Download citation
Download citation
link to html
The title compound, [U(C10H15)2Cl2(C2H3N)], is a bent uranium(IV) metallocene, in contrast with the recently reported linear ones that can be obtained in acetonitrile with anions less strongly coordinating than chloride. The two chloride ions in the equatorial plane are located next to each other, with the acetonitrile ligand on one side.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806040591/dn2071sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806040591/dn2071Isup2.hkl
Contains datablock I

CCDC reference: 627489

Key indicators

  • Single-crystal X-ray study
  • T = 110 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.021
  • wR factor = 0.058
  • Data-to-parameter ratio = 17.6

checkCIF/PLATON results

No syntax errors found



Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.514 0.746 Tmin and Tmax expected: 0.463 0.746 RR = 1.110 Please check that your absorption correction is appropriate. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.12 PLAT432_ALERT_2_C Short Inter X...Y Contact Cl1 .. C10 .. 3.18 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact Cl1 .. C5 .. 3.20 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact N1 .. C13 .. 2.98 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact N1 .. C12 .. 3.02 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact N1 .. C7 .. 3.04 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.40 Ratio
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: HKL-2000 (Otwinowski & Minor, 1997); data reduction: HKL-2000; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXTL (Bruker, 1999) and PLATON (Spek, 2003).

(Acetonitrile-κN)dichloro-bis(η5-pentamethylcyclopentadienyl)uranium(IV) top
Crystal data top
[UCl2(C10H15)2(C2H3N)]Z = 2
Mr = 620.42F(000) = 596
Triclinic, P1Dx = 1.800 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.6352 (4) ÅCell parameters from 54071 reflections
b = 9.4663 (6) Åθ = 3.1–25.7°
c = 14.7519 (11) ŵ = 7.33 mm1
α = 85.405 (4)°T = 110 K
β = 89.476 (5)°Platelet, translucent dark orange
γ = 72.268 (4)°0.21 × 0.09 × 0.04 mm
V = 1144.74 (13) Å3
Data collection top
Nonius Kappa-CCD area-detector
diffractometer
4339 independent reflections
Radiation source: fine-focus sealed tube4126 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
two φ and eight ω scans with 2° stepsθmax = 25.7°, θmin = 3.1°
Absorption correction: multi-scan
(SCALEPACK; Otwinowski & Minor, 1997)
h = 010
Tmin = 0.514, Tmax = 0.746k = 1011
54071 measured reflectionsl = 1717
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.021Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.058H-atom parameters constrained
S = 1.10 w = 1/[σ2(Fo2) + (0.0352P)2 + 1.5058P]
where P = (Fo2 + 2Fc2)/3
4339 reflections(Δ/σ)max = 0.002
246 parametersΔρmax = 0.80 e Å3
0 restraintsΔρmin = 1.11 e Å3
Special details top

Experimental. crystal-to-detector distance 30 mm

1H NMR of [(C5Me5)2UCl2] (acetonitrile, 296 K, δ): 12.72 (s, w1/2 = 20 Hz, C5Me5)

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
xyzUiso*/Ueq
U10.724412 (15)0.728304 (14)0.738848 (9)0.01569 (6)
Cl11.03459 (11)0.71180 (11)0.74998 (7)0.0243 (2)
Cl20.75967 (13)0.81074 (12)0.56601 (7)0.0283 (2)
N10.4460 (4)0.7816 (4)0.6600 (2)0.0231 (7)
C10.3287 (5)0.8167 (4)0.6171 (3)0.0228 (8)
C20.1809 (5)0.8640 (5)0.5611 (3)0.0309 (10)
H2A0.17540.95520.52590.046*
H2B0.08790.87950.59960.046*
H2C0.18200.78860.52110.046*
C30.6255 (5)0.4820 (4)0.7786 (3)0.0189 (8)
C40.7580 (5)0.4588 (4)0.8389 (3)0.0193 (8)
C50.9010 (5)0.4328 (4)0.7874 (3)0.0181 (8)
C60.8583 (5)0.4414 (4)0.6945 (3)0.0200 (8)
C70.6865 (5)0.4705 (4)0.6890 (3)0.0191 (8)
C80.4532 (5)0.4948 (5)0.8067 (3)0.0264 (9)
H8A0.44690.39840.82860.040*
H8B0.38090.53260.75530.040*
H8C0.42230.56140.85410.040*
C90.7555 (5)0.4326 (5)0.9410 (3)0.0253 (9)
H9A0.64960.48390.96250.038*
H9B0.83520.46930.96770.038*
H9C0.78030.32790.95770.038*
C101.0714 (5)0.3791 (5)0.8259 (3)0.0253 (9)
H10A1.07990.43720.87500.038*
H10B1.14630.38940.77920.038*
H10C1.09680.27630.84810.038*
C110.9717 (6)0.4107 (5)0.6162 (3)0.0294 (9)
H11A1.01350.30520.61170.044*
H11B1.06020.44970.62560.044*
H11C0.91420.45750.56090.044*
C120.5930 (6)0.4698 (5)0.6028 (3)0.0285 (9)
H12A0.61630.53730.55640.043*
H12B0.47860.50050.61460.043*
H12C0.62500.37120.58260.043*
C130.4792 (5)0.9322 (4)0.8255 (3)0.0235 (8)
C140.5977 (5)0.8661 (4)0.8942 (3)0.0222 (8)
C150.7387 (5)0.9096 (4)0.8737 (3)0.0211 (8)
C160.7048 (5)1.0027 (4)0.7904 (3)0.0217 (8)
C170.5443 (5)1.0170 (4)0.7613 (3)0.0220 (8)
C180.3060 (5)0.9308 (5)0.8311 (3)0.0313 (10)
H18A0.30330.82990.83530.047*
H18B0.24690.98360.77760.047*
H18C0.25700.97810.88390.047*
C190.5676 (6)0.7902 (5)0.9838 (3)0.0291 (9)
H19A0.51600.86411.02460.044*
H19B0.66930.72811.01000.044*
H19C0.49830.73040.97380.044*
C200.8851 (5)0.8804 (5)0.9341 (3)0.0312 (10)
H20A0.86600.95600.97610.047*
H20B0.97760.88150.89780.047*
H20C0.90570.78480.96720.047*
C210.8147 (6)1.0827 (5)0.7458 (3)0.0295 (10)
H21A0.79551.09480.68120.044*
H21B0.92601.02580.75870.044*
H21C0.79291.17870.76890.044*
C220.4579 (6)1.1169 (5)0.6803 (3)0.0308 (10)
H22A0.44831.21840.68950.046*
H22B0.35161.10660.67340.046*
H22C0.51921.08910.62640.046*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
U10.01395 (9)0.01421 (8)0.01850 (9)0.00363 (6)0.00022 (5)0.00158 (5)
Cl10.0159 (5)0.0222 (5)0.0351 (5)0.0063 (4)0.0005 (4)0.0019 (4)
Cl20.0291 (5)0.0322 (5)0.0224 (5)0.0094 (4)0.0015 (4)0.0038 (4)
N10.0209 (18)0.0209 (17)0.0249 (18)0.0022 (14)0.0028 (15)0.0024 (14)
C10.028 (2)0.0188 (19)0.022 (2)0.0083 (17)0.0059 (17)0.0023 (16)
C20.020 (2)0.037 (2)0.033 (2)0.0069 (18)0.0061 (17)0.0046 (19)
C30.0175 (19)0.0150 (18)0.025 (2)0.0066 (15)0.0001 (15)0.0005 (15)
C40.024 (2)0.0182 (18)0.0169 (19)0.0077 (15)0.0021 (15)0.0029 (15)
C50.0159 (19)0.0127 (17)0.024 (2)0.0023 (14)0.0006 (15)0.0015 (15)
C60.022 (2)0.0160 (18)0.022 (2)0.0050 (15)0.0062 (16)0.0032 (15)
C70.019 (2)0.0153 (18)0.021 (2)0.0033 (15)0.0046 (15)0.0003 (15)
C80.018 (2)0.027 (2)0.035 (2)0.0104 (17)0.0007 (17)0.0022 (18)
C90.028 (2)0.025 (2)0.021 (2)0.0058 (17)0.0003 (16)0.0028 (16)
C100.016 (2)0.025 (2)0.033 (2)0.0030 (16)0.0027 (16)0.0014 (17)
C110.034 (2)0.028 (2)0.024 (2)0.0049 (18)0.0089 (18)0.0041 (17)
C120.033 (2)0.023 (2)0.028 (2)0.0073 (18)0.0085 (18)0.0031 (17)
C130.021 (2)0.022 (2)0.030 (2)0.0070 (16)0.0027 (16)0.0095 (17)
C140.025 (2)0.0198 (19)0.022 (2)0.0070 (16)0.0054 (16)0.0060 (16)
C150.021 (2)0.0171 (19)0.024 (2)0.0039 (15)0.0025 (16)0.0063 (15)
C160.022 (2)0.0150 (18)0.027 (2)0.0036 (16)0.0001 (16)0.0049 (16)
C170.021 (2)0.0158 (18)0.028 (2)0.0033 (15)0.0001 (16)0.0052 (16)
C180.017 (2)0.035 (2)0.042 (3)0.0051 (18)0.0056 (18)0.013 (2)
C190.040 (3)0.023 (2)0.024 (2)0.0092 (19)0.0098 (18)0.0068 (17)
C200.026 (2)0.040 (3)0.028 (2)0.0096 (19)0.0019 (18)0.0060 (19)
C210.033 (2)0.021 (2)0.037 (3)0.0121 (18)0.0050 (19)0.0038 (18)
C220.031 (2)0.021 (2)0.037 (3)0.0029 (18)0.0059 (19)0.0001 (18)
Geometric parameters (Å, º) top
U1—Cl12.6410 (9)C10—H10A0.9600
U1—Cl22.6484 (10)C10—H10B0.9600
U1—N12.570 (3)C10—H10C0.9600
U1—C32.738 (4)C11—H11A0.9600
U1—C42.779 (4)C11—H11B0.9600
U1—C52.787 (4)C11—H11C0.9600
U1—C62.739 (4)C12—H12A0.9600
U1—C72.717 (4)C12—H12B0.9600
U1—C132.775 (4)C12—H12C0.9600
U1—C142.777 (4)C13—C141.411 (6)
U1—C152.756 (4)C13—C171.415 (6)
U1—C162.720 (4)C13—C181.501 (6)
U1—C172.747 (4)C14—C151.422 (6)
N1—C11.144 (5)C14—C191.513 (6)
C1—C21.457 (6)C15—C161.430 (6)
C2—H2A0.9600C15—C201.496 (6)
C2—H2B0.9600C16—C171.418 (6)
C2—H2C0.9600C16—C211.502 (6)
C3—C41.409 (5)C17—C221.512 (6)
C3—C71.418 (6)C18—H18A0.9600
C3—C81.513 (5)C18—H18B0.9600
C4—C51.412 (5)C18—H18C0.9600
C4—C91.507 (5)C19—H19A0.9600
C5—C61.411 (6)C19—H19B0.9600
C5—C101.504 (5)C19—H19C0.9600
C6—C71.426 (6)C20—H20A0.9600
C6—C111.497 (5)C20—H20B0.9600
C7—C121.514 (6)C20—H20C0.9600
C8—H8A0.9600C21—H21A0.9600
C8—H8B0.9600C21—H21B0.9600
C8—H8C0.9600C21—H21C0.9600
C9—H9A0.9600C22—H22A0.9600
C9—H9B0.9600C22—H22B0.9600
C9—H9C0.9600C22—H22C0.9600
Cl1—U1—Cl282.80 (3)C10—C5—U1125.7 (3)
Cl2—U1—N173.10 (8)C5—C6—C7107.4 (3)
Cl1—U1—N1155.87 (8)C5—C6—C11127.0 (4)
U1—N1—C1171.3 (3)C7—C6—C11125.3 (4)
N1—C1—C2178.6 (5)C5—C6—U177.1 (2)
N1—U1—C770.21 (11)C7—C6—U174.0 (2)
Cl1—U1—C7111.53 (8)C11—C6—U1119.4 (3)
Cl2—U1—C789.80 (9)C3—C7—C6107.9 (3)
N1—U1—C16100.89 (11)C3—C7—C12127.2 (4)
Cl1—U1—C1678.47 (9)C6—C7—C12124.5 (4)
Cl2—U1—C1691.92 (9)C3—C7—U175.7 (2)
C7—U1—C16169.99 (12)C6—C7—U175.7 (2)
N1—U1—C373.41 (11)C12—C7—U1120.3 (3)
Cl1—U1—C3120.91 (8)C3—C8—H8A109.5
Cl2—U1—C3118.50 (9)C3—C8—H8B109.5
C7—U1—C330.14 (12)H8A—C8—H8B109.5
C16—U1—C3144.29 (12)C3—C8—H8C109.5
N1—U1—C698.12 (11)H8A—C8—H8C109.5
Cl1—U1—C681.25 (9)H8B—C8—H8C109.5
Cl2—U1—C686.78 (9)C4—C9—H9A109.5
C7—U1—C630.29 (12)C4—C9—H9B109.5
C16—U1—C6159.68 (13)H9A—C9—H9B109.5
C3—U1—C649.65 (11)C4—C9—H9C109.5
N1—U1—C1771.32 (11)H9A—C9—H9C109.5
Cl1—U1—C17107.63 (9)H9B—C9—H9C109.5
Cl2—U1—C1788.44 (9)C5—C10—H10A109.5
C7—U1—C17140.24 (12)C5—C10—H10B109.5
C16—U1—C1730.06 (12)H10A—C10—H10B109.5
C3—U1—C17125.82 (12)C5—C10—H10C109.5
C6—U1—C17169.31 (12)H10A—C10—H10C109.5
N1—U1—C15116.00 (11)H10B—C10—H10C109.5
Cl1—U1—C1575.44 (9)C6—C11—H11A109.5
Cl2—U1—C15120.73 (9)C6—C11—H11B109.5
C7—U1—C15149.47 (12)H11A—C11—H11B109.5
C16—U1—C1530.27 (12)C6—C11—H11C109.5
C3—U1—C15120.07 (12)H11A—C11—H11C109.5
C6—U1—C15140.44 (12)H11B—C11—H11C109.5
C17—U1—C1549.67 (12)C7—C12—H12A109.5
N1—U1—C1367.70 (11)C7—C12—H12B109.5
Cl1—U1—C13123.54 (9)H12A—C12—H12B109.5
Cl2—U1—C13113.96 (9)C7—C12—H12C109.5
C7—U1—C13121.41 (12)H12A—C12—H12C109.5
C16—U1—C1349.14 (12)H12B—C12—H12C109.5
C3—U1—C1398.40 (12)C14—C13—C17108.5 (4)
C6—U1—C13148.06 (12)C14—C13—C18123.7 (4)
C17—U1—C1329.68 (12)C17—C13—C18127.0 (4)
C15—U1—C1349.11 (12)C14—C13—U175.4 (2)
N1—U1—C1494.55 (11)C17—C13—U174.0 (2)
Cl1—U1—C14102.59 (9)C18—C13—U1124.6 (3)
Cl2—U1—C14137.09 (9)C13—C14—C15108.5 (4)
C7—U1—C14125.22 (12)C13—C14—C19125.3 (4)
C16—U1—C1449.26 (12)C15—C14—C19125.0 (4)
C3—U1—C1495.41 (12)C13—C14—U175.2 (2)
C6—U1—C14136.08 (12)C15—C14—U174.3 (2)
C17—U1—C1449.06 (12)C19—C14—U1126.5 (3)
C15—U1—C1429.77 (12)C14—C15—C16106.9 (4)
C13—U1—C1429.45 (12)C14—C15—C20126.1 (4)
N1—U1—C4102.34 (11)C16—C15—C20126.5 (4)
Cl1—U1—C495.42 (8)C14—C15—U175.9 (2)
Cl2—U1—C4135.21 (8)C16—C15—U173.5 (2)
C7—U1—C449.16 (11)C20—C15—U1122.4 (3)
C16—U1—C4131.78 (12)C17—C16—C15108.5 (4)
C3—U1—C429.57 (11)C17—C16—C21125.6 (4)
C6—U1—C449.07 (11)C15—C16—C21125.8 (4)
C17—U1—C4133.43 (12)C17—C16—U176.0 (2)
C15—U1—C4101.64 (11)C15—C16—U176.3 (2)
C13—U1—C4104.20 (12)C21—C16—U1118.3 (3)
C14—U1—C487.17 (11)C13—C17—C16107.6 (4)
N1—U1—C5118.06 (11)C13—C17—C22127.6 (4)
Cl1—U1—C572.14 (8)C16—C17—C22124.6 (4)
Cl2—U1—C5112.78 (8)C13—C17—U176.3 (2)
C7—U1—C549.07 (11)C16—C17—U173.9 (2)
C16—U1—C5138.10 (12)C22—C17—U1119.7 (3)
C3—U1—C548.82 (11)C13—C18—H18A109.5
C6—U1—C529.58 (12)C13—C18—H18B109.5
C17—U1—C5158.26 (12)H18A—C18—H18B109.5
C15—U1—C5111.51 (12)C13—C18—H18C109.5
C13—U1—C5132.11 (12)H18A—C18—H18C109.5
C14—U1—C5109.28 (12)H18B—C18—H18C109.5
C4—U1—C529.38 (11)C14—C19—H19A109.5
C1—C2—H2A109.5C14—C19—H19B109.5
C1—C2—H2B109.5H19A—C19—H19B109.5
H2A—C2—H2B109.5C14—C19—H19C109.5
C1—C2—H2C109.5H19A—C19—H19C109.5
H2A—C2—H2C109.5H19B—C19—H19C109.5
H2B—C2—H2C109.5C15—C20—H20A109.5
C4—C3—C7108.0 (3)C15—C20—H20B109.5
C4—C3—C8125.1 (4)H20A—C20—H20B109.5
C7—C3—C8126.4 (4)C15—C20—H20C109.5
C4—C3—U176.9 (2)H20A—C20—H20C109.5
C7—C3—U174.1 (2)H20B—C20—H20C109.5
C8—C3—U1121.7 (3)C16—C21—H21A109.5
C3—C4—C5108.1 (3)C16—C21—H21B109.5
C3—C4—C9126.3 (4)H21A—C21—H21B109.5
C5—C4—C9124.3 (4)C16—C21—H21C109.5
C3—C4—U173.6 (2)H21A—C21—H21C109.5
C5—C4—U175.6 (2)H21B—C21—H21C109.5
C9—C4—U1126.8 (3)C17—C22—H22A109.5
C6—C5—C4108.6 (3)C17—C22—H22B109.5
C6—C5—C10125.4 (4)H22A—C22—H22B109.5
C4—C5—C10125.2 (4)C17—C22—H22C109.5
C6—C5—U173.3 (2)H22A—C22—H22C109.5
C4—C5—U175.0 (2)H22B—C22—H22C109.5
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C21—H21C···CG1i0.962.573.458 (4)155
C19—H19A···CG2ii0.962.923.868 (4)171
Symmetry codes: (i) x, y+1, z; (ii) x+1, y+2, z+2.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds