Literature DB >> 21202477

Dioxidobis(pentane-2,4-dionato-κO,O')(pyridine-4-carbaldehyde oxime-κN)uranium(VI).

Abstract

The title compound, [U(C(5)H(7)O(2))(2)O(2)(C(6)H(6)N(2)O)], exhibits a penta-gonal-bipyramidal coordination geometry around the U(VI) atom, involving two bidentate acetyl-acetonate ions and the pyridine ring of the pyridine-4-carbaldehyde oxime ligand. Hydrogen bonds exist between the OH group of the pyridine-4-carbaldehyde oxime ligand and the two O atoms of the acetyl-acetonate ions.

Entities: Chemical Disease Species

Year: 2008 PMID： 21202477 PMCID： PMC2961597 DOI： 10.1107/S1600536808012889

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

Related literature

For related literature, see: Alcock et al. (1984 ▶, 1987 ▶); Kawasaki et al. (2006 ▶); Saeki et al. (2006 ▶).

Experimental

Crystal data

[U(C5H7O2)2O2(C6H6N2O)] M = 590.37 Triclinic, a = 8.1969 (6) Å b = 11.2632 (9) Å c = 11.7448 (9) Å α = 71.016 (1)° β = 75.660 (2)° γ = 80.137 (2)° V = 988.51 (13) Å3 Z = 2 Mo Kα radiation μ = 8.25 mm−1 T = 291 K 0.20 × 0.18 × 0.15 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.289, T max = 0.371 (expected range = 0.226–0.290) 7404 measured reflections 4832 independent reflections 4538 reflections with I > 2σ(I) R int = 0.013

Refinement

R[F 2 > 2σ(F 2)] = 0.019 wR(F 2) = 0.048 S = 1.09 4832 reflections 240 parameters H-atom parameters constrained Δρmax = 0.63 e Å−3 Δρmin = −0.71 e Å−3 Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT (Bruker, 2001 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶) and CrystalMaker (CrystalMaker, 2007 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808012889/im2063sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808012889/im2063Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[U(C₅H₇O₂)₂O₂(C₆H₆N₂O)]	Z = 2
M_r = 590.37	F₀₀₀ = 556
Triclinic, P1	D_x = 1.983 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation λ = 0.71073 Å
a = 8.1969 (6) Å	Cell parameters from 5400 reflections
b = 11.2632 (9) Å	θ = 2.3–28.3º
c = 11.7448 (9) Å	µ = 8.25 mm⁻¹
α = 71.016 (1)º	T = 291 K
β = 75.660 (2)º	Block, orange
γ = 80.137 (2)º	0.20 × 0.18 × 0.15 mm
V = 988.51 (13) Å³

Bruker SMART CCD area-detector diffractometer	4832 independent reflections
Radiation source: fine-focus sealed tube	4538 reflections with I > 2σ(I)
Monochromator: graphite	R_int = 0.013
Detector resolution: 8.366 pixels mm^-1	θ_max = 28.3º
T = 291 K	θ_min = 1.9º
φ and ω scans	h = −10→9
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)	k = −14→15
T_min = 0.289, T_max = 0.371	l = −15→15
7404 measured reflections

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.019	H-atom parameters constrained
wR(F²) = 0.048	w = 1/[σ²(F_o²) + (0.018P)² + 0.4544P] where P = (F_o² + 2F_c²)/3
S = 1.09	(Δ/σ)_max = 0.016
4832 reflections	Δρ_max = 0.63 e Å⁻³
240 parameters	Δρ_min = −0.71 e Å⁻³
Primary atom site location: structure-invariant direct methods	Extinction correction: none

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
U1	0.097943 (12)	0.796870 (9)	0.824753 (9)	0.03536 (4)
O1	−0.0310 (3)	0.9423 (2)	0.7952 (2)	0.0525 (6)
O2	0.2248 (3)	0.6515 (2)	0.8605 (2)	0.0503 (5)
O3	0.3515 (3)	0.8856 (2)	0.7061 (2)	0.0499 (5)
O4	0.2204 (3)	0.8617 (2)	0.9494 (2)	0.0490 (5)
O5	0.1115 (3)	0.7877 (3)	0.6262 (2)	0.0601 (7)
O6	−0.1153 (3)	0.6784 (3)	0.8304 (2)	0.0579 (6)
O7	−0.5265 (4)	0.6725 (3)	1.5844 (2)	0.0731 (8)
H7	−0.5787	0.7280	1.6141	0.110*
N1	−0.0878 (3)	0.7423 (2)	1.0457 (2)	0.0420 (5)
N2	−0.4406 (4)	0.7272 (3)	1.4648 (3)	0.0593 (8)
C1	0.4046 (6)	0.8379 (5)	1.0811 (4)	0.0735 (12)
H1A	0.3173	0.8863	1.1233	0.110*
H1B	0.5126	0.8648	1.0740	0.110*
H1C	0.4033	0.7501	1.1266	0.110*
C2	0.3743 (4)	0.8576 (3)	0.9552 (3)	0.0470 (7)
C3	0.5049 (4)	0.8757 (4)	0.8536 (3)	0.0531 (8)
H3	0.6133	0.8728	0.8664	0.064*
C4	0.4875 (4)	0.8978 (3)	0.7336 (3)	0.0442 (7)
C5	0.6322 (5)	0.9391 (4)	0.6284 (4)	0.0598 (9)
H5A	0.6415	0.8938	0.5701	0.090*
H5B	0.7351	0.9220	0.6584	0.090*
H5C	0.6127	1.0279	0.5890	0.090*
C6	−0.2910 (7)	0.5394 (5)	0.8211 (5)	0.0811 (14)
H6A	−0.2656	0.4802	0.8959	0.122*
H6B	−0.2988	0.4946	0.7660	0.122*
H6C	−0.3968	0.5882	0.8394	0.122*
C7	−0.1524 (5)	0.6261 (3)	0.7615 (4)	0.0546 (9)
C8	−0.0769 (6)	0.6479 (4)	0.6384 (4)	0.0612 (10)
H8	−0.1122	0.6050	0.5946	0.073*
C9	0.0470 (5)	0.7286 (4)	0.5752 (3)	0.0551 (8)
C10	0.1107 (7)	0.7529 (6)	0.4392 (4)	0.0844 (14)
H10A	0.0741	0.8381	0.3971	0.127*
H10B	0.0667	0.6955	0.4119	0.127*
H10C	0.2321	0.7406	0.4216	0.127*
C11	−0.1242 (4)	0.8257 (3)	1.1105 (3)	0.0454 (7)
H11	−0.0868	0.9054	1.0725	0.054*
C12	−0.2131 (4)	0.7997 (3)	1.2294 (3)	0.0450 (7)
H12	−0.2366	0.8607	1.2704	0.054*
C13	−0.2680 (4)	0.6800 (3)	1.2880 (3)	0.0422 (6)
C14	−0.2309 (5)	0.5944 (3)	1.2224 (3)	0.0499 (8)
H14	−0.2650	0.5136	1.2590	0.060*
C15	−0.1426 (4)	0.6286 (3)	1.1019 (3)	0.0477 (7)
H15	−0.1205	0.5699	1.0582	0.057*
C16	−0.3646 (4)	0.6443 (3)	1.4146 (3)	0.0499 (7)
H16	−0.3700	0.5594	1.4585	0.060*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
U1	0.03482 (6)	0.03467 (6)	0.03998 (6)	−0.00562 (4)	−0.00817 (4)	−0.01417 (4)
O1	0.0479 (13)	0.0446 (13)	0.0623 (14)	0.0015 (10)	−0.0158 (11)	−0.0122 (11)
O2	0.0508 (13)	0.0390 (11)	0.0602 (14)	0.0021 (10)	−0.0093 (11)	−0.0185 (10)
O3	0.0451 (12)	0.0615 (14)	0.0453 (12)	−0.0194 (11)	−0.0089 (10)	−0.0120 (10)
O4	0.0425 (12)	0.0625 (14)	0.0517 (13)	−0.0112 (10)	−0.0082 (10)	−0.0279 (11)
O5	0.0639 (15)	0.0816 (19)	0.0458 (13)	−0.0301 (14)	−0.0099 (11)	−0.0229 (12)
O6	0.0551 (14)	0.0736 (17)	0.0558 (14)	−0.0292 (13)	−0.0066 (11)	−0.0255 (12)
O7	0.081 (2)	0.081 (2)	0.0483 (14)	−0.0147 (16)	0.0146 (13)	−0.0240 (14)
N1	0.0463 (14)	0.0372 (12)	0.0438 (13)	−0.0086 (11)	−0.0025 (11)	−0.0166 (10)
N2	0.0593 (18)	0.068 (2)	0.0463 (15)	−0.0052 (15)	0.0015 (13)	−0.0211 (14)
C1	0.076 (3)	0.098 (3)	0.061 (2)	−0.014 (2)	−0.027 (2)	−0.030 (2)
C2	0.0491 (18)	0.0439 (16)	0.0576 (19)	−0.0041 (14)	−0.0196 (15)	−0.0219 (14)
C3	0.0380 (16)	0.065 (2)	0.063 (2)	−0.0031 (15)	−0.0154 (15)	−0.0240 (17)
C4	0.0367 (15)	0.0370 (15)	0.0599 (19)	−0.0051 (12)	−0.0083 (13)	−0.0162 (13)
C5	0.0427 (18)	0.066 (2)	0.068 (2)	−0.0156 (16)	−0.0021 (16)	−0.0179 (19)
C6	0.088 (3)	0.074 (3)	0.092 (3)	−0.043 (3)	−0.037 (3)	−0.009 (2)
C7	0.056 (2)	0.0462 (18)	0.070 (2)	−0.0095 (15)	−0.0324 (18)	−0.0129 (16)
C8	0.081 (3)	0.060 (2)	0.059 (2)	−0.015 (2)	−0.035 (2)	−0.0203 (18)
C9	0.064 (2)	0.062 (2)	0.0488 (18)	−0.0043 (17)	−0.0251 (17)	−0.0193 (16)
C10	0.101 (4)	0.113 (4)	0.052 (2)	−0.022 (3)	−0.027 (2)	−0.028 (2)
C11	0.0494 (17)	0.0335 (14)	0.0522 (17)	−0.0071 (13)	−0.0011 (14)	−0.0168 (13)
C12	0.0470 (17)	0.0408 (16)	0.0516 (17)	−0.0059 (13)	−0.0046 (13)	−0.0230 (13)
C13	0.0398 (15)	0.0447 (16)	0.0443 (15)	−0.0046 (12)	−0.0067 (12)	−0.0174 (13)
C14	0.061 (2)	0.0338 (15)	0.0496 (17)	−0.0106 (14)	−0.0003 (15)	−0.0110 (13)
C15	0.062 (2)	0.0337 (15)	0.0469 (16)	−0.0083 (14)	0.0011 (14)	−0.0185 (13)
C16	0.0557 (19)	0.0467 (17)	0.0467 (17)	−0.0092 (15)	−0.0036 (14)	−0.0162 (14)

U1—O1	1.772 (2)	C5—H5A	0.9600
U1—O2	1.768 (2)	C5—H5B	0.9600
U1—O3	2.374 (2)	C5—H5C	0.9600
U1—O4	2.314 (2)	C6—C7	1.509 (5)
U1—O5	2.342 (2)	C6—H6A	0.9600
U1—O6	2.350 (2)	C6—H6B	0.9600
U1—N1	2.599 (3)	C6—H6C	0.9600
O3—C4	1.275 (4)	C7—C8	1.383 (6)
O4—C2	1.272 (4)	C8—C9	1.382 (6)
O5—C9	1.272 (4)	C8—H8	0.9300
O6—C7	1.260 (4)	C9—C10	1.500 (6)
O7—N2	1.394 (4)	C10—H10A	0.9600
O7—H7	0.8200	C10—H10B	0.9600
N1—C15	1.334 (4)	C10—H10C	0.9600
N1—C11	1.345 (4)	C11—C12	1.367 (4)
N2—C16	1.259 (5)	C11—H11	0.9300
C1—C2	1.499 (5)	C12—C13	1.394 (4)
C1—H1A	0.9600	C12—H12	0.9300
C1—H1B	0.9600	C13—C14	1.372 (4)
C1—H1C	0.9600	C13—C16	1.462 (4)
C2—C3	1.377 (5)	C14—C15	1.382 (5)
C3—C4	1.389 (5)	C14—H14	0.9300
C3—H3	0.9300	C15—H15	0.9300
C4—C5	1.497 (5)	C16—H16	0.9300

O1—U1—O2	177.73 (10)	C4—C5—H5A	109.5
O1—U1—O3	94.67 (10)	C4—C5—H5B	109.5
O1—U1—O4	89.96 (10)	H5A—C5—H5B	109.5
O1—U1—O5	90.77 (11)	C4—C5—H5C	109.5
O1—U1—O6	93.99 (11)	H5A—C5—H5C	109.5
O1—U1—N1	86.40 (10)	H5B—C5—H5C	109.5
O2—U1—O3	86.31 (10)	C7—C6—H6A	109.5
O2—U1—O4	88.42 (10)	C7—C6—H6B	109.5
O2—U1—O5	91.46 (11)	H6A—C6—H6B	109.5
O2—U1—O6	86.34 (11)	C7—C6—H6C	109.5
O2—U1—N1	91.57 (10)	H6A—C6—H6C	109.5
O3—U1—O4	71.32 (8)	H6B—C6—H6C	109.5
O3—U1—O5	75.30 (8)	O6—C7—C8	123.4 (3)
O3—U1—O6	145.01 (9)	O6—C7—C6	115.5 (4)
O3—U1—N1	142.48 (8)	C8—C7—C6	121.1 (3)
O4—U1—O5	146.56 (8)	C9—C8—C7	125.1 (3)
O4—U1—O6	142.51 (8)	C9—C8—H8	117.4
O4—U1—N1	71.18 (8)	C7—C8—H8	117.4
O5—U1—O6	70.74 (8)	O5—C9—C8	123.3 (3)
O5—U1—N1	142.22 (8)	O5—C9—C10	116.0 (4)
O6—U1—N1	71.89 (8)	C8—C9—C10	120.6 (3)
C4—O3—U1	133.1 (2)	C9—C10—H10A	109.5
C2—O4—U1	131.5 (2)	C9—C10—H10B	109.5
C9—O5—U1	138.1 (2)	H10A—C10—H10B	109.5
C7—O6—U1	137.8 (2)	C9—C10—H10C	109.5
N2—O7—H7	109.5	H10A—C10—H10C	109.5
C15—N1—C11	117.3 (3)	H10B—C10—H10C	109.5
C15—N1—U1	121.6 (2)	N1—C11—C12	123.6 (3)
C11—N1—U1	121.0 (2)	N1—C11—H11	118.2
C16—N2—O7	111.2 (3)	C12—C11—H11	118.2
C2—C1—H1A	109.5	C11—C12—C13	118.7 (3)
C2—C1—H1B	109.5	C11—C12—H12	120.6
H1A—C1—H1B	109.5	C13—C12—H12	120.6
C2—C1—H1C	109.5	C14—C13—C12	118.0 (3)
H1A—C1—H1C	109.5	C14—C13—C16	119.6 (3)
H1B—C1—H1C	109.5	C12—C13—C16	122.4 (3)
O4—C2—C3	123.3 (3)	C13—C14—C15	119.8 (3)
O4—C2—C1	115.3 (3)	C13—C14—H14	120.1
C3—C2—C1	121.3 (3)	C15—C14—H14	120.1
C2—C3—C4	125.1 (3)	N1—C15—C14	122.6 (3)
C2—C3—H3	117.5	N1—C15—H15	118.7
C4—C3—H3	117.5	C14—C15—H15	118.7
O3—C4—C3	123.4 (3)	N2—C16—C13	120.8 (3)
O3—C4—C5	116.4 (3)	N2—C16—H16	119.6
C3—C4—C5	120.2 (3)	C13—C16—H16	119.6

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7···O5ⁱ	0.82	2.49	3.018 (4)	123
O7—H7···O3ⁱ	0.82	2.29	3.083 (4)	163

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7⋯O5ⁱ	0.82	2.49	3.018 (4)	123
O7—H7⋯O3ⁱ	0.82	2.29	3.083 (4)	163

Symmetry code: (i) .

1 in total

1. A short history of SHELX.

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

1 in total

1. Crystal structure of dioxidobis(pentane-2,4-dionato-κ(2) O,O')[1-phenyl-3-(pyridin-4-yl)propane-κN]uranium(VI).

Authors: Takeshi Kawasaki; Takafumi Kitazawa
Journal: Acta Crystallogr E Crystallogr Commun Date: 2015-01-01

1 in total