Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805012857/wm6064sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805012857/wm6064Isup2.hkl |
Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996); software used to prepare material for publication: SHELXL97.
PrI3·9H20 | F(000) = 616 |
Mr = 683.75 | Dx = 2.700 Mg m−3 |
Orthorhombic, Pmmn | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ab 2a | Cell parameters from 2000 reflections |
a = 11.720 (2) Å | θ = 1.9–27.7° |
b = 8.0163 (15) Å | µ = 8.42 mm−1 |
c = 8.952 (2) Å | T = 298 K |
V = 841.1 (3) Å3 | Irregular, pale yellow to green |
Z = 2 | 0.30 × 0.10 × 0.05 mm |
Stoe IPDS-I diffractometer | 1016 independent reflections |
Radiation source: fine-focus sealed tube | 870 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.072 |
Detector resolution: not measured pixels mm-1 | θmax = 27.7°, θmin = 1.9° |
φ scans | h = −15→15 |
Absorption correction: numerical X-RED (Stoe & Cie, 2002) and X-SHAPE (Stoe & Cie, 1999) | k = −9→9 |
Tmin = 0.151, Tmax = 0.607 | l = −11→11 |
8456 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | H-atom parameters not defined |
R[F2 > 2σ(F2)] = 0.050 | w = 1/[σ2(Fo2) + (0.0732P)2 + 3.5369P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.136 | (Δ/σ)max < 0.001 |
S = 1.09 | Δρmax = 1.12 e Å−3 |
1016 reflections | Δρmin = −1.62 e Å−3 |
41 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.030 (3) |
Primary atom site location: structure-invariant direct methods |
Experimental. A suitable single-crystal was carefully selected under a polarizing microscope and mounted in a glass capillary. The scattering intensities were collected with an imaging plate diffractometer (Stoe IPDS-I) equipped with a fine focus sealed tube X-ray source (Mo Kα, λ = 0.71073 Å) operating at 50 kV and 30 mA. Intensity data for [Pr(OH2)9]I3 were collected at 298 K by φ scans in 100 frames (0 < φ < 200° exposure time of 5 min) in the 2Θ range 5–56 °·Structure solution and refinement were carried out using the program SHELXL97 (Sheldrick, 1997). A numerical absorption correction (X-RED (Stoe & Cie, 2001) was applied after optimization of the crystal shape (X-SHAPE (Stoe & Cie, 1999)). The final difference maps were free of any chemically significant features. The refinement was based on F2 for ALL reflections. |
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-factorsbased 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 | ||
Pr | 0.2500 | 0.2500 | 0.33185 (8) | 0.0438 (3) | |
I1 | 0.00245 (6) | 0.7500 | 0.17176 (8) | 0.0658 (4) | |
I2 | 0.2500 | 0.7500 | −0.29036 (15) | 0.0647 (4) | |
O1 | 0.0570 (6) | 0.2500 | 0.2053 (9) | 0.069 (2) | |
O2 | 0.2500 | 0.0422 (12) | 0.1196 (10) | 0.074 (2) | |
O3 | 0.3788 (4) | 0.4737 (8) | 0.4354 (6) | 0.0663 (16) | |
O4 | 0.2500 | 0.2500 | 0.6158 (12) | 0.064 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pr | 0.0313 (4) | 0.0669 (6) | 0.0333 (4) | 0.000 | 0.000 | 0.000 |
I1 | 0.0653 (6) | 0.0916 (8) | 0.0405 (5) | 0.000 | −0.0033 (3) | 0.000 |
I2 | 0.0541 (6) | 0.0834 (9) | 0.0567 (7) | 0.000 | 0.000 | 0.000 |
O1 | 0.054 (4) | 0.104 (7) | 0.048 (4) | 0.000 | −0.016 (3) | 0.000 |
O2 | 0.061 (4) | 0.096 (7) | 0.064 (5) | 0.000 | 0.000 | −0.017 (5) |
O3 | 0.053 (3) | 0.088 (5) | 0.057 (3) | −0.016 (2) | 0.002 (2) | −0.004 (3) |
O4 | 0.050 (5) | 0.101 (9) | 0.041 (5) | 0.000 | 0.000 | 0.000 |
Pr—O3 | 2.520 (6) | Pr—O2ii | 2.527 (9) |
Pr—O3i | 2.520 (6) | Pr—O1 | 2.530 (7) |
Pr—O3ii | 2.520 (6) | Pr—O1ii | 2.530 (7) |
Pr—O3iii | 2.520 (6) | Pr—O4 | 2.542 (11) |
Pr—O2 | 2.527 (9) | ||
O3—Pr—O3i | 73.6 (3) | O3iii—Pr—O1 | 134.43 (14) |
O3—Pr—O3ii | 136.9 (3) | O2—Pr—O1 | 70.32 (15) |
O3i—Pr—O3ii | 90.7 (3) | O2ii—Pr—O1 | 70.32 (15) |
O3—Pr—O3iii | 90.7 (3) | O3—Pr—O1ii | 68.24 (17) |
O3i—Pr—O3iii | 136.9 (3) | O3i—Pr—O1ii | 134.43 (14) |
O3ii—Pr—O3iii | 73.6 (3) | O3ii—Pr—O1ii | 134.43 (14) |
O3—Pr—O2 | 138.20 (16) | O3iii—Pr—O1ii | 68.24 (17) |
O3i—Pr—O2 | 138.20 (16) | O2—Pr—O1ii | 70.32 (15) |
O3ii—Pr—O2 | 78.9 (2) | O2ii—Pr—O1ii | 70.32 (15) |
O3iii—Pr—O2 | 78.9 (2) | O1—Pr—O1ii | 126.8 (4) |
O3—Pr—O2ii | 78.9 (2) | O3—Pr—O4 | 68.43 (13) |
O3i—Pr—O2ii | 78.9 (2) | O3i—Pr—O4 | 68.43 (13) |
O3ii—Pr—O2ii | 138.20 (16) | O3ii—Pr—O4 | 68.43 (13) |
O3iii—Pr—O2ii | 138.20 (16) | O3iii—Pr—O4 | 68.43 (13) |
O2—Pr—O2ii | 82.5 (4) | O2—Pr—O4 | 138.8 (2) |
O3—Pr—O1 | 134.43 (14) | O2ii—Pr—O4 | 138.8 (2) |
O3i—Pr—O1 | 68.24 (17) | O1—Pr—O4 | 116.60 (19) |
O3ii—Pr—O1 | 68.24 (17) | O1ii—Pr—O4 | 116.60 (19) |
Symmetry codes: (i) −x+1/2, y, z; (ii) −x+1/2, −y+1/2, z; (iii) x, −y+1/2, z. |