Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804008566/wm6014sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804008566/wm6014Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (In-Pd) = 0.002 Å
- R factor = 0.040
- wR factor = 0.112
- Data-to-parameter ratio = 15.0
checkCIF/PLATON results
No syntax errors found
Alert level C GOODF01_ALERT_2_C The least squares goodness of fit parameter lies outside the range 0.80 <> 2.00 Goodness of fit given = 0.795 STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.380 From the CIF: _refine_ls_abs_structure_Flack_su 0.140 PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.38 PLAT731_ALERT_1_C Bond Calc 2.948(4), Rep 2.9484(19) ...... 2.11 su-Rat PD1 -IN 1.555 7.665 PLAT731_ALERT_1_C Bond Calc 3.071(2), Rep 3.0710(8) ...... 2.50 su-Rat PD1 -CE 1.555 7.665 PLAT731_ALERT_1_C Bond Calc 3.071(2), Rep 3.0710(8) ...... 2.50 su-Rat PD1 -CE 1.555 7.666
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.05 From the CIF: _reflns_number_total 195 Count of symmetry unique reflns 118 Completeness (_total/calc) 165.25% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 77 Fraction of Friedel pairs measured 0.653 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: WinGX (Farrugia, 1999).
CePdIn | Dx = 8.715 Mg m−3 |
Mr = 361.34 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P62m | Cell parameters from 25 reflections |
Hall symbol: P -6 -2 | θ = 7.3–18.9° |
a = 7.7036 (15) Å | µ = 30.63 mm−1 |
c = 4.0190 (14) Å | T = 293 K |
V = 206.56 (9) Å3 | Prism, metallic dark grey |
Z = 3 | 0.09 × 0.03 × 0.03 mm |
F(000) = 459 |
Enraf–Nonius CAD-4 diffractometer | 171 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.077 |
Graphite monochromator | θmax = 27.1°, θmin = 3.1° |
ω scans | h = 0→9 |
Absorption correction: ψ scan (North et al., 1968) | k = −9→8 |
Tmin = 0.285, Tmax = 0.393 | l = 0→5 |
551 measured reflections | 1 standard reflections every 120 min |
195 independent reflections | intensity decay: 1% |
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)] = 0.040 | w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.112 | (Δ/σ)max < 0.001 |
S = 0.80 | Δρmax = 1.59 e Å−3 |
195 reflections | Δρmin = −1.90 e Å−3 |
13 parameters | Absolute structure: Flack (1983), 118 Friedel pairs |
0 restraints | Absolute structure parameter: 0.38 (14) |
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. andis 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 | ||
In | 0.2487 (4) | 0.0000 | 0.5000 | 0.0082 (7) | |
Ce | 0.5868 (3) | 0.0000 | 0.0000 | 0.0086 (7) | |
Pd1 | 0.3333 | 0.6667 | 0.5000 | 0.0081 (8) | |
Pd2 | 0.0000 | 0.0000 | 0.0000 | 0.0093 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
In | 0.0105 (11) | 0.0089 (15) | 0.0047 (13) | 0.0044 (7) | 0.000 | 0.000 |
Ce | 0.0104 (10) | 0.0113 (12) | 0.0045 (10) | 0.0057 (6) | 0.000 | 0.000 |
Pd1 | 0.0096 (11) | 0.0096 (11) | 0.0050 (19) | 0.0048 (6) | 0.000 | 0.000 |
Pd2 | 0.0105 (15) | 0.0105 (15) | 0.007 (3) | 0.0053 (8) | 0.000 | 0.000 |
In—Pd2 | 2.777 (2) | Ce—Inxv | 3.4267 (18) |
In—Pd2i | 2.777 (2) | Ce—Inxvi | 3.4267 (18) |
In—Pd1ii | 2.9484 (19) | Ce—Cexii | 4.0190 (14) |
In—Pd1iii | 2.9484 (19) | Pd1—Inxvii | 2.9484 (19) |
In—Cei | 3.290 (3) | Pd1—Iniii | 2.9484 (19) |
In—Ce | 3.290 (3) | Pd1—Inviii | 2.9484 (19) |
In—Iniv | 3.319 (5) | Pd1—Ceiii | 3.0710 (8) |
In—Iniii | 3.319 (5) | Pd1—Cexviii | 3.0710 (8) |
In—Cev | 3.4267 (18) | Pd1—Cexix | 3.0710 (8) |
In—Cevi | 3.4267 (18) | Pd1—Cexvii | 3.0710 (8) |
In—Cevii | 3.4267 (18) | Pd1—Ceviii | 3.0710 (8) |
In—Ceviii | 3.4267 (18) | Pd1—Cevi | 3.0710 (8) |
Ce—Pd1iii | 3.0710 (8) | Pd2—Inxx | 2.777 (2) |
Ce—Pd1ix | 3.0710 (8) | Pd2—Iniii | 2.777 (2) |
Ce—Pd1x | 3.0710 (8) | Pd2—Iniv | 2.777 (2) |
Ce—Pd1ii | 3.0710 (8) | Pd2—Inx | 2.777 (2) |
Ce—Pd2xi | 3.183 (3) | Pd2—Inxii | 2.777 (2) |
Ce—Inxii | 3.290 (3) | Pd2—Ceviii | 3.183 (3) |
Ce—Inxiii | 3.4267 (18) | Pd2—Cexxi | 3.183 (3) |
Ce—Inxiv | 3.4267 (18) | Pd2—Cev | 3.183 (3) |
Pd2—In—Pd2i | 92.73 (8) | Pd2i—In—Pd1ii | 116.941 (6) |
Pd2—In—Pd1ii | 116.941 (6) | Pd2—In—Pd1iii | 116.941 (6) |
Symmetry codes: (i) x, y, z+1; (ii) x, y−1, z; (iii) y, x, z; (iv) −x, −x+y, z; (v) y, x−1, z; (vi) −x+1, −x+y+1, z+1; (vii) y, x−1, z+1; (viii) −x+1, −x+y+1, z; (ix) x, y−1, z−1; (x) y, x, z−1; (xi) x+1, y, z; (xii) x, y, z−1; (xiii) y+1, x, z; (xiv) −x+1, −x+y, z−1; (xv) y+1, x, z−1; (xvi) −x+1, −x+y, z; (xvii) x, y+1, z; (xviii) x, y+1, z+1; (xix) y, x, z+1; (xx) −x, −x+y, z−1; (xxi) x−1, y, z. |