catena-Poly[[tris­(acetonitrile-κN)praseodymium(III)]tris­(μ-trifluoro­methane­sulfonato-κ2O:O′)]

Apostolidis, C.; Walter, O.

doi:10.1107/S1600536812049525

metal-organic compounds

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ISSN: 2056-9890

Volume 69| Part 1| January 2013| Page m21

https://doi.org/10.1107/S1600536812049525

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catena-Poly[[tris(acetonitrile-κN)praseodymium(III)]tris(μ-trifluoromethanesulfonato-κ²O:O′)]

Christos Apostolidis ^a and Olaf Walter ^a ^*‡

^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

(Received 26 November 2012; accepted 3 December 2012; online 8 December 2012)

In the colourless title compound, [Pr(CF₃O₃S)₃(CH₃CN)₃]_n, the three trifluoromethanesulfonate anions form three bridges via O:O′-coordination between two Pr^III 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 Pr^III atom is nine-coordinate in a distorted tricapped trigonal-prismatic environment.

Related literature

For the isostructural Eu^III and U^III compounds, see: Tang et al. (2011 ) and Natrajan et al. (2005 ), respectively.

Experimental

Crystal data

[Pr(CF₃O₃S)₃(C₂H₃N)₃]
M_r = 711.28
Triclinic, $[P \overline 1]$
a = 5.8044 (6) Å
b = 10.5062 (10) Å
c = 18.9887 (19) Å
α = 97.307 (1)°
β = 94.163 (1)°
γ = 91.695 (1)°
V = 1144.7 (2) Å³
Z = 2
Mo Kα radiation
μ = 2.52 mm⁻¹
T = 103 K
0.24 × 0.02 × 0.01 mm

Data collection

Bruker APEXII Quazar diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ) T_min = 0.578, T_max = 0.978
20544 measured reflections
5251 independent reflections
4674 reflections with I > 2σ(I)
R_int = 0.039

Refinement

R[F² > 2σ(F²)] = 0.036
wR(F²) = 0.076
S = 1.16
5251 reflections
311 parameters
H-atom parameters constrained
Δρ_max = 1.04 e Å⁻³
Δρ_min = −1.15 e Å⁻³

Table 1
Selected bond lengths (Å)

Pr1—O1ⁱ	2.435 (3)
Pr1—O2	2.464 (3)
Pr1—O4ⁱ	2.455 (3)
Pr1—O5	2.464 (3)
Pr1—O7	2.459 (3)
Pr1—O8ⁱ	2.473 (3)
Pr1—N1	2.621 (4)
Pr1—N2	2.648 (4)
Pr1—N3	2.651 (4)
Symmetry code: (i) x+1, y, z.

Data collection: APEX2 (Bruker, 2007 ); cell refinement: 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

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536812049525/vn2063sup1.cif

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

checkCIF report

Comment top

The coordination environment of the Pr^III 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 Pr^III 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.

Related literature top

For the isostructural Eu^III and U^III compounds, see: Tang et al. (2011) and Natrajan et al. (2005), respectively.

Experimental top

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.

Structure description top

For the isostructural Eu^III and U^III compounds, see: Tang et al. (2011) and Natrajan et al. (2005), respectively.

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: 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).

Figures top

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).

catena-Poly[[tris(acetonitrile-κN)praseodymium(III)]tris(µ- trifluoromethanesulfonato-κ²O:O')] top

Crystal data top

[Pr(CF₃O₃S)₃(C₂H₃N)₃]	Z = 2
M_r = 711.28	F(000) = 688
Triclinic, P1	D_x = 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

Data collection top

Bruker APEXII Quazar diffractometer	5251 independent reflections
Radiation source: fine-focus sealed tube	4674 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.039
Detector resolution: 66 pixels mm^-1	θ_max = 28.2°, θ_min = 1.1°
combined ω and φ scans	h = −7→7
Absorption correction: multi-scan (SADABS; Bruker, 2001)	k = −13→13
T_min = 0.578, T_max = 0.978	l = −25→24
20544 measured reflections

Refinement top

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(F_o²) + (0.0169P)² + 4.422P] where P = (F_o² + 2F_c²)/3
5251 reflections	(Δ/σ)_max = 0.001
311 parameters	Δρ_max = 1.04 e Å⁻³
0 restraints	Δρ_min = −1.15 e Å⁻³

Crystal data top

[Pr(CF₃O₃S)₃(C₂H₃N)₃]	γ = 91.695 (1)°
M_r = 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)°

Data collection top

Bruker APEXII Quazar diffractometer	5251 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2001)	4674 reflections with I > 2σ(I)
T_min = 0.578, T_max = 0.978	R_int = 0.039
20544 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	0 restraints
wR(F²) = 0.076	H-atom parameters constrained
S = 1.16	Δρ_max = 1.04 e Å⁻³
5251 reflections	Δρ_min = −1.15 e Å⁻³
311 parameters

Special details top

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

	x	y	z	U_iso*/U_eq
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)*

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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]
M_r	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)
T_min, T_max	0.578, 0.978
No. of measured, independent and observed [I > 2σ(I)] reflections	20544, 5251, 4674
R_int	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
Δρ_max, Δρ_min (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).

Selected bond lengths (Å) top

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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