Literature DB >> 23476322

catena-Poly[[tris-(acetonitrile-κN)praseodymium(III)]tris-(μ-trifluoro-methane-sulfonato-κ(2) O:O')].

Abstract

In the colourless title compound, [Pr(CF3O3S)3(CH3CN)3] n , the three trifluoro-methane-sulfonate 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.

Entities: Chemical Disease Gene

Year: 2012 PMID： 23476322 PMCID： PMC3588273 DOI： 10.1107/S1600536812049525

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For the isostructural EuIII and UIII compounds, see: Tang et al. (2011 ▶) and Natrajan et al. (2005 ▶), respectively.

Experimental

Crystal data

[Pr(CF3O3S)3(C2H3N)3] M = 711.28 Triclinic, 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[F 2 > 2σ(F 2)] = 0.036 wR(F 2) = 0.076 S = 1.16 5251 reflections 311 parameters H-atom parameters constrained Δρmax = 1.04 e Å−3 Δρmin = −1.15 e Å−3 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 ▶). Click here for additional data file. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812049525/vn2063sup1.cif Click here for additional data file. Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812049525/vn2063Isup2.hkl Click here for additional data file. Supplementary material file. DOI: 10.1107/S1600536812049525/vn2063Isup3.mol Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[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

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 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

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	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)*

	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

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) .

2 in total

1. A short history of SHELX.

Authors: George M Sheldrick
Journal: Acta Crystallogr A Date: 2007-12-21 Impact factor: 2.290

2. Practical synthetic routes to solvates of U(OTf)3: X-ray crystal structure of [U(OTf)3(MeCN)3]n, a unique U(III) coordination polymer.

Authors: Louise Natrajan; Marinella Mazzanti; Jean-Philippe Bezombes; Jacques Pécaut
Journal: Inorg Chem Date: 2005-08-22 Impact factor: 5.165

2 in total