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In the title compound, tetrakis­(tetra­hydro­furan)­lithium(I) tri-[mu]-phenyl­thiol­ato-bis­[tris­(phenyl­thiol­ato)­titanate(IV)], [Li(C4H8O)4][Ti2(C6H5S)9], (I), the central structural motif of the [Ti2(SC6H5)9]- anion features a face-sharing bi-octa­hedron. The charge is balanced with a [Li(C4H8O)4]+ cation. The asymmetric unit contains Ti, Li and a heavily disordered tetra­hydro­furan mol­ecule on a threefold axis, and two terminal and a bridging thio­phenolate moiety and a slightly disordered tetra­hydro­furan mol­ecule on general positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100014979/qa0422sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100014979/qa0422Isup2.hkl
Contains datablock I

CCDC reference: 156188

Comment top

NO COMMENT

Experimental top

Mixing TiCl4.2THF with LiSPh in a 1:6 stoichiometry in diethyl ether and storing the filtered solution at 263 K afforded black crystals of the title compound in low isolated yield.

Computing details top

Data collection: CAD-4 Operations Manual (Enraf-Nonius, 1977); cell refinement: CAD-4 Operations Manual; data reduction: PROCESS MolEN (Fair, 1990); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).

(I) top
Crystal data top
[Li(C4H8O)4][Ti2(C6H5S)9]Mo Kα radiation, λ = 0.71073 Å
Mr = 1372.91Cell parameters from 25 reflections
Cubic, P213θ = 7.4–8.3°
a = 19.096 (3) ŵ = 0.55 mm1
V = 6963.9 (19) Å3T = 120 K
Z = 4Block, black
F(000) = 28800.30 × 0.25 × 0.20 mm
Dx = 1.300 Mg m3
Data collection top
Enraf-Nonius CAD-4
diffractometer
Rint = 0.000
Graphite monochromatorθmax = 26.1°, θmin = 1.5°
θ/2θ scansh = 023
Absorption correction: ψ scan
(North et al., 1968)
k = 023
Tmin = 0.885, Tmax = 0.897l = 023
2511 measured reflections3 standard reflections every 50 min
2511 independent reflections intensity decay: 0.1%
1802 reflections with I > 2σ(I)
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)] = 0.046H-atom parameters constrained
wR(F2) = 0.127 w = 1/[σ2(Fo2) + (0.0892P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max = 0.022
2511 reflectionsΔρmax = 0.57 e Å3
251 parametersΔρmin = 0.27 e Å3
36 restraintsAbsolute structure: Flack (1983), no Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.05 (7)
Crystal data top
[Li(C4H8O)4][Ti2(C6H5S)9]Z = 4
Mr = 1372.91Mo Kα radiation
Cubic, P213µ = 0.55 mm1
a = 19.096 (3) ÅT = 120 K
V = 6963.9 (19) Å30.30 × 0.25 × 0.20 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
1802 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.000
Tmin = 0.885, Tmax = 0.8973 standard reflections every 50 min
2511 measured reflections intensity decay: 0.1%
2511 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.046H-atom parameters constrained
wR(F2) = 0.127Δρmax = 0.57 e Å3
S = 0.98Δρmin = 0.27 e Å3
2511 reflectionsAbsolute structure: Flack (1983), no Friedel pairs
251 parametersAbsolute structure parameter: 0.05 (7)
36 restraints
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)
Ti10.38661 (5)0.11339 (5)0.88661 (5)0.0477 (4)
Ti20.49381 (4)0.00619 (4)0.99381 (4)0.0413 (3)
S10.28124 (8)0.07822 (9)0.83549 (8)0.0618 (4)
S20.50131 (7)0.13194 (6)0.95058 (7)0.0461 (3)
S30.59641 (7)0.03528 (7)0.94316 (7)0.0525 (3)
C10.2171 (3)0.0403 (3)0.8905 (3)0.0574 (14)
C20.2016 (3)0.0655 (3)0.9556 (4)0.0632 (15)
H2A0.22570.10400.97300.076*
C30.1509 (3)0.0343 (4)0.9952 (4)0.0772 (19)
H3A0.14120.05161.03970.093*
C40.1136 (4)0.0229 (4)0.9699 (5)0.084 (2)
H4A0.07980.04450.99760.101*
C50.1275 (4)0.0475 (4)0.9026 (4)0.0769 (19)
H5A0.10190.08460.88410.092*
C60.1797 (3)0.0163 (3)0.8638 (4)0.0685 (16)
H6A0.19010.03320.81930.082*
C70.5771 (3)0.1514 (3)0.9002 (3)0.0493 (12)
C80.6192 (3)0.2057 (3)0.9230 (3)0.0608 (14)
H8A0.60560.23200.96170.073*
C90.6816 (3)0.2216 (3)0.8890 (4)0.0696 (17)
H9A0.70940.25830.90490.083*
C100.7017 (3)0.1834 (4)0.8328 (4)0.0700 (18)
H10A0.74400.19280.81050.084*
C110.6592 (3)0.1310 (4)0.8094 (3)0.0640 (16)
H11A0.67290.10530.77040.077*
C120.5967 (3)0.1150 (3)0.8414 (3)0.0578 (14)
H12A0.56810.08000.82340.069*
C130.6659 (3)0.0333 (3)1.0036 (3)0.0587 (14)
C140.6881 (4)0.0919 (5)1.0352 (4)0.091 (2)
H14A0.66680.13461.02570.109*
C150.7462 (5)0.0878 (6)1.0848 (5)0.110 (3)
H15A0.76100.12721.10930.132*
C160.7774 (4)0.0265 (6)1.0940 (5)0.104 (3)
H16A0.81500.02391.12480.125*
C170.7577 (4)0.0301 (5)1.0620 (4)0.086 (2)
H17A0.78130.07201.07030.104*
C180.7024 (3)0.0289 (4)1.0159 (4)0.0703 (17)
H18A0.68930.06970.99280.084*
Li10.8070 (7)0.1930 (7)0.8070 (7)0.078 (5)*
O10.7208 (6)0.1396 (6)0.7979 (7)0.082 (4)*0.50
C210.6628 (10)0.1808 (10)0.7719 (14)0.121 (7)*0.50
H21A0.67060.19210.72300.145*0.50
H21B0.65980.22430.79800.145*0.50
C220.6049 (9)0.1463 (9)0.7784 (9)0.176 (6)*0.50
H22A0.59080.14040.82680.211*0.50
H22B0.56690.16640.75130.211*0.50
C230.6347 (7)0.0778 (7)0.7453 (8)0.076 (4)*0.50
H23A0.64090.08290.69510.091*0.50
H23B0.60390.03840.75420.091*0.50
C240.7055 (7)0.0681 (7)0.7823 (8)0.079 (4)*0.50
H24A0.74030.04760.75160.094*0.50
H24B0.70110.04000.82440.094*0.50
O1A0.7204 (7)0.1589 (8)0.7790 (8)0.098 (5)*0.50
C21A0.6583 (7)0.1818 (8)0.8163 (9)0.079 (4)*0.50
H21C0.65260.23220.81390.095*0.50
H21D0.65940.16740.86500.095*0.50
C22A0.6049 (9)0.1463 (9)0.7784 (9)0.176 (6)*0.50
H22C0.56760.17940.76880.211*0.50
H22D0.58570.11000.80820.211*0.50
C23A0.6235 (9)0.1180 (10)0.7198 (9)0.095 (5)*0.50
H23C0.61150.06860.71940.114*0.50
H23D0.60030.14080.68080.114*0.50
C24A0.6963 (12)0.1267 (16)0.7151 (14)0.160 (10)*0.50
H24C0.71890.08160.70880.192*0.50
H24D0.70780.15610.67540.192*0.50
O2A0.8842 (7)0.1439 (10)0.8539 (10)0.082 (5)*0.33
C310.9383 (19)0.118 (3)0.901 (2)0.265 (18)*0.33
H31A0.91940.09090.93910.318*0.33
H31B0.96760.15560.91870.318*0.33
C320.972 (3)0.078 (3)0.853 (3)0.265 (18)*0.33
H32A1.01430.05720.87210.318*0.33
H32B0.94220.04140.83440.318*0.33
C330.989 (2)0.134 (4)0.797 (3)0.265 (18)*0.33
H33A0.99940.11260.75180.318*0.33
H33B1.02770.16340.81100.318*0.33
C340.930 (2)0.167 (3)0.796 (2)0.265 (18)*0.33
H34A0.93840.21720.80090.318*0.33
H34B0.90620.15960.75190.318*0.33
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti10.0477 (4)0.0477 (4)0.0477 (4)0.0015 (4)0.0015 (4)0.0015 (4)
Ti20.0413 (3)0.0413 (3)0.0413 (3)0.0006 (4)0.0006 (4)0.0006 (4)
S10.0502 (8)0.0751 (10)0.0602 (9)0.0004 (7)0.0082 (7)0.0007 (7)
S20.0480 (7)0.0435 (6)0.0469 (6)0.0024 (6)0.0007 (6)0.0013 (5)
S30.0489 (7)0.0551 (8)0.0536 (8)0.0033 (6)0.0045 (6)0.0030 (6)
C10.042 (3)0.064 (3)0.066 (3)0.005 (3)0.006 (3)0.001 (3)
C20.043 (3)0.071 (4)0.076 (4)0.011 (3)0.004 (3)0.001 (3)
C30.053 (3)0.092 (5)0.086 (5)0.017 (3)0.014 (4)0.002 (4)
C40.053 (4)0.086 (5)0.114 (6)0.002 (3)0.012 (4)0.018 (4)
C50.068 (4)0.059 (4)0.104 (5)0.007 (3)0.007 (4)0.003 (4)
C60.058 (3)0.067 (4)0.081 (4)0.008 (3)0.007 (3)0.013 (3)
C70.050 (3)0.050 (3)0.049 (3)0.004 (2)0.003 (2)0.011 (2)
C80.057 (3)0.056 (3)0.070 (4)0.006 (3)0.002 (3)0.002 (3)
C90.061 (4)0.064 (4)0.084 (4)0.017 (3)0.010 (3)0.013 (4)
C100.053 (3)0.082 (4)0.075 (4)0.004 (3)0.010 (3)0.028 (4)
C110.064 (4)0.073 (4)0.056 (3)0.005 (3)0.003 (3)0.013 (3)
C120.059 (3)0.065 (3)0.050 (3)0.003 (3)0.000 (3)0.012 (3)
C130.044 (3)0.070 (4)0.062 (3)0.011 (3)0.004 (3)0.000 (3)
C140.074 (4)0.105 (6)0.093 (6)0.012 (4)0.001 (4)0.021 (5)
C150.079 (5)0.135 (8)0.117 (7)0.042 (6)0.004 (5)0.045 (6)
C160.061 (5)0.130 (8)0.120 (7)0.008 (5)0.018 (5)0.012 (6)
C170.058 (4)0.110 (6)0.090 (5)0.003 (4)0.014 (4)0.002 (5)
C180.053 (3)0.085 (4)0.074 (4)0.009 (3)0.003 (3)0.008 (3)
Geometric parameters (Å, º) top
Ti1—S1i2.3351 (17)C14—C151.462 (13)
Ti1—S1ii2.3351 (17)C15—C161.325 (14)
Ti1—S12.3351 (17)C16—C171.298 (13)
Ti1—S22.5329 (17)C17—C181.374 (10)
Ti1—S2ii2.5330 (17)Li1—O1A1.856 (17)
Ti1—S2i2.5330 (17)Li1—O1Aiii1.856 (17)
Ti2—S3i2.3240 (15)Li1—O1Aiv1.856 (17)
Ti2—S32.3240 (15)Li1—O1iii1.944 (13)
Ti2—S3ii2.3241 (15)Li1—O11.944 (13)
Ti2—S2ii2.5434 (16)Li1—O1iv1.944 (13)
Ti2—S22.5435 (16)Li1—O2Aiv1.96 (3)
Ti2—S2i2.5435 (16)Li1—O2A1.96 (3)
S1—C11.770 (6)Li1—O2Aiii1.96 (3)
S2—C71.778 (5)Li1—C34iv2.40 (4)
S3—C131.759 (6)Li1—C342.40 (4)
C1—C21.365 (9)Li1—C34iii2.40 (4)
C1—C61.392 (9)O1—C241.428 (14)
C2—C31.365 (9)O1—C211.446 (16)
C3—C41.392 (11)C21—C221.29 (2)
C4—C51.394 (11)C22—C231.56 (2)
C5—C61.378 (10)C23—C241.536 (19)
C7—C121.373 (8)O1A—C24A1.44 (2)
C7—C81.382 (8)O1A—C21A1.452 (18)
C8—C91.391 (9)C23A—C24A1.40 (2)
C9—C101.353 (10)O2A—C311.452 (19)
C10—C111.365 (10)O2A—C341.471 (19)
C11—C121.375 (8)C31—C321.36 (4)
C13—C141.341 (10)C32—C331.54 (4)
C13—C181.397 (9)C33—C341.31 (4)
S1i—Ti1—S1ii90.46 (7)O1—Li1—O1iv114.5 (6)
S1i—Ti1—S190.45 (7)O1A—Li1—O2Aiv106.3 (9)
S1ii—Ti1—S190.45 (7)O1Aiii—Li1—O2Aiv118.8 (11)
S1i—Ti1—S296.22 (5)O1Aiv—Li1—O2Aiv129.3 (10)
S1ii—Ti1—S295.87 (5)O1iii—Li1—O2Aiv103.4 (10)
S1—Ti1—S2170.75 (7)O1—Li1—O2Aiv92.0 (8)
S1i—Ti1—S2ii95.87 (5)O1iv—Li1—O2Aiv115.2 (10)
S1ii—Ti1—S2ii170.75 (7)O1A—Li1—O2A129.3 (11)
S1—Ti1—S2ii96.22 (5)O1Aiii—Li1—O2A106.3 (9)
S2—Ti1—S2ii76.78 (6)O1Aiv—Li1—O2A118.8 (11)
S1i—Ti1—S2i170.75 (7)O1iii—Li1—O2A92.0 (8)
S1ii—Ti1—S2i96.22 (5)O1—Li1—O2A115.2 (10)
S1—Ti1—S2i95.87 (5)O1iv—Li1—O2A103.4 (10)
S2—Ti1—S2i76.78 (6)O2Aiv—Li1—O2A23.2 (7)
S2ii—Ti1—S2i76.78 (6)O1A—Li1—O2Aiii118.8 (11)
S3i—Ti2—S3101.86 (6)O1Aiii—Li1—O2Aiii129.3 (11)
S3i—Ti2—S3ii101.85 (6)O1Aiv—Li1—O2Aiii106.3 (9)
S3—Ti2—S3ii101.86 (6)O1iii—Li1—O2Aiii115.2 (10)
S3i—Ti2—S2ii158.44 (7)O1—Li1—O2Aiii103.4 (10)
S3—Ti2—S2ii82.04 (5)O1iv—Li1—O2Aiii92.0 (8)
S3ii—Ti2—S2ii97.99 (5)O2Aiv—Li1—O2Aiii23.2 (7)
S3i—Ti2—S282.04 (5)O2A—Li1—O2Aiii23.2 (7)
S3—Ti2—S298.00 (5)O1A—Li1—C34iv68.9 (9)
S3ii—Ti2—S2158.43 (7)O1Aiii—Li1—C34iv119.5 (19)
S2ii—Ti2—S276.41 (6)O1Aiv—Li1—C34iv140.6 (19)
S3i—Ti2—S2i98.00 (5)O1iii—Li1—C34iv107.7 (19)
S3—Ti2—S2i158.43 (7)O1—Li1—C34iv55.6 (10)
S3ii—Ti2—S2i82.04 (5)O1iv—Li1—C34iv135.4 (18)
S2ii—Ti2—S2i76.41 (6)O2Aiv—Li1—C34iv37.7 (8)
S2—Ti2—S2i76.41 (6)O2A—Li1—C34iv60.4 (11)
C1—S1—Ti1117.8 (2)O2Aiii—Li1—C34iv56.2 (12)
C7—S2—Ti1118.21 (18)O1A—Li1—C34140.6 (19)
C7—S2—Ti2114.77 (18)O1Aiii—Li1—C3468.9 (9)
Ti1—S2—Ti288.61 (5)O1Aiv—Li1—C34119.5 (19)
C13—S3—Ti2110.84 (19)O1iii—Li1—C3455.6 (10)
C2—C1—C6119.8 (6)O1—Li1—C34135.4 (18)
C2—C1—S1123.1 (5)O1iv—Li1—C34107.7 (19)
C6—C1—S1117.0 (5)O2Aiv—Li1—C3456.2 (12)
C1—C2—C3120.2 (6)O2A—Li1—C3437.7 (8)
C2—C3—C4120.9 (7)O2Aiii—Li1—C3460.4 (11)
C3—C4—C5119.1 (7)C34iv—Li1—C3484.4 (12)
C6—C5—C4119.3 (7)O1A—Li1—C34iii119.5 (19)
C5—C6—C1120.6 (6)O1Aiii—Li1—C34iii140.6 (19)
C12—C7—C8118.7 (5)O1Aiv—Li1—C34iii68.9 (9)
C12—C7—S2124.0 (4)O1iii—Li1—C34iii135.4 (18)
C8—C7—S2117.4 (4)O1—Li1—C34iii107.7 (19)
C7—C8—C9121.0 (6)O1iv—Li1—C34iii55.6 (10)
C10—C9—C8119.8 (6)O2Aiv—Li1—C34iii60.4 (11)
C9—C10—C11119.1 (6)O2A—Li1—C34iii56.2 (12)
C10—C11—C12122.2 (6)O2Aiii—Li1—C34iii37.7 (8)
C7—C12—C11119.2 (6)C34iv—Li1—C34iii84.4 (12)
C14—C13—C18118.4 (6)C34—Li1—C34iii84.4 (12)
C14—C13—S3121.0 (6)C24—O1—C21106.9 (12)
C18—C13—S3120.4 (5)C24—O1—Li1133.9 (10)
C13—C14—C15119.1 (9)C21—O1—Li1113.2 (13)
C16—C15—C14118.3 (8)C22—C21—O1110.3 (16)
C17—C16—C15122.9 (8)C21—C22—C2394.4 (15)
C16—C17—C18120.6 (8)C24—C23—C22103.6 (12)
C17—C18—C13120.4 (7)O1—C24—C2399.3 (10)
O1A—Li1—O1Aiii99.0 (11)C24A—O1A—C21A106.5 (13)
O1A—Li1—O1Aiv99.0 (11)C24A—O1A—Li1132.7 (13)
O1Aiii—Li1—O1Aiv99.0 (11)C21A—O1A—Li1118.7 (10)
O1A—Li1—O1iii104.7 (9)C23A—C24A—O1A108.3 (18)
O1Aiii—Li1—O1iii15.4 (6)C31—O2A—C3498 (2)
O1Aiv—Li1—O1iii111.7 (10)C31—O2A—Li1168 (3)
O1A—Li1—O115.4 (6)C34—O2A—Li187.5 (19)
O1Aiii—Li1—O1111.7 (10)C32—C31—O2A97 (3)
O1Aiv—Li1—O1104.7 (9)C31—C32—C33100 (3)
O1iii—Li1—O1114.6 (6)C34—C33—C3299 (3)
O1A—Li1—O1iv111.7 (10)C33—C34—O2A111 (3)
O1Aiii—Li1—O1iv104.7 (9)C33—C34—Li1161 (4)
O1Aiv—Li1—O1iv15.4 (6)O2A—C34—Li154.8 (14)
O1iii—Li1—O1iv114.5 (6)
S1i—Ti1—S1—C1173.2 (2)C34iii—Li1—O1—C21111.8 (18)
S1ii—Ti1—S1—C182.8 (2)C24—O1—C21—C2234 (3)
S2—Ti1—S1—C150.4 (4)Li1—O1—C21—C22169.0 (16)
S2ii—Ti1—S1—C190.8 (2)O1—C21—C22—C2348 (2)
S2i—Ti1—S1—C113.5 (2)C21—C22—C23—C2446.6 (17)
S1i—Ti1—S2—C716.7 (2)C21—O1—C24—C230.6 (18)
S1ii—Ti1—S2—C7107.8 (2)Li1—O1—C24—C23149.2 (14)
S1—Ti1—S2—C7119.3 (4)C22—C23—C24—O127.6 (14)
S2ii—Ti1—S2—C777.9 (2)O1Aiii—Li1—O1A—C24A30 (3)
S2i—Ti1—S2—C7157.2 (2)O1Aiv—Li1—O1A—C24A131 (2)
S1i—Ti1—S2—Ti2134.22 (5)O1iii—Li1—O1A—C24A16 (3)
S1ii—Ti1—S2—Ti2134.67 (5)O1—Li1—O1A—C24A116 (4)
S1—Ti1—S2—Ti21.8 (3)O1iv—Li1—O1A—C24A140 (2)
S2ii—Ti1—S2—Ti239.633 (19)O2Aiv—Li1—O1A—C24A93 (2)
S2i—Ti1—S2—Ti239.638 (19)O2A—Li1—O1A—C24A89 (3)
S3i—Ti2—S2—C799.6 (2)O2Aiii—Li1—O1A—C24A114 (2)
S3—Ti2—S2—C71.4 (2)C34iv—Li1—O1A—C24A88 (3)
S3ii—Ti2—S2—C7158.3 (2)C34—Li1—O1A—C24A37 (4)
S2ii—Ti2—S2—C781.1 (2)C34iii—Li1—O1A—C24A158 (2)
S2i—Ti2—S2—C7160.15 (19)O1Aiii—Li1—O1A—C21A130.4 (11)
S3i—Ti2—S2—Ti1139.79 (5)O1Aiv—Li1—O1A—C21A30 (2)
S3—Ti2—S2—Ti1119.27 (5)O1iii—Li1—O1A—C21A145.1 (13)
S3ii—Ti2—S2—Ti137.64 (15)O1—Li1—O1A—C21A83 (3)
S2ii—Ti2—S2—Ti139.511 (19)O1iv—Li1—O1A—C21A21 (2)
S2i—Ti2—S2—Ti139.516 (19)O2Aiv—Li1—O1A—C21A105.9 (16)
S3i—Ti2—S3—C1312.7 (2)O2A—Li1—O1A—C21A109.8 (15)
S3ii—Ti2—S3—C1392.2 (2)O2Aiii—Li1—O1A—C21A84.6 (16)
S2ii—Ti2—S3—C13171.2 (2)C34iv—Li1—O1A—C21A111 (2)
S2—Ti2—S3—C1396.2 (2)C34—Li1—O1A—C21A161.9 (18)
S2i—Ti2—S3—C13169.4 (2)C34iii—Li1—O1A—C21A41 (2)
Ti1—S1—C1—C242.1 (5)C21A—O1A—C24A—C23A11 (3)
Ti1—S1—C1—C6140.3 (4)Li1—O1A—C24A—C23A173.7 (18)
C6—C1—C2—C31.7 (9)O1A—Li1—O2A—C31117 (10)
S1—C1—C2—C3179.2 (5)O1Aiii—Li1—O2A—C31126 (10)
C1—C2—C3—C40.7 (10)O1Aiv—Li1—O2A—C3116 (10)
C2—C3—C4—C51.4 (10)O1iii—Li1—O2A—C31132 (10)
C3—C4—C5—C62.5 (10)O1—Li1—O2A—C31109 (10)
C4—C5—C6—C11.6 (10)O1iv—Li1—O2A—C3116 (10)
C2—C1—C6—C50.5 (9)O2Aiv—Li1—O2A—C31107 (10)
S1—C1—C6—C5178.2 (5)O2Aiii—Li1—O2A—C3146 (10)
Ti1—S2—C7—C1247.5 (5)C34iv—Li1—O2A—C31119 (10)
Ti2—S2—C7—C1255.1 (5)C34—Li1—O2A—C31118 (11)
Ti1—S2—C7—C8133.9 (4)C34iii—Li1—O2A—C3114 (10)
Ti2—S2—C7—C8123.6 (4)O1A—Li1—O2A—C34125 (3)
C12—C7—C8—C92.6 (9)O1Aiii—Li1—O2A—C348 (3)
S2—C7—C8—C9176.1 (5)O1Aiv—Li1—O2A—C34102 (3)
C7—C8—C9—C100.1 (9)O1iii—Li1—O2A—C3414 (3)
C8—C9—C10—C111.8 (10)O1—Li1—O2A—C34133 (3)
C9—C10—C11—C120.7 (9)O1iv—Li1—O2A—C34102 (3)
C8—C7—C12—C113.6 (8)O2Aiv—Li1—O2A—C34135 (5)
S2—C7—C12—C11175.1 (4)O2Aiii—Li1—O2A—C34164 (5)
C10—C11—C12—C72.0 (9)C34iv—Li1—O2A—C34123.4 (15)
Ti2—S3—C13—C14103.0 (6)C34iii—Li1—O2A—C34132.3 (15)
Ti2—S3—C13—C1881.5 (5)C34—O2A—C31—C3250 (4)
C18—C13—C14—C154.2 (10)Li1—O2A—C31—C32167 (8)
S3—C13—C14—C15179.8 (6)O2A—C31—C32—C3357 (4)
C13—C14—C15—C163.5 (13)C31—C32—C33—C3442 (7)
C14—C15—C16—C171.3 (15)C32—C33—C34—O2A9 (8)
C15—C16—C17—C180.1 (15)C32—C33—C34—Li127 (19)
C16—C17—C18—C130.9 (12)C31—O2A—C34—C3324 (7)
C14—C13—C18—C173.0 (10)Li1—O2A—C34—C33167 (6)
S3—C13—C18—C17178.6 (5)C31—O2A—C34—Li1169 (3)
O1A—Li1—O1—C24118 (3)O1A—Li1—C34—C3350 (17)
O1Aiii—Li1—O1—C2482 (2)O1Aiii—Li1—C34—C33129 (17)
O1Aiv—Li1—O1—C24171.9 (14)O1Aiv—Li1—C34—C33143 (16)
O1iii—Li1—O1—C2465 (2)O1iii—Li1—C34—C33120 (17)
O1iv—Li1—O1—C24159.3 (13)O1—Li1—C34—C3329 (17)
O2Aiv—Li1—O1—C2440.3 (17)O1iv—Li1—C34—C33132 (16)
O2A—Li1—O1—C2439.5 (19)O2Aiv—Li1—C34—C3323 (15)
O2Aiii—Li1—O1—C2460.8 (16)O2A—Li1—C34—C3343 (14)
C34iv—Li1—O1—C2430 (2)O2Aiii—Li1—C34—C3350 (15)
C34—Li1—O1—C240 (3)C34iv—Li1—C34—C334 (15)
C34iii—Li1—O1—C2499.8 (16)C34iii—Li1—C34—C3381 (15)
O1A—Li1—O1—C2130 (2)O1A—Li1—C34—O2A93 (3)
O1Aiii—Li1—O1—C2166.6 (16)O1Aiii—Li1—C34—O2A171 (3)
O1Aiv—Li1—O1—C2139.6 (19)O1Aiv—Li1—C34—O2A100 (3)
O1iii—Li1—O1—C2183.0 (16)O1iii—Li1—C34—O2A163 (4)
O1iv—Li1—O1—C2152.3 (19)O1—Li1—C34—O2A71 (4)
O2Aiv—Li1—O1—C21171.2 (15)O1iv—Li1—C34—O2A89 (3)
O2A—Li1—O1—C21172.1 (15)O2Aiv—Li1—C34—O2A20 (2)
O2Aiii—Li1—O1—C21150.8 (14)O2Aiii—Li1—C34—O2A7 (2)
C34iv—Li1—O1—C21178 (3)C34iv—Li1—C34—O2A46.8 (15)
C34—Li1—O1—C21148 (2)C34iii—Li1—C34—O2A38.1 (15)
Symmetry codes: (i) y+1/2, z+1, x+1/2; (ii) z1/2, x+1/2, y+1; (iii) y+1, z1, x; (iv) z, x1, y+1.

Experimental details

Crystal data
Chemical formula[Li(C4H8O)4][Ti2(C6H5S)9]
Mr1372.91
Crystal system, space groupCubic, P213
Temperature (K)120
a (Å)19.096 (3)
V3)6963.9 (19)
Z4
Radiation typeMo Kα
µ (mm1)0.55
Crystal size (mm)0.30 × 0.25 × 0.20
Data collection
DiffractometerEnraf-Nonius CAD-4
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.885, 0.897
No. of measured, independent and
observed [I > 2σ(I)] reflections
2511, 2511, 1802
Rint0.000
(sin θ/λ)max1)0.618
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.046, 0.127, 0.98
No. of reflections2511
No. of parameters251
No. of restraints36
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.57, 0.27
Absolute structureFlack (1983), no Friedel pairs
Absolute structure parameter0.05 (7)

Computer programs: CAD-4 Operations Manual (Enraf-Nonius, 1977), CAD-4 Operations Manual, PROCESS MolEN (Fair, 1990), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997).

Selected geometric parameters (Å, º) top
Ti1—S1i2.3351 (17)Ti2—S3i2.3240 (15)
Ti1—S22.5329 (17)Ti2—S2ii2.5434 (16)
S1i—Ti1—S1ii90.46 (7)S3i—Ti2—S3101.86 (6)
S1i—Ti1—S296.22 (5)S3i—Ti2—S2ii158.44 (7)
S1ii—Ti1—S295.87 (5)S3—Ti2—S2ii82.04 (5)
S1—Ti1—S2170.75 (7)S3ii—Ti2—S2ii97.99 (5)
S2—Ti1—S2ii76.78 (6)S2ii—Ti2—S276.41 (6)
S1i—Ti1—S2i170.75 (7)S3i—Ti2—S2i98.00 (5)
S1ii—Ti1—S2i96.22 (5)S3—Ti2—S2i158.43 (7)
S1—Ti1—S2i95.87 (5)S3ii—Ti2—S2i82.04 (5)
S2—Ti1—S2i76.78 (6)
Symmetry codes: (i) y+1/2, z+1, x+1/2; (ii) z1/2, x+1/2, y+1.
 

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