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Both ions of the title compound, (C8H18N)[ZrCl5(C4H8O)], exhibit approximate Cs symmetry. The equatorial Cl atoms of the anion display an umbrella effect with significant bending towards the tetra­hydro­furan fragment, as observed before for similar anions. The cation exhibits bond lengths and angles in the expected range.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806045880/sg2085sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806045880/sg2085Isup2.hkl
Contains datablock I

CCDC reference: 630457

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.034
  • wR factor = 0.108
  • Data-to-parameter ratio = 21.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zr1 - Cl2 .. 9.63 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zr1 - Cl4 .. 6.08 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zr1 - Cl5 .. 6.81 su
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART-NT (Bruker, 2003); cell refinement: SAINT-NT (Bruker, 2003); data reduction: SAINT-NT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: XP in SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: XP in SHELXTL.

N,N-Diethylpyrrolidinium pentachloro(tetrahydrofuran)zirconate top
Crystal data top
(C8H18N)[ZrCl5(C4H8O)]F(000) = 1904.0
Mr = 468.81Dx = 1.581 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 7412 reflections
a = 15.4148 (17) Åθ = 2.6–26.1°
b = 14.9772 (17) ŵ = 1.23 mm1
c = 17.0633 (19) ÅT = 173 K
V = 3939.4 (8) Å3Block, yellow
Z = 80.35 × 0.18 × 0.14 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
3922 independent reflections
Radiation source: fine-focus sealed tube3440 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
φ and ω scansθmax = 26.2°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2000)
h = 1919
Tmin = 0.668, Tmax = 0.841k = 1818
54795 measured reflectionsl = 2121
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H-atom parameters constrained
S = 1.10 w = 1/[σ2(Fo2) + (0.0622P)2 + 4.0936P]
where P = (Fo2 + 2Fc2)/3
3922 reflections(Δ/σ)max = 0.027
183 parametersΔρmax = 1.02 e Å3
96 restraintsΔρmin = 0.52 e Å3
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
xyzUiso*/Ueq
Zr11.048908 (18)0.746204 (17)0.396971 (17)0.02940 (12)
Cl21.05252 (4)0.91068 (4)0.37741 (5)0.03458 (18)
Cl31.03538 (5)0.58741 (5)0.42745 (5)0.03987 (19)
Cl40.90238 (5)0.74390 (5)0.33967 (5)0.03805 (19)
Cl51.18131 (5)0.75453 (5)0.47640 (6)0.0460 (2)
Cl61.12565 (7)0.71663 (6)0.27546 (5)0.0560 (3)
O10.98246 (13)0.77316 (14)0.51104 (12)0.0344 (4)
C90.2038 (2)0.9009 (2)0.1561 (2)0.0429 (7)
H9A0.23200.86890.11220.051*
H9B0.21690.86770.20490.051*
N10.24286 (15)0.99312 (15)0.16222 (16)0.0328 (5)
C50.2134 (2)1.0400 (2)0.23508 (19)0.0452 (6)
H5A0.15061.03010.24390.054*
H5B0.22411.10500.23100.054*
C70.3495 (3)0.9670 (3)0.2614 (3)0.0663 (9)
H7A0.40060.99890.28260.080*
H7B0.35730.90220.27050.080*
C40.9081 (2)0.7231 (3)0.5415 (2)0.0537 (9)
H4A0.92020.65820.54070.064*
H4B0.85580.73490.50950.064*
C110.2223 (3)1.0490 (2)0.0914 (2)0.0481 (7)
H11A0.24981.10830.09790.058*
H11B0.15881.05830.08900.058*
C30.8948 (3)0.7546 (3)0.6237 (3)0.0644 (10)
H3A0.83230.75630.63700.077*
H3B0.92520.71530.66140.077*
C120.2521 (3)1.0093 (3)0.0146 (2)0.0693 (13)
H12A0.31300.99120.01910.104*
H12B0.24621.05380.02710.104*
H12C0.21650.95700.00210.104*
C100.1068 (2)0.8998 (3)0.1432 (2)0.0527 (9)
H10A0.07800.93130.18630.079*
H10B0.08630.83780.14140.079*
H10C0.09310.92940.09350.079*
C11.0060 (2)0.8434 (2)0.5671 (2)0.0503 (8)
H1A1.01240.90170.54030.060*
H1B1.06120.82880.59390.060*
C60.2659 (3)1.0001 (3)0.3011 (2)0.0621 (9)
H6A0.23440.95000.32600.075*
H6B0.27911.04560.34140.075*
C80.3392 (2)0.9859 (2)0.1753 (2)0.0508 (7)
H8A0.36410.93680.14350.061*
H8B0.36861.04240.16090.061*
C20.9327 (3)0.8457 (3)0.6240 (3)0.0703 (11)
H2A0.95380.86140.67700.084*
H2B0.88880.89030.60770.084*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zr10.02996 (19)0.02775 (18)0.03049 (19)0.00009 (10)0.00494 (10)0.00206 (10)
Cl20.0329 (4)0.0243 (3)0.0466 (4)0.0015 (2)0.0023 (3)0.0047 (3)
Cl30.0517 (4)0.0285 (3)0.0395 (4)0.0030 (3)0.0011 (3)0.0060 (3)
Cl40.0408 (4)0.0366 (4)0.0368 (4)0.0055 (3)0.0121 (3)0.0027 (3)
Cl50.0236 (3)0.0484 (4)0.0660 (5)0.0015 (3)0.0053 (3)0.0080 (4)
Cl60.0815 (6)0.0423 (4)0.0442 (4)0.0158 (4)0.0332 (4)0.0093 (3)
O10.0286 (8)0.0447 (9)0.0299 (7)0.0060 (8)0.0031 (6)0.0048 (6)
C90.0439 (14)0.0328 (12)0.0519 (19)0.0077 (11)0.0055 (14)0.0055 (10)
N10.0321 (10)0.0281 (11)0.0381 (9)0.0006 (8)0.0058 (9)0.0001 (8)
C50.0436 (15)0.0544 (17)0.0375 (11)0.0026 (13)0.0051 (11)0.0080 (11)
C70.0586 (17)0.053 (2)0.087 (2)0.0016 (16)0.0330 (15)0.002 (2)
C40.0335 (16)0.083 (2)0.0440 (16)0.0185 (14)0.0132 (12)0.0070 (15)
C110.068 (2)0.0380 (15)0.0388 (11)0.0070 (15)0.0024 (13)0.0064 (11)
C30.052 (2)0.097 (2)0.0440 (16)0.0100 (18)0.0187 (16)0.0076 (18)
C120.100 (4)0.070 (3)0.0389 (12)0.027 (3)0.0146 (19)0.0033 (16)
C100.0455 (14)0.058 (2)0.055 (2)0.0169 (14)0.0109 (16)0.0091 (17)
C10.061 (2)0.0498 (18)0.0406 (15)0.0066 (13)0.0061 (13)0.0149 (12)
C60.068 (2)0.077 (3)0.0418 (11)0.0221 (18)0.0102 (12)0.0115 (16)
C80.0311 (10)0.0449 (18)0.0765 (16)0.0019 (11)0.0051 (12)0.0086 (16)
C20.095 (3)0.0655 (19)0.0500 (19)0.0151 (18)0.0286 (18)0.0106 (15)
Geometric parameters (Å, º) top
Zr1—O12.236 (2)C4—H4A0.9900
Zr1—Cl62.4279 (8)C4—H4B0.9900
Zr1—Cl32.4434 (8)C11—C121.510 (5)
Zr1—Cl52.4532 (9)C11—H11A0.9900
Zr1—Cl42.4615 (8)C11—H11B0.9900
Zr1—Cl22.4865 (8)C3—C21.484 (6)
O1—C41.465 (4)C3—H3A0.9900
O1—C11.468 (4)C3—H3B0.9900
C9—C101.511 (5)C12—H12A0.9800
C9—N11.511 (4)C12—H12B0.9800
C9—H9A0.9900C12—H12C0.9800
C9—H9B0.9900C10—H10A0.9800
N1—C51.499 (4)C10—H10B0.9800
N1—C111.503 (4)C10—H10C0.9800
N1—C81.506 (4)C1—C21.491 (5)
C5—C61.511 (5)C1—H1A0.9900
C5—H5A0.9900C1—H1B0.9900
C5—H5B0.9900C6—H6A0.9900
C7—C81.505 (6)C6—H6B0.9900
C7—C61.537 (6)C8—H8A0.9900
C7—H7A0.9900C8—H8B0.9900
C7—H7B0.9900C2—H2A0.9900
C4—C31.492 (5)C2—H2B0.9900
O1—Zr1—Cl6178.08 (6)N1—C11—C12114.4 (3)
O1—Zr1—Cl387.21 (6)N1—C11—H11A108.7
Cl6—Zr1—Cl392.63 (3)C12—C11—H11A108.7
O1—Zr1—Cl583.74 (6)N1—C11—H11B108.7
Cl6—Zr1—Cl594.34 (4)C12—C11—H11B108.7
Cl3—Zr1—Cl590.17 (3)H11A—C11—H11B107.6
O1—Zr1—Cl485.87 (6)C2—C3—C4103.9 (4)
Cl6—Zr1—Cl496.05 (4)C2—C3—H3A111.0
Cl3—Zr1—Cl489.57 (3)C4—C3—H3A111.0
Cl5—Zr1—Cl4169.61 (3)C2—C3—H3B111.0
O1—Zr1—Cl287.03 (6)C4—C3—H3B111.0
Cl6—Zr1—Cl293.16 (3)H3A—C3—H3B109.0
Cl3—Zr1—Cl2174.14 (3)C11—C12—H12A109.5
Cl5—Zr1—Cl290.29 (3)C11—C12—H12B109.5
Cl4—Zr1—Cl288.92 (2)H12A—C12—H12B109.5
C4—O1—C1109.2 (2)C11—C12—H12C109.5
C4—O1—Zr1125.12 (19)H12A—C12—H12C109.5
C1—O1—Zr1125.68 (18)H12B—C12—H12C109.5
C10—C9—N1114.5 (3)C9—C10—H10A109.5
C10—C9—H9A108.6C9—C10—H10B109.5
N1—C9—H9A108.6H10A—C10—H10B109.5
C10—C9—H9B108.6C9—C10—H10C109.5
N1—C9—H9B108.6H10A—C10—H10C109.5
H9A—C9—H9B107.6H10B—C10—H10C109.5
C5—N1—C11110.0 (2)O1—C1—C2104.6 (3)
C5—N1—C8102.2 (3)O1—C1—H1A110.8
C11—N1—C8111.5 (3)C2—C1—H1A110.8
C5—N1—C9111.4 (3)O1—C1—H1B110.8
C11—N1—C9111.7 (3)C2—C1—H1B110.8
C8—N1—C9109.8 (2)H1A—C1—H1B108.9
N1—C5—C6105.7 (3)C5—C6—C7104.4 (3)
N1—C5—H5A110.6C5—C6—H6A110.9
C6—C5—H5A110.6C7—C6—H6A110.9
N1—C5—H5B110.6C5—C6—H6B110.9
C6—C5—H5B110.6C7—C6—H6B110.9
H5A—C5—H5B108.7H6A—C6—H6B108.9
C8—C7—C6106.3 (3)C7—C8—N1105.1 (3)
C8—C7—H7A110.5C7—C8—H8A110.7
C6—C7—H7A110.5N1—C8—H8A110.7
C8—C7—H7B110.5C7—C8—H8B110.7
C6—C7—H7B110.5N1—C8—H8B110.7
H7A—C7—H7B108.7H8A—C8—H8B108.8
O1—C4—C3106.2 (3)C3—C2—C1106.0 (3)
O1—C4—H4A110.5C3—C2—H2A110.5
C3—C4—H4A110.5C1—C2—H2A110.5
O1—C4—H4B110.5C3—C2—H2B110.5
C3—C4—H4B110.5C1—C2—H2B110.5
H4A—C4—H4B108.7H2A—C2—H2B108.7
Cl3—Zr1—O1—C441.4 (3)Zr1—O1—C4—C3171.3 (3)
Cl5—Zr1—O1—C4131.9 (3)C5—N1—C11—C12178.1 (3)
Cl4—Zr1—O1—C448.3 (3)C8—N1—C11—C1265.5 (4)
Cl2—Zr1—O1—C4137.5 (3)C9—N1—C11—C1257.7 (4)
Cl3—Zr1—O1—C1138.6 (2)O1—C4—C3—C225.2 (5)
Cl5—Zr1—O1—C148.1 (2)C4—O1—C1—C211.2 (4)
Cl4—Zr1—O1—C1131.6 (2)Zr1—O1—C1—C2168.8 (3)
Cl2—Zr1—O1—C142.5 (2)N1—C5—C6—C726.0 (4)
C10—C9—N1—C567.4 (4)C8—C7—C6—C52.2 (4)
C10—C9—N1—C1156.0 (4)C6—C7—C8—N122.1 (4)
C10—C9—N1—C8179.8 (3)C5—N1—C8—C737.8 (3)
C11—N1—C5—C6158.1 (3)C11—N1—C8—C7155.3 (3)
C8—N1—C5—C639.7 (3)C9—N1—C8—C780.4 (3)
C9—N1—C5—C677.4 (3)C4—C3—C2—C132.3 (5)
C1—O1—C4—C38.7 (4)O1—C1—C2—C327.1 (5)
 

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