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Mol­ecules of the title compound, [Li2Br2(C4H8O)4], are located on crystallographic centres of inversion with one half-mol­ecule in the asymmetric unit. The title compound is isostructural with the chloro compound.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806039626/kj2036sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806039626/kj2036Isup2.hkl
Contains datablock I

CCDC reference: 627960

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.015 Å
  • Disorder in main residue
  • R factor = 0.067
  • wR factor = 0.184
  • Data-to-parameter ratio = 19.2

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 2 PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C4
Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C13 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C14 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C15 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Li1 PLAT301_ALERT_3_C Main Residue Disorder ......................... 14.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 15 PLAT411_ALERT_2_C Short Inter H...H Contact H4A .. H15C .. 2.14 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 8 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 7 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: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97.

Di-µ-bromo-bis[(tetrahydrofuran)lithium(I)] top
Crystal data top
[Li2Br2(C4H8O)4]F(000) = 472
Mr = 462.12Dx = 1.375 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5073 reflections
a = 9.5741 (15) Åθ = 3.4–25.8°
b = 11.9446 (15) ŵ = 3.64 mm1
c = 9.8172 (14) ÅT = 173 K
β = 96.075 (12)°Plate, colourless
V = 1116.4 (3) Å30.22 × 0.14 × 0.05 mm
Z = 2
Data collection top
Stoe IPDS-II two-circle
diffractometer
2090 independent reflections
Radiation source: fine-focus sealed tube1502 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.077
ω scansθmax = 25.7°, θmin = 3.6°
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
h = 1111
Tmin = 0.501, Tmax = 0.839k = 1414
6611 measured reflectionsl = 1111
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.067H-atom parameters constrained
wR(F2) = 0.184 w = 1/[σ2(Fo2) + (0.1004P)2 + 0.2164P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
2090 reflectionsΔρmax = 0.61 e Å3
109 parametersΔρmin = 0.98 e Å3
6 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.020 (5)
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*/UeqOcc. (<1)
Br10.59790 (8)0.64572 (5)0.51736 (7)0.0699 (4)
Li10.4669 (10)0.5056 (7)0.6512 (9)0.047 (2)
O10.5907 (4)0.4568 (4)0.8063 (5)0.0654 (12)
C20.6952 (8)0.3732 (7)0.7823 (13)0.097 (3)
H2A0.67980.34430.68730.117*
H2B0.69230.30980.84680.117*
C30.8337 (9)0.4348 (8)0.8061 (14)0.109 (4)
H3A0.90940.38390.84490.130*
H3B0.86020.46680.71950.130*
C40.8092 (10)0.5242 (13)0.9042 (14)0.140 (5)
H4A0.84780.50240.99800.168*
H4B0.85540.59440.87940.168*
C50.6566 (8)0.5401 (10)0.8975 (8)0.096 (3)
H5A0.62510.53180.98980.115*
H5B0.63090.61600.86300.115*
O110.3044 (5)0.5778 (4)0.7178 (6)0.0733 (13)
C120.3070 (11)0.6968 (8)0.7474 (12)0.107 (3)
H12A0.39790.73050.72960.128*
H12B0.29110.71110.84390.128*
C130.1900 (13)0.7420 (8)0.6518 (13)0.134 (5)
H13A0.22910.78710.58020.160*0.53 (4)
H13B0.13140.79190.70280.160*0.53 (4)
H13C0.21500.74600.55660.160*0.47 (4)
H13D0.15940.81670.68070.160*0.47 (4)
C140.101 (2)0.6509 (11)0.585 (3)0.120 (9)*0.53 (4)
H14A0.10130.65180.48470.144*0.53 (4)
H14B0.00240.65700.60800.144*0.53 (4)
C150.1704 (13)0.5481 (12)0.647 (2)0.073 (5)*0.53 (4)
H15A0.11080.51370.71240.087*0.53 (4)
H15B0.18330.49280.57460.087*0.53 (4)
C14'0.0819 (17)0.6542 (12)0.668 (3)0.090 (8)*0.47 (4)
H14C0.01790.64600.58250.108*0.47 (4)
H14D0.02570.67350.74370.108*0.47 (4)
C15'0.1635 (10)0.5488 (13)0.699 (3)0.077 (6)*0.47 (4)
H15C0.13510.51360.78350.092*0.47 (4)
H15D0.14590.49500.62270.092*0.47 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br10.0971 (6)0.0545 (4)0.0597 (5)0.0344 (3)0.0154 (3)0.0092 (3)
Li10.048 (5)0.045 (5)0.047 (5)0.003 (4)0.002 (4)0.004 (4)
O10.043 (2)0.085 (3)0.065 (3)0.004 (2)0.006 (2)0.009 (2)
C20.057 (4)0.073 (5)0.154 (9)0.008 (4)0.021 (5)0.027 (5)
C30.057 (5)0.075 (5)0.193 (12)0.001 (4)0.004 (6)0.038 (7)
C40.063 (6)0.207 (15)0.143 (10)0.038 (8)0.019 (6)0.023 (10)
C50.066 (5)0.157 (9)0.061 (4)0.018 (5)0.013 (4)0.024 (5)
O110.057 (3)0.067 (3)0.098 (4)0.013 (2)0.019 (3)0.003 (3)
C120.119 (7)0.078 (6)0.132 (8)0.004 (6)0.054 (7)0.035 (6)
C130.201 (13)0.086 (7)0.115 (8)0.063 (8)0.022 (8)0.014 (6)
Geometric parameters (Å, º) top
Br1—Li1i2.485 (9)O11—C121.451 (10)
Br1—Li12.540 (9)C12—C131.484 (15)
Li1—O11.918 (10)C12—H12A0.9900
Li1—O111.951 (10)C12—H12B0.9900
Li1—Br1i2.485 (9)C13—C141.492 (10)
Li1—Li1i3.104 (18)C13—C14'1.493 (9)
O1—C51.438 (9)C13—H13A0.9900
O1—C21.451 (10)C13—H13B0.9900
C2—C31.512 (12)C13—H13C0.9900
C2—H2A0.9900C13—H13D0.9900
C2—H2B0.9900C14—C151.496 (10)
C3—C41.473 (17)C14—H14A0.9900
C3—H3A0.9900C14—H14B0.9900
C3—H3B0.9900C15—H15A0.9900
C4—C51.468 (13)C15—H15B0.9900
C4—H4A0.9900C14'—C15'1.496 (10)
C4—H4B0.9900C14'—H14C0.9900
C5—H5A0.9900C14'—H14D0.9900
C5—H5B0.9900C15'—H15C0.9900
O11—C15'1.386 (9)C15'—H15D0.9900
O11—C151.436 (9)
Li1i—Br1—Li176.3 (3)O11—C12—H12A111.1
O1—Li1—O11108.4 (5)C13—C12—H12A111.1
O1—Li1—Br1i113.4 (4)O11—C12—H12B111.1
O11—Li1—Br1i113.1 (4)C13—C12—H12B111.1
O1—Li1—Br1108.3 (4)H12A—C12—H12B109.0
O11—Li1—Br1109.7 (4)C12—C13—C14111.8 (10)
Br1i—Li1—Br1103.7 (3)C12—C13—C14'99.4 (11)
O1—Li1—Li1i125.1 (6)C12—C13—H13A109.3
O11—Li1—Li1i126.1 (6)C14—C13—H13A109.3
Br1i—Li1—Li1i52.7 (3)C12—C13—H13B109.3
Br1—Li1—Li1i51.0 (3)C14—C13—H13B109.3
C5—O1—C2108.2 (6)H13A—C13—H13B107.9
C5—O1—Li1118.5 (6)C12—C13—H13C111.9
C2—O1—Li1117.3 (6)C14—C13—H13C78.9
O1—C2—C3104.4 (7)C14'—C13—H13C111.9
O1—C2—H2A110.9C12—C13—H13D111.9
C3—C2—H2A110.9C14—C13—H13D127.5
O1—C2—H2B110.9C14'—C13—H13D111.9
C3—C2—H2B110.9H13C—C13—H13D109.6
H2A—C2—H2B108.9C13—C14—C15102.1 (12)
C4—C3—C2104.8 (9)C13—C14—H14A111.3
C4—C3—H3A110.8C15—C14—H14A111.3
C2—C3—H3A110.8C13—C14—H14B111.3
C4—C3—H3B110.8C15—C14—H14B111.3
C2—C3—H3B110.8H14A—C14—H14B109.2
H3A—C3—H3B108.9O11—C15—C14109.3 (11)
C5—C4—C3106.9 (8)O11—C15—H15A109.8
C5—C4—H4A110.3C14—C15—H15A109.8
C3—C4—H4A110.3O11—C15—H15B109.8
C5—C4—H4B110.3C14—C15—H15B109.8
C3—C4—H4B110.3H15A—C15—H15B108.3
H4A—C4—H4B108.6C13—C14'—C15'105.1 (12)
O1—C5—C4107.9 (9)C13—C14'—H14C110.7
O1—C5—H5A110.1C15'—C14'—H14C110.7
C4—C5—H5A110.1C13—C14'—H14D110.7
O1—C5—H5B110.1C15'—C14'—H14D110.7
C4—C5—H5B110.1H14C—C14'—H14D108.8
H5A—C5—H5B108.4O11—C15'—C14'107.2 (12)
C15'—O11—C12105.5 (9)O11—C15'—H15C110.3
C15—O11—C12109.5 (8)C14'—C15'—H15C110.3
C15'—O11—Li1130.2 (10)O11—C15'—H15D110.3
C15—O11—Li1115.7 (9)C14'—C15'—H15D110.3
C12—O11—Li1120.2 (5)H15C—C15'—H15D108.5
O11—C12—C13103.5 (8)
Li1i—Br1—Li1—O1120.8 (6)Br1—Li1—O11—C15105.9 (10)
Li1i—Br1—Li1—O11121.1 (6)Li1i—Li1—O11—C1550.4 (12)
Li1i—Br1—Li1—Br1i0.0O1—Li1—O11—C1288.8 (8)
O11—Li1—O1—C565.0 (7)Br1i—Li1—O11—C12144.4 (7)
Br1i—Li1—O1—C5168.4 (5)Br1—Li1—O11—C1229.2 (8)
Br1—Li1—O1—C553.9 (7)Li1i—Li1—O11—C1284.8 (9)
Li1i—Li1—O1—C5108.6 (7)C15'—O11—C12—C1340.5 (15)
O11—Li1—O1—C2162.1 (5)C15—O11—C12—C1318.6 (14)
Br1i—Li1—O1—C235.5 (7)Li1—O11—C12—C13119.0 (8)
Br1—Li1—O1—C279.0 (6)O11—C12—C13—C1411.1 (19)
Li1i—Li1—O1—C224.3 (9)O11—C12—C13—C14'42.9 (14)
C5—O1—C2—C325.6 (10)C12—C13—C14—C150 (2)
Li1—O1—C2—C3111.8 (8)C14'—C13—C14—C1573 (2)
O1—C2—C3—C427.6 (12)C15'—O11—C15—C14102 (3)
C2—C3—C4—C519.7 (13)C12—O11—C15—C1419.9 (19)
C2—O1—C5—C413.6 (11)Li1—O11—C15—C14119.8 (16)
Li1—O1—C5—C4123.1 (9)C13—C14—C15—O1112 (2)
C3—C4—C5—O14.4 (13)C12—C13—C14'—C15'30.5 (18)
O1—Li1—O11—C15'117.5 (15)C14—C13—C14'—C15'85 (2)
Br1i—Li1—O11—C15'9.2 (16)C15—O11—C15'—C14'84 (3)
Br1—Li1—O11—C15'124.5 (15)C12—O11—C15'—C14'20 (2)
Li1i—Li1—O11—C15'68.9 (17)Li1—O11—C15'—C14'136.5 (13)
O1—Li1—O11—C15136.0 (10)C13—C14'—C15'—O117 (2)
Br1i—Li1—O11—C159.3 (11)
Symmetry code: (i) x+1, y+1, z+1.
 

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