Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806005113/wm6136sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806005113/wm6136Isup2.hkl |
Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97.
FeI12Pr7 | Dx = 5.461 Mg m−3 |
Mr = 2565.02 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3 | Cell parameters from 13127 reflections |
Hall symbol: -R 3 | θ = 2.4–32.2° |
a = 15.8296 (10) Å | µ = 23.02 mm−1 |
c = 10.7833 (6) Å | T = 293 K |
V = 2340.0 (2) Å3 | Rhomb, black |
Z = 3 | 0.25 × 0.15 × 0.05 mm |
F(000) = 3225 |
Stoe IPDS-II diffractometer | 1829 independent reflections |
Radiation source: fine-focus sealed tube | 1593 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.065 |
ω and φ scans | θmax = 32.2°, θmin = 2.4° |
Absorption correction: numerical [X-SHAPE (Stoe & Cie, 1999) and X-RED (Stoe & Cie, 2001)] | h = −23→23 |
Tmin = 0.027, Tmax = 0.324 | k = −23→23 |
13579 measured reflections | l = −15→16 |
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)] = 0.046 | w = 1/[σ2(Fo2) + (0.0261P)2 + 153.022P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.099 | (Δ/σ)max = 0.001 |
S = 1.04 | Δρmax = 3.54 e Å−3 |
1829 reflections | Δρmin = −5.98 e Å−3 |
33 parameters | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00067 (3) |
Experimental. A suitable single-crystal was carefully selected under a polarizing microscope and mounted in a glass capillary. The scattering intensities were collected on an imaging plate diffractometer (IPDS II, Stoe & Cie) equipped with a fine focus sealed tube X-ray source (Mo Kα, λ = 0.71073 Å) operating at 50 kV and 40 mA. Intensity data for the title compound were collected at room temperature by ω-scans in 254 frames (0 < ω < 180°; φ = O°, 0 < ω < 74°; φ = 90°, Δω = 1°, exposure time of 5 min) in the 2 Θ range 2.9 to 64.8°. Structure solution and refinement were carried out using the programs SIR92 (Altomare et al., 1993) and 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 last cycles of refinement included atomic positions and anisotropic parameters for all atoms. 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-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 | ||
Pr2 | 0.44849 (3) | 0.62205 (3) | 0.01862 (4) | 0.02645 (14) | |
Pr1 | 0.3333 | 0.6667 | 0.6667 | 0.0507 (4) | |
I1 | 0.41239 (4) | 0.43177 (4) | 0.16421 (5) | 0.03380 (16) | |
I2 | 0.52062 (4) | 0.80126 (4) | 0.82596 (5) | 0.02966 (15) | |
Fe | 0.3333 | 0.6667 | 0.1667 | 0.0180 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pr2 | 0.0257 (2) | 0.0217 (2) | 0.0285 (2) | 0.00922 (15) | −0.00511 (14) | 0.00157 (14) |
Pr1 | 0.0282 (4) | 0.0282 (4) | 0.0957 (12) | 0.01410 (18) | 0.000 | 0.000 |
I1 | 0.0424 (3) | 0.0327 (3) | 0.0369 (3) | 0.0267 (2) | 0.0131 (2) | 0.0087 (2) |
I2 | 0.0314 (3) | 0.0299 (3) | 0.0285 (3) | 0.0159 (2) | 0.00662 (18) | 0.00437 (17) |
Fe | 0.0170 (6) | 0.0170 (6) | 0.0200 (10) | 0.0085 (3) | 0.000 | 0.000 |
Pr2—Fe | 2.7672 (5) | Pr1—I2 | 3.1564 (6) |
Pr2—I1 | 3.1847 (7) | Pr1—I2vi | 3.1564 (6) |
Pr2—I1i | 3.1950 (7) | Pr1—I2x | 3.1564 (6) |
Pr2—I2ii | 3.2292 (7) | I1—Pr2v | 3.1951 (7) |
Pr2—I2iii | 3.2367 (7) | I1—Pr2iv | 3.3674 (7) |
Pr2—I1iv | 3.3674 (7) | I2—Pr2xi | 3.2292 (7) |
Pr2—Pr2v | 3.9119 (8) | I2—Pr2xii | 3.2367 (7) |
Pr2—Pr2i | 3.9119 (8) | Fe—Pr2v | 2.7672 (5) |
Pr2—Pr2vi | 3.9150 (8) | Fe—Pr2vi | 2.7672 (5) |
Pr2—Pr2vii | 3.9150 (8) | Fe—Pr2vii | 2.7672 (5) |
Pr1—I2viii | 3.1564 (6) | Fe—Pr2i | 2.7672 (5) |
Pr1—I2vii | 3.1564 (6) | Fe—Pr2xiii | 2.7673 (5) |
Pr1—I2ix | 3.1564 (6) | ||
Fe—Pr2—I1 | 97.320 (16) | I1iv—Pr2—Pr2vii | 134.585 (15) |
Fe—Pr2—I1i | 97.080 (16) | Pr2v—Pr2—Pr2vii | 90.0 |
I1—Pr2—I1i | 89.147 (11) | Pr2i—Pr2—Pr2vii | 59.973 (7) |
Fe—Pr2—I2ii | 97.798 (16) | Pr2vi—Pr2—Pr2vii | 60.0 |
I1—Pr2—I2ii | 164.88 (2) | I2viii—Pr1—I2vii | 180.0 |
I1i—Pr2—I2ii | 88.923 (18) | I2viii—Pr1—I2ix | 93.198 (13) |
Fe—Pr2—I2iii | 97.624 (16) | I2vii—Pr1—I2ix | 86.802 (13) |
I1—Pr2—I2iii | 87.705 (19) | I2viii—Pr1—I2 | 86.803 (13) |
I1i—Pr2—I2iii | 165.24 (2) | I2vii—Pr1—I2 | 93.197 (13) |
I2ii—Pr2—I2iii | 90.36 (2) | I2ix—Pr1—I2 | 180.0 |
Fe—Pr2—I1iv | 179.395 (18) | I2viii—Pr1—I2vi | 86.803 (13) |
I1—Pr2—I1iv | 83.112 (17) | I2vii—Pr1—I2vi | 93.197 (13) |
I1i—Pr2—I1iv | 83.344 (18) | I2ix—Pr1—I2vi | 86.803 (13) |
I2ii—Pr2—I1iv | 81.771 (17) | I2—Pr1—I2vi | 93.197 (13) |
I2iii—Pr2—I1iv | 81.964 (18) | I2viii—Pr1—I2x | 93.198 (13) |
Fe—Pr2—Pr2v | 45.022 (6) | I2vii—Pr1—I2x | 86.802 (13) |
I1—Pr2—Pr2v | 52.302 (15) | I2ix—Pr1—I2x | 93.197 (13) |
I1i—Pr2—Pr2v | 94.597 (18) | I2—Pr1—I2x | 86.803 (13) |
I2ii—Pr2—Pr2v | 142.815 (14) | I2vi—Pr1—I2x | 180.0 |
I2iii—Pr2—Pr2v | 94.865 (14) | Pr2—I1—Pr2v | 75.64 (2) |
I1iv—Pr2—Pr2v | 135.413 (15) | Pr2—I1—Pr2iv | 96.888 (17) |
Fe—Pr2—Pr2i | 45.022 (6) | Pr2v—I1—Pr2iv | 172.53 (2) |
I1—Pr2—Pr2i | 95.633 (19) | Pr1—I2—Pr2xi | 87.532 (16) |
I1i—Pr2—Pr2i | 52.061 (15) | Pr1—I2—Pr2xii | 87.402 (16) |
I2ii—Pr2—Pr2i | 94.987 (14) | Pr2xi—I2—Pr2xii | 74.53 (2) |
I2iii—Pr2—Pr2i | 142.641 (15) | Pr2v—Fe—Pr2vi | 89.955 (12) |
I1iv—Pr2—Pr2i | 135.395 (16) | Pr2v—Fe—Pr2vii | 180.0 |
Pr2v—Pr2—Pr2i | 60.051 (14) | Pr2vi—Fe—Pr2vii | 90.045 (12) |
Fe—Pr2—Pr2vi | 44.977 (6) | Pr2v—Fe—Pr2i | 90.046 (12) |
I1—Pr2—Pr2vi | 94.706 (18) | Pr2vi—Fe—Pr2i | 180.0 |
I1i—Pr2—Pr2vi | 142.053 (14) | Pr2vii—Fe—Pr2i | 89.954 (12) |
I2ii—Pr2—Pr2vi | 96.025 (13) | Pr2v—Fe—Pr2 | 89.956 (12) |
I2iii—Pr2—Pr2vi | 52.650 (15) | Pr2vi—Fe—Pr2 | 90.045 (12) |
I1iv—Pr2—Pr2vi | 134.602 (16) | Pr2vii—Fe—Pr2 | 90.045 (12) |
Pr2v—Pr2—Pr2vi | 59.973 (7) | Pr2i—Fe—Pr2 | 89.956 (12) |
Pr2i—Pr2—Pr2vi | 90.0 | Pr2v—Fe—Pr2xiii | 90.044 (12) |
Fe—Pr2—Pr2vii | 44.977 (6) | Pr2vi—Fe—Pr2xiii | 89.955 (12) |
I1—Pr2—Pr2vii | 142.294 (15) | Pr2vii—Fe—Pr2xiii | 89.954 (12) |
I1i—Pr2—Pr2vii | 95.402 (18) | Pr2i—Fe—Pr2xiii | 90.044 (12) |
I2ii—Pr2—Pr2vii | 52.824 (14) | Pr2—Fe—Pr2xiii | 179.999 (13) |
I2iii—Pr2—Pr2vii | 95.900 (13) |
Symmetry codes: (i) x−y+2/3, x+1/3, −z+1/3; (ii) x, y, z−1; (iii) −x+y, −x+1, z−1; (iv) −x+1, −y+1, −z; (v) y−1/3, −x+y+1/3, −z+1/3; (vi) −x+y, −x+1, z; (vii) −y+1, x−y+1, z; (viii) y−1/3, −x+y+1/3, −z+4/3; (ix) −x+2/3, −y+4/3, −z+4/3; (x) x−y+2/3, x+1/3, −z+4/3; (xi) x, y, z+1; (xii) −y+1, x−y+1, z+1; (xiii) −x+2/3, −y+4/3, −z+1/3. |