metal-organic compounds
catena-Poly[[tris(acetonitrile-κN)praseodymium(III)]tris(μ-trifluoromethanesulfonato-κ2O:O′)]
aEuropean Commission, Joint Research Centre, Institute for Transuranium Elements, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany
*Correspondence e-mail: olaf.walter@ec.europa.eu
In the colourless title compound, [Pr(CF3O3S)3(CH3CN)3]n, the three trifluoromethanesulfonate anions form three bridges via O:O′-coordination between two PrIII atoms. The structure contains [Pr(NCMe)3-μ2(OTf)3—Pr(NCMe)3-μ2(OTf)3]n (NCMe is acetonitrile; OTf is trifluoromethanesulfonate) chains parallel to the a axis. The PrIII atom is nine-coordinate in a distorted tricapped trigonal-prismatic environment.
Related literature
For the isostructural EuIII and UIII compounds, see: Tang et al. (2011) and Natrajan et al. (2005), respectively.
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2007); cell SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XPMA (Zsolnai, 1996) and ORTEP-3 (Farrugia, 2012); software used to prepare material for publication: publCIF (Westrip, 2010).
Supporting information
https://doi.org/10.1107/S1600536812049525/vn2063sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812049525/vn2063Isup2.hkl
Supporting information file. DOI: https://doi.org/10.1107/S1600536812049525/vn2063Isup3.mol
Crystals from the title compound precipitated after a ligand exchange reaction from 103.1 mg (0.13 mmol) [Pr(H2O)9](OTf)3 in 2 ml of MeCN. Crystals in the form of needles suitable for x-ray analysis were obtained by re-crystallization from hot MeCN.
All H atoms were placed on geometrical positions according to the
of the atoms they are bound to. One common isotropic U value was used and refined for all hydrogen atoms.The coordination environment of the PrIII atom ion in the title compound can be described as a distorted trigonal tri-capped prism. 6 O atoms are forming the trigonal prismatic environment around the PrIII atom and the three N atoms of the coordinated MeCN solvent molecules are forming the cappings over the rectangular sides of the prism. The metal-O distances in the title compound are with an average of 2.458 (13) Å about 0.05 Å longer than in the corresponding Eu complex (Tang et al., 2011) and 0.04 Å shorter than in its U analogue (Natrajan et al., 2005) reflecting the effects of the lanthanide contraction and also the change from a lanthanide to an actinide ion. The metal-N distances with 2.588 (17) Å for the Eu complex are about 0.05 Å shorter than for the here presented Pr compound with 2.640 (17) Å, whereas the latter are found to be in very good agreement with those in the U complex with 2.651 (14) Å. The ion size increase while changing the metal ion in the complex from Pr to U seems to influence more the shorter metal-O distances than the longer metal-N distances for the solvent molecules forming the cappings of the trigonal prism.
For the isostructural EuIII and UIII compounds, see: Tang et al. (2011) and Natrajan et al. (2005), respectively.
Data collection: APEX2 (Bruker, 2007); cell
SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XPMA (Zsolnai, 1996) and ORTEP-3 (Farrugia, 2012); software used to prepare material for publication: publCIF (Westrip, 2010).Fig. 1. Molecular structure of the title compound; ellipsoids at the 50% probability level (symmetry codes: a = x + 1, y, z; b = x - 1, y, z). |
[Pr(CF3O3S)3(C2H3N)3] | Z = 2 |
Mr = 711.28 | F(000) = 688 |
Triclinic, P1 | Dx = 2.064 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 5.8044 (6) Å | Cell parameters from 9222 reflections |
b = 10.5062 (10) Å | θ = 2.2–28.1° |
c = 18.9887 (19) Å | µ = 2.52 mm−1 |
α = 97.307 (1)° | T = 103 K |
β = 94.163 (1)° | Needle, colourless |
γ = 91.695 (1)° | 0.24 × 0.02 × 0.01 mm |
V = 1144.7 (2) Å3 |
Bruker APEXII Quazar diffractometer | 5251 independent reflections |
Radiation source: fine-focus sealed tube | 4674 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
Detector resolution: 66 pixels mm-1 | θmax = 28.2°, θmin = 1.1° |
combined ω and φ scans | h = −7→7 |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | k = −13→13 |
Tmin = 0.578, Tmax = 0.978 | l = −25→24 |
20544 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)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.076 | H-atom parameters constrained |
S = 1.16 | w = 1/[σ2(Fo2) + (0.0169P)2 + 4.422P] where P = (Fo2 + 2Fc2)/3 |
5251 reflections | (Δ/σ)max = 0.001 |
311 parameters | Δρmax = 1.04 e Å−3 |
0 restraints | Δρmin = −1.15 e Å−3 |
[Pr(CF3O3S)3(C2H3N)3] | γ = 91.695 (1)° |
Mr = 711.28 | V = 1144.7 (2) Å3 |
Triclinic, P1 | Z = 2 |
a = 5.8044 (6) Å | Mo Kα radiation |
b = 10.5062 (10) Å | µ = 2.52 mm−1 |
c = 18.9887 (19) Å | T = 103 K |
α = 97.307 (1)° | 0.24 × 0.02 × 0.01 mm |
β = 94.163 (1)° |
Bruker APEXII Quazar diffractometer | 5251 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 4674 reflections with I > 2σ(I) |
Tmin = 0.578, Tmax = 0.978 | Rint = 0.039 |
20544 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | 0 restraints |
wR(F2) = 0.076 | H-atom parameters constrained |
S = 1.16 | Δρmax = 1.04 e Å−3 |
5251 reflections | Δρmin = −1.15 e Å−3 |
311 parameters |
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 | ||
Pr1 | 1.07535 (4) | 0.07978 (2) | 0.262548 (13) | 0.01276 (7) | |
S1 | 0.56250 (16) | 0.18346 (10) | 0.15067 (6) | 0.0158 (2) | |
S2 | 0.61165 (16) | 0.18294 (10) | 0.39162 (6) | 0.0158 (2) | |
S3 | 0.55261 (16) | −0.16488 (10) | 0.24609 (6) | 0.0147 (2) | |
F1 | 0.6947 (6) | 0.3922 (3) | 0.10237 (19) | 0.0467 (9) | |
F2 | 0.3309 (6) | 0.3778 (3) | 0.11712 (19) | 0.0450 (9) | |
F3 | 0.5755 (5) | 0.4245 (3) | 0.20746 (15) | 0.0299 (6) | |
F4 | 0.7997 (5) | 0.3949 (3) | 0.46088 (18) | 0.0440 (8) | |
F5 | 0.4258 (5) | 0.3828 (3) | 0.45649 (18) | 0.0422 (8) | |
F6 | 0.5975 (5) | 0.4226 (3) | 0.36502 (17) | 0.0344 (7) | |
F7 | 0.7193 (5) | −0.3223 (3) | 0.14700 (16) | 0.0320 (7) | |
F8 | 0.3474 (5) | −0.3357 (3) | 0.14802 (16) | 0.0338 (7) | |
F9 | 0.5120 (4) | −0.1770 (3) | 0.10682 (14) | 0.0258 (6) | |
O1 | 0.3838 (5) | 0.1578 (3) | 0.19688 (18) | 0.0240 (7) | |
O2 | 0.7937 (5) | 0.1773 (3) | 0.18415 (17) | 0.0216 (7) | |
O3 | 0.5278 (6) | 0.1225 (3) | 0.07935 (17) | 0.0276 (7) | |
O4 | 0.3864 (5) | 0.1540 (3) | 0.35450 (17) | 0.0223 (7) | |
O5 | 0.7984 (5) | 0.1725 (3) | 0.34527 (17) | 0.0230 (7) | |
O6 | 0.6489 (5) | 0.1277 (3) | 0.45609 (17) | 0.0270 (7) | |
O7 | 0.7431 (5) | −0.0746 (3) | 0.24309 (17) | 0.0208 (7) | |
O8 | 0.3323 (5) | −0.1040 (3) | 0.25044 (16) | 0.0186 (6) | |
O9 | 0.5924 (5) | −0.2595 (3) | 0.29293 (17) | 0.0233 (7) | |
N1 | 1.0406 (6) | −0.0433 (4) | 0.1330 (2) | 0.0225 (8) | |
N2 | 1.1033 (6) | 0.3339 (4) | 0.2835 (2) | 0.0216 (8) | |
N3 | 1.0456 (6) | −0.0546 (4) | 0.3708 (2) | 0.0214 (8) | |
C1 | 0.5396 (8) | 0.3551 (4) | 0.1440 (3) | 0.0238 (10) | |
C2 | 0.6081 (8) | 0.3553 (5) | 0.4193 (3) | 0.0270 (11) | |
C3 | 0.5309 (7) | −0.2545 (4) | 0.1566 (2) | 0.0207 (9) | |
C4 | 1.0185 (7) | −0.1019 (5) | 0.0786 (3) | 0.0219 (10) | |
C5 | 0.9892 (9) | −0.1778 (6) | 0.0081 (3) | 0.0377 (13) | |
H5A | 0.9788 | −0.2693 | 0.0134 | 0.083 (9)* | |
H5B | 1.1219 | −0.1607 | −0.0189 | 0.083 (9)* | |
H5C | 0.8472 | −0.1540 | −0.0174 | 0.083 (9)* | |
C6 | 1.0979 (7) | 0.4424 (5) | 0.2948 (3) | 0.0261 (11) | |
C7 | 1.0879 (10) | 0.5816 (5) | 0.3096 (5) | 0.057 (2) | |
H7A | 0.9471 | 0.6098 | 0.2854 | 0.083 (9)* | |
H7B | 1.2236 | 0.6219 | 0.2923 | 0.083 (9)* | |
H7C | 1.0864 | 0.6067 | 0.3611 | 0.083 (9)* | |
C8 | 0.9551 (7) | −0.1080 (4) | 0.4105 (2) | 0.0212 (9) | |
C9 | 0.8291 (8) | −0.1738 (5) | 0.4598 (3) | 0.0283 (11) | |
H9A | 0.7095 | −0.1184 | 0.4790 | 0.083 (9)* | |
H9B | 0.9365 | −0.1933 | 0.4989 | 0.083 (9)* | |
H9C | 0.7567 | −0.2538 | 0.4346 | 0.083 (9)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pr1 | 0.00653 (9) | 0.01308 (12) | 0.01839 (12) | −0.00110 (7) | 0.00174 (7) | 0.00089 (8) |
S1 | 0.0118 (4) | 0.0162 (5) | 0.0198 (5) | −0.0006 (4) | 0.0023 (4) | 0.0039 (4) |
S2 | 0.0104 (4) | 0.0182 (5) | 0.0177 (5) | −0.0012 (4) | 0.0018 (4) | −0.0015 (4) |
S3 | 0.0101 (4) | 0.0124 (5) | 0.0215 (5) | −0.0011 (3) | 0.0013 (4) | 0.0017 (4) |
F1 | 0.069 (2) | 0.0256 (17) | 0.051 (2) | −0.0047 (15) | 0.0294 (18) | 0.0160 (16) |
F2 | 0.0451 (19) | 0.0280 (17) | 0.059 (2) | 0.0138 (14) | −0.0205 (16) | 0.0072 (16) |
F3 | 0.0326 (15) | 0.0204 (15) | 0.0351 (17) | 0.0005 (11) | 0.0012 (12) | −0.0014 (12) |
F4 | 0.0312 (16) | 0.0360 (18) | 0.055 (2) | −0.0067 (13) | −0.0136 (14) | −0.0178 (16) |
F5 | 0.0357 (16) | 0.0319 (18) | 0.056 (2) | 0.0040 (13) | 0.0219 (15) | −0.0165 (15) |
F6 | 0.0276 (15) | 0.0199 (15) | 0.056 (2) | −0.0004 (11) | 0.0017 (13) | 0.0051 (14) |
F7 | 0.0307 (15) | 0.0266 (16) | 0.0381 (17) | 0.0115 (12) | 0.0087 (12) | −0.0034 (13) |
F8 | 0.0293 (15) | 0.0263 (16) | 0.0419 (18) | −0.0140 (12) | 0.0013 (12) | −0.0068 (13) |
F9 | 0.0236 (13) | 0.0315 (16) | 0.0222 (14) | 0.0012 (11) | 0.0006 (10) | 0.0031 (12) |
O1 | 0.0164 (14) | 0.0217 (17) | 0.0349 (19) | −0.0018 (12) | 0.0103 (13) | 0.0036 (14) |
O2 | 0.0137 (14) | 0.0215 (17) | 0.0292 (18) | −0.0002 (12) | −0.0021 (12) | 0.0045 (14) |
O3 | 0.0307 (17) | 0.0279 (19) | 0.0228 (18) | −0.0002 (14) | 0.0009 (13) | −0.0010 (14) |
O4 | 0.0141 (14) | 0.0206 (17) | 0.0297 (18) | −0.0033 (12) | −0.0037 (12) | −0.0019 (14) |
O5 | 0.0198 (15) | 0.0198 (17) | 0.0299 (18) | 0.0023 (12) | 0.0111 (13) | −0.0002 (14) |
O6 | 0.0243 (16) | 0.034 (2) | 0.0228 (18) | 0.0030 (14) | 0.0035 (13) | 0.0051 (15) |
O7 | 0.0120 (13) | 0.0223 (17) | 0.0275 (18) | −0.0090 (11) | 0.0001 (12) | 0.0034 (14) |
O8 | 0.0146 (14) | 0.0171 (16) | 0.0242 (17) | 0.0023 (11) | 0.0031 (11) | 0.0010 (13) |
O9 | 0.0208 (15) | 0.0204 (17) | 0.0304 (19) | −0.0004 (12) | 0.0013 (13) | 0.0110 (14) |
N1 | 0.0139 (17) | 0.029 (2) | 0.024 (2) | 0.0009 (15) | 0.0015 (14) | 0.0008 (18) |
N2 | 0.0129 (16) | 0.020 (2) | 0.032 (2) | −0.0025 (14) | 0.0031 (14) | 0.0038 (17) |
N3 | 0.0165 (17) | 0.022 (2) | 0.026 (2) | 0.0023 (14) | 0.0029 (15) | 0.0017 (17) |
C1 | 0.025 (2) | 0.018 (2) | 0.029 (3) | 0.0009 (17) | 0.0011 (18) | 0.008 (2) |
C2 | 0.018 (2) | 0.025 (3) | 0.034 (3) | −0.0017 (18) | 0.0005 (18) | −0.010 (2) |
C3 | 0.0157 (19) | 0.017 (2) | 0.027 (3) | −0.0003 (16) | 0.0022 (17) | −0.0055 (19) |
C4 | 0.0127 (19) | 0.029 (3) | 0.024 (3) | 0.0004 (17) | 0.0024 (16) | 0.005 (2) |
C5 | 0.038 (3) | 0.051 (4) | 0.021 (3) | 0.000 (2) | 0.002 (2) | −0.006 (2) |
C6 | 0.0120 (19) | 0.023 (3) | 0.044 (3) | −0.0016 (16) | 0.0060 (18) | 0.004 (2) |
C7 | 0.032 (3) | 0.016 (3) | 0.123 (7) | −0.001 (2) | 0.022 (3) | 0.002 (3) |
C8 | 0.017 (2) | 0.022 (2) | 0.025 (2) | 0.0014 (17) | 0.0001 (17) | 0.002 (2) |
C9 | 0.022 (2) | 0.041 (3) | 0.023 (2) | −0.005 (2) | 0.0025 (18) | 0.010 (2) |
Pr1—O1i | 2.435 (3) | F4—C2 | 1.340 (5) |
Pr1—O2 | 2.464 (3) | F5—C2 | 1.333 (5) |
Pr1—O4i | 2.455 (3) | F6—C2 | 1.320 (6) |
Pr1—O5 | 2.464 (3) | F7—C3 | 1.333 (5) |
Pr1—O7 | 2.459 (3) | F8—C3 | 1.332 (5) |
Pr1—O8i | 2.473 (3) | F9—C3 | 1.324 (5) |
Pr1—N1 | 2.621 (4) | O1—Pr1ii | 2.435 (3) |
Pr1—N2 | 2.648 (4) | O4—Pr1ii | 2.455 (3) |
Pr1—N3 | 2.651 (4) | O8—Pr1ii | 2.473 (3) |
S1—O3 | 1.420 (3) | N1—C4 | 1.130 (6) |
S1—O1 | 1.447 (3) | N2—C6 | 1.134 (6) |
S1—O2 | 1.450 (3) | N3—C8 | 1.142 (6) |
S1—C1 | 1.832 (5) | C4—C5 | 1.464 (7) |
S2—O6 | 1.426 (3) | C5—H5A | 0.9800 |
S2—O5 | 1.443 (3) | C5—H5B | 0.9800 |
S2—O4 | 1.445 (3) | C5—H5C | 0.9800 |
S2—C2 | 1.822 (5) | C6—C7 | 1.457 (7) |
S3—O9 | 1.429 (3) | C7—H7A | 0.9800 |
S3—O7 | 1.444 (3) | C7—H7B | 0.9800 |
S3—O8 | 1.449 (3) | C7—H7C | 0.9800 |
S3—C3 | 1.829 (5) | C8—C9 | 1.457 (6) |
F1—C1 | 1.322 (5) | C9—H9A | 0.9800 |
F2—C1 | 1.320 (5) | C9—H9B | 0.9800 |
F3—C1 | 1.326 (5) | C9—H9C | 0.9800 |
O1i—Pr1—O4i | 75.59 (11) | O9—S3—C3 | 105.0 (2) |
O1i—Pr1—O7 | 139.23 (11) | O7—S3—C3 | 102.39 (19) |
O4i—Pr1—O7 | 139.22 (11) | O8—S3—C3 | 103.59 (19) |
O1i—Pr1—O2 | 88.88 (10) | S1—O1—Pr1ii | 170.4 (2) |
O4i—Pr1—O2 | 137.29 (10) | S1—O2—Pr1 | 151.05 (19) |
O7—Pr1—O2 | 75.57 (10) | S2—O4—Pr1ii | 162.7 (2) |
O1i—Pr1—O5 | 137.30 (11) | S2—O5—Pr1 | 161.1 (2) |
O4i—Pr1—O5 | 88.00 (10) | S3—O7—Pr1 | 169.2 (2) |
O7—Pr1—O5 | 76.01 (10) | S3—O8—Pr1ii | 155.19 (18) |
O2—Pr1—O5 | 76.90 (11) | C4—N1—Pr1 | 175.9 (4) |
O1i—Pr1—O8i | 77.31 (10) | C6—N2—Pr1 | 174.3 (3) |
O4i—Pr1—O8i | 79.12 (10) | C8—N3—Pr1 | 156.4 (3) |
O7—Pr1—O8i | 88.37 (10) | F2—C1—F1 | 109.2 (4) |
O2—Pr1—O8i | 136.43 (10) | F2—C1—F3 | 108.1 (4) |
O5—Pr1—O8i | 138.43 (10) | F1—C1—F3 | 108.5 (4) |
O1i—Pr1—N1 | 71.04 (11) | F2—C1—S1 | 110.0 (3) |
O4i—Pr1—N1 | 137.12 (11) | F1—C1—S1 | 109.9 (3) |
O7—Pr1—N1 | 68.20 (11) | F3—C1—S1 | 111.1 (3) |
O2—Pr1—N1 | 68.43 (11) | F6—C2—F5 | 107.8 (4) |
O5—Pr1—N1 | 134.88 (11) | F6—C2—F4 | 107.8 (4) |
O8i—Pr1—N1 | 68.00 (11) | F5—C2—F4 | 108.2 (4) |
O1i—Pr1—N2 | 70.21 (11) | F6—C2—S2 | 112.9 (3) |
O4i—Pr1—N2 | 70.03 (11) | F5—C2—S2 | 110.0 (3) |
O7—Pr1—N2 | 132.10 (10) | F4—C2—S2 | 110.0 (3) |
O2—Pr1—N2 | 67.28 (11) | F9—C3—F8 | 108.5 (4) |
O5—Pr1—N2 | 67.15 (11) | F9—C3—F7 | 108.1 (4) |
O8i—Pr1—N2 | 139.51 (10) | F8—C3—F7 | 108.3 (4) |
N1—Pr1—N2 | 120.35 (12) | F9—C3—S3 | 111.7 (3) |
O1i—Pr1—N3 | 136.38 (11) | F8—C3—S3 | 110.3 (3) |
O4i—Pr1—N3 | 71.01 (11) | F7—C3—S3 | 109.8 (3) |
O7—Pr1—N3 | 68.24 (11) | N1—C4—C5 | 179.8 (6) |
O2—Pr1—N3 | 134.74 (10) | C4—C5—H5A | 109.5 |
O5—Pr1—N3 | 68.85 (11) | C4—C5—H5B | 109.5 |
O8i—Pr1—N3 | 69.59 (11) | H5A—C5—H5B | 109.5 |
N1—Pr1—N3 | 118.54 (12) | C4—C5—H5C | 109.5 |
N2—Pr1—N3 | 120.91 (12) | H5A—C5—H5C | 109.5 |
O3—S1—O1 | 115.7 (2) | H5B—C5—H5C | 109.5 |
O3—S1—O2 | 115.4 (2) | N2—C6—C7 | 179.2 (5) |
O1—S1—O2 | 112.91 (19) | C6—C7—H7A | 109.5 |
O3—S1—C1 | 104.8 (2) | C6—C7—H7B | 109.5 |
O1—S1—C1 | 103.3 (2) | H7A—C7—H7B | 109.5 |
O2—S1—C1 | 102.54 (19) | C6—C7—H7C | 109.5 |
O6—S2—O5 | 115.65 (19) | H7A—C7—H7C | 109.5 |
O6—S2—O4 | 114.9 (2) | H7B—C7—H7C | 109.5 |
O5—S2—O4 | 113.45 (19) | N3—C8—C9 | 177.2 (5) |
O6—S2—C2 | 105.1 (2) | C8—C9—H9A | 109.5 |
O5—S2—C2 | 102.6 (2) | C8—C9—H9B | 109.5 |
O4—S2—C2 | 102.99 (19) | H9A—C9—H9B | 109.5 |
O9—S3—O7 | 115.75 (18) | C8—C9—H9C | 109.5 |
O9—S3—O8 | 115.15 (19) | H9A—C9—H9C | 109.5 |
O7—S3—O8 | 112.91 (18) | H9B—C9—H9C | 109.5 |
Symmetry codes: (i) x+1, y, z; (ii) x−1, y, z. |
Experimental details
Crystal data | |
Chemical formula | [Pr(CF3O3S)3(C2H3N)3] |
Mr | 711.28 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 103 |
a, b, c (Å) | 5.8044 (6), 10.5062 (10), 18.9887 (19) |
α, β, γ (°) | 97.307 (1), 94.163 (1), 91.695 (1) |
V (Å3) | 1144.7 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.52 |
Crystal size (mm) | 0.24 × 0.02 × 0.01 |
Data collection | |
Diffractometer | Bruker APEXII Quazar |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.578, 0.978 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 20544, 5251, 4674 |
Rint | 0.039 |
(sin θ/λ)max (Å−1) | 0.666 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.076, 1.16 |
No. of reflections | 5251 |
No. of parameters | 311 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.04, −1.15 |
Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XPMA (Zsolnai, 1996) and ORTEP-3 (Farrugia, 2012), publCIF (Westrip, 2010).
Pr1—O1i | 2.435 (3) | Pr1—O8i | 2.473 (3) |
Pr1—O2 | 2.464 (3) | Pr1—N1 | 2.621 (4) |
Pr1—O4i | 2.455 (3) | Pr1—N2 | 2.648 (4) |
Pr1—O5 | 2.464 (3) | Pr1—N3 | 2.651 (4) |
Pr1—O7 | 2.459 (3) |
Symmetry code: (i) x+1, y, z. |
Footnotes
‡Also affiliated to: IKFT, KIT-Campus Nord, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany.
References
Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2007). APEX and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849–854. Web of Science CrossRef CAS IUCr Journals Google Scholar
Natrajan, L., Mazzanti, M., Bezombes, J.-P. & Pecaut, J. (2005). Inorg. Chem. 44, 6115–6121. Web of Science CSD CrossRef PubMed CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Tang, S. (2011). Cryst. Growth Des. 11, 1437–1440. CSD CrossRef CAS Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zsolnai, L. (1996). XPMA. University of Heidelberg, Germany. Google Scholar
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The coordination environment of the PrIII atom ion in the title compound can be described as a distorted trigonal tri-capped prism. 6 O atoms are forming the trigonal prismatic environment around the PrIII atom and the three N atoms of the coordinated MeCN solvent molecules are forming the cappings over the rectangular sides of the prism. The metal-O distances in the title compound are with an average of 2.458 (13) Å about 0.05 Å longer than in the corresponding Eu complex (Tang et al., 2011) and 0.04 Å shorter than in its U analogue (Natrajan et al., 2005) reflecting the effects of the lanthanide contraction and also the change from a lanthanide to an actinide ion. The metal-N distances with 2.588 (17) Å for the Eu complex are about 0.05 Å shorter than for the here presented Pr compound with 2.640 (17) Å, whereas the latter are found to be in very good agreement with those in the U complex with 2.651 (14) Å. The ion size increase while changing the metal ion in the complex from Pr to U seems to influence more the shorter metal-O distances than the longer metal-N distances for the solvent molecules forming the cappings of the trigonal prism.