries \overline{4}m2 for Pd and one Sb atom, and 4mm for U and the other Sb atom.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806005666/wm2002sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806005666/wm2002Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma]() = 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

Computing details top

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.

uranium palladium diantimonide top
Crystal data top
UPd0.60Sb2Dx = 10.279 Mg m3
Mr = 545.37Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/nmmCell parameters from 1893 reflections
Hall symbol: -P 4a 2aθ = 2.2–27.3°
a = 4.3459 (7) ŵ = 63.74 mm1
c = 9.330 (3) ÅT = 120 K
V = 176.21 (7) Å3Bar, grey
Z = 20.08 × 0.05 × 0.05 mm
F(000) = 443
Data collection top
Bruker SMART APEX CCD
diffractometer
150 independent reflections
Radiation source: fine-focus sealed tube149 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
Detector resolution: 8.3 pixels mm-1θmax = 27.3°, θmin = 2.2°
ω scansh = 55
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
k = 55
Tmin = 0.043, Tmax = 0.057l = 1211
1893 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary 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 = 1.16Δρmax = 1.58 e Å3
150 reflectionsΔρmin = 1.79 e Å3
13 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0067 (8)
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
U0.25000.25000.24033 (6)0.0106 (3)
Sb10.75000.25000.50000.0105 (3)
Sb20.25000.25000.83816 (13)0.0148 (3)
Pd0.75000.25000.00000.0109 (7)0.603 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
U0.0087 (3)0.0087 (3)0.0143 (4)0.0000.0000.000
Sb10.0095 (4)0.0095 (4)0.0127 (6)0.0000.0000.000
Sb20.0106 (4)0.0106 (4)0.0232 (7)0.0000.0000.000
Pd0.0105 (8)0.0105 (8)0.0116 (12)0.0000.0000.000
Geometric parameters (Å, º) top
U—Pdi3.1224 (7)Sb2—Pdv2.6460 (8)
U—Pdii3.1224 (7)Sb2—Pdxi2.6460 (8)
U—Pdiii3.1224 (7)Sb2—Pdvii2.6460 (8)
U—Pd3.1224 (7)Sb2—Pdxii2.6460 (8)
U—Sb2iv3.1591 (6)Sb2—Uiv3.1591 (6)
U—Sb2v3.1591 (6)Sb2—Uv3.1591 (6)
U—Sb2vi3.1591 (6)Sb2—Uvii3.1591 (6)
U—Sb2vii3.1591 (6)Sb2—Uvi3.1591 (6)
U—Sb13.2543 (7)Pd—Sb2v2.6460 (8)
U—Sb1v3.2543 (7)Pd—Sb2xiii2.6460 (8)
U—Sb1ii3.2543 (7)Pd—Sb2vii2.6460 (8)
U—Sb1vii3.2543 (7)Pd—Sb2xiv2.6460 (8)
Sb1—Sb1viii3.0730 (5)Pd—Pdxv3.0730 (5)
Sb1—Sb1vii3.0730 (5)Pd—Pdi3.0730 (5)
Sb1—Sb1v3.0730 (5)Pd—Pdiii3.0730 (5)
Sb1—Sb1ix3.0730 (5)Pd—Pdxvi3.0730 (5)
Sb1—Uv3.2543 (7)Pd—Ux3.1224 (7)
Sb1—Uvii3.2543 (7)Pd—Ui3.1224 (7)
Sb1—Ux3.2543 (7)Pd—Uiii3.1224 (7)
Pdi—U—Pdii58.957 (14)Pdv—Sb2—Pdxi71.00 (2)
Pdi—U—Pdiii88.20 (2)Pdv—Sb2—Pdvii110.41 (5)
Pdii—U—Pdiii58.957 (14)Pdxi—Sb2—Pdvii71.00 (2)
Pdi—U—Pd58.957 (14)Pdv—Sb2—Pdxii71.00 (2)
Pdii—U—Pd88.20 (2)Pdxi—Sb2—Pdxii110.41 (5)
Pdiii—U—Pd58.957 (14)Pdvii—Sb2—Pdxii71.00 (2)
Pdi—U—Sb2iv49.822 (17)Pdv—Sb2—Uiv134.199 (19)
Pdii—U—Sb2iv49.822 (17)Pdxi—Sb2—Uiv134.199 (19)
Pdiii—U—Sb2iv108.19 (3)Pdvii—Sb2—Uiv64.368 (12)
Pd—U—Sb2iv108.19 (3)Pdxii—Sb2—Uiv64.368 (12)
Pdi—U—Sb2v108.19 (3)Pdv—Sb2—Uv64.368 (12)
Pdii—U—Sb2v108.19 (3)Pdxi—Sb2—Uv64.368 (12)
Pdiii—U—Sb2v49.822 (17)Pdvii—Sb2—Uv134.199 (19)
Pd—U—Sb2v49.822 (17)Pdxii—Sb2—Uv134.199 (19)
Sb2iv—U—Sb2v153.19 (5)Uiv—Sb2—Uv153.19 (5)
Pdi—U—Sb2vi108.19 (2)Pdv—Sb2—Uvii134.199 (19)
Pdii—U—Sb2vi49.822 (17)Pdxi—Sb2—Uvii64.368 (12)
Pdiii—U—Sb2vi49.822 (17)Pdvii—Sb2—Uvii64.368 (12)
Pd—U—Sb2vi108.19 (3)Pdxii—Sb2—Uvii134.199 (19)
Sb2iv—U—Sb2vi86.919 (11)Uiv—Sb2—Uvii86.919 (11)
Sb2v—U—Sb2vi86.919 (11)Uv—Sb2—Uvii86.919 (11)
Pdi—U—Sb2vii49.822 (17)Pdv—Sb2—Uvi64.368 (12)
Pdii—U—Sb2vii108.19 (2)Pdxi—Sb2—Uvi134.199 (19)
Pdiii—U—Sb2vii108.19 (3)Pdvii—Sb2—Uvi134.199 (19)
Pd—U—Sb2vii49.822 (17)Pdxii—Sb2—Uvi64.368 (12)
Sb2iv—U—Sb2vii86.919 (11)Uiv—Sb2—Uvi86.919 (11)
Sb2v—U—Sb2vii86.919 (11)Uvii—Sb2—Uvi153.19 (5)
Sb2vi—U—Sb2vii153.19 (5)Sb2v—Pd—Sb2xiii109.00 (2)
Pdi—U—Sb1122.315 (12)Sb2v—Pd—Sb2vii110.41 (5)
Pdii—U—Sb1177.789 (14)Sb2xiii—Pd—Sb2vii109.00 (2)
Pdiii—U—Sb1122.315 (11)Sb2v—Pd—Sb2xiv109.00 (2)
Pd—U—Sb194.01 (2)Sb2xiii—Pd—Sb2xiv110.41 (5)
Sb2iv—U—Sb1129.19 (2)Sb2vii—Pd—Sb2xiv109.00 (2)
Sb2v—U—Sb173.34 (2)Sb2v—Pd—Pdxv54.501 (11)
Sb2vi—U—Sb1129.19 (2)Sb2xiii—Pd—Pdxv125.499 (11)
Sb2vii—U—Sb173.34 (2)Sb2vii—Pd—Pdxv125.499 (11)
Pdi—U—Sb1v177.789 (14)Sb2xiv—Pd—Pdxv54.501 (11)
Pdii—U—Sb1v122.315 (12)Sb2v—Pd—Pdi125.499 (11)
Pdiii—U—Sb1v94.01 (2)Sb2xiii—Pd—Pdi54.501 (11)
Pd—U—Sb1v122.315 (11)Sb2vii—Pd—Pdi54.501 (11)
Sb2iv—U—Sb1v129.19 (2)Sb2xiv—Pd—Pdi125.499 (11)
Sb2v—U—Sb1v73.34 (2)Pdxv—Pd—Pdi180.0
Sb2vi—U—Sb1v73.34 (2)Sb2v—Pd—Pdiii54.501 (11)
Sb2vii—U—Sb1v129.19 (2)Sb2xiii—Pd—Pdiii54.501 (11)
Sb1—U—Sb1v56.347 (14)Sb2vii—Pd—Pdiii125.499 (11)
Pdi—U—Sb1ii122.315 (11)Sb2xiv—Pd—Pdiii125.499 (11)
Pdii—U—Sb1ii94.01 (2)Pdxv—Pd—Pdiii90.0
Pdiii—U—Sb1ii122.315 (11)Pdi—Pd—Pdiii90.0
Pd—U—Sb1ii177.789 (14)Sb2v—Pd—Pdxvi125.499 (11)
Sb2iv—U—Sb1ii73.34 (2)Sb2xiii—Pd—Pdxvi125.499 (11)
Sb2v—U—Sb1ii129.19 (2)Sb2vii—Pd—Pdxvi54.501 (11)
Sb2vi—U—Sb1ii73.34 (2)Sb2xiv—Pd—Pdxvi54.501 (11)
Sb2vii—U—Sb1ii129.19 (2)Pdxv—Pd—Pdxvi90.0
Sb1—U—Sb1ii83.78 (2)Pdi—Pd—Pdxvi90.0
Sb1v—U—Sb1ii56.347 (14)Pdiii—Pd—Pdxvi180.0
Pdi—U—Sb1vii94.01 (2)Sb2v—Pd—U65.810 (17)
Pdii—U—Sb1vii122.315 (11)Sb2xiii—Pd—U80.69 (3)
Pdiii—U—Sb1vii177.789 (14)Sb2vii—Pd—U65.810 (17)
Pd—U—Sb1vii122.315 (11)Sb2xiv—Pd—U168.89 (2)
Sb2iv—U—Sb1vii73.34 (2)Pdxv—Pd—U119.479 (7)
Sb2v—U—Sb1vii129.19 (2)Pdi—Pd—U60.521 (7)
Sb2vi—U—Sb1vii129.19 (2)Pdiii—Pd—U60.521 (7)
Sb2vii—U—Sb1vii73.34 (2)Pdxvi—Pd—U119.479 (8)
Sb1—U—Sb1vii56.347 (14)Sb2v—Pd—Ux65.810 (17)
Sb1v—U—Sb1vii83.78 (2)Sb2xiii—Pd—Ux168.89 (2)
Sb1ii—U—Sb1vii56.347 (14)Sb2vii—Pd—Ux65.810 (17)
Sb1viii—Sb1—Sb1vii180.0Sb2xiv—Pd—Ux80.69 (3)
Sb1viii—Sb1—Sb1v90.0Pdxv—Pd—Ux60.521 (7)
Sb1vii—Sb1—Sb1v90.0Pdi—Pd—Ux119.479 (7)
Sb1viii—Sb1—Sb1ix90.0Pdiii—Pd—Ux119.479 (7)
Sb1vii—Sb1—Sb1ix90.0Pdxvi—Pd—Ux60.521 (7)
Sb1v—Sb1—Sb1ix180.0U—Pd—Ux88.20 (2)
Sb1viii—Sb1—Uv61.827 (7)Sb2v—Pd—Ui168.89 (2)
Sb1vii—Sb1—Uv118.173 (7)Sb2xiii—Pd—Ui65.810 (17)
Sb1v—Sb1—Uv61.827 (7)Sb2vii—Pd—Ui80.69 (3)
Sb1ix—Sb1—Uv118.173 (7)Sb2xiv—Pd—Ui65.810 (17)
Sb1viii—Sb1—Uvii118.173 (7)Pdxv—Pd—Ui119.479 (7)
Sb1vii—Sb1—Uvii61.827 (7)Pdi—Pd—Ui60.521 (7)
Sb1v—Sb1—Uvii118.173 (7)Pdiii—Pd—Ui119.479 (7)
Sb1ix—Sb1—Uvii61.827 (7)Pdxvi—Pd—Ui60.521 (7)
Uv—Sb1—Uvii83.78 (2)U—Pd—Ui121.043 (15)
Sb1viii—Sb1—Ux61.827 (7)Ux—Pd—Ui121.043 (14)
Sb1vii—Sb1—Ux118.173 (7)Sb2v—Pd—Uiii80.69 (3)
Sb1v—Sb1—Ux118.173 (7)Sb2xiii—Pd—Uiii65.810 (18)
Sb1ix—Sb1—Ux61.827 (7)Sb2vii—Pd—Uiii168.89 (2)
Uv—Sb1—Ux123.653 (14)Sb2xiv—Pd—Uiii65.810 (18)
Uvii—Sb1—Ux123.653 (14)Pdxv—Pd—Uiii60.521 (7)
Sb1viii—Sb1—U118.173 (7)Pdi—Pd—Uiii119.479 (7)
Sb1vii—Sb1—U61.827 (7)Pdiii—Pd—Uiii60.521 (7)
Sb1v—Sb1—U61.827 (7)Pdxvi—Pd—Uiii119.479 (7)
Sb1ix—Sb1—U118.173 (7)U—Pd—Uiii121.043 (15)
Uv—Sb1—U123.653 (14)Ux—Pd—Uiii121.043 (14)
Uvii—Sb1—U123.653 (14)Ui—Pd—Uiii88.20 (2)
Ux—Sb1—U83.78 (2)
Symmetry codes: (i) x+1, y, z; (ii) x1, 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) x1, y, z+1; (xiii) x, y, z1; (xiv) x+1, y, z1; (xv) x+2, y+1, z; (xvi) x+2, y, z.
 

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