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The optical rotation (OR) of CsLiB6O10 (CLBO, space group I\bar{4}2d) along the a axis has been determined by the HAUP method [Kobayashi & Uesu (1983). J Appl. Cryst. 16, 204–211] at a wavelength of 632.8 nm and by the TILTER method [Kaminsky & Glazer (1996). Ferroelectrics, 183, 133–141] at 532 nm and 650 nm. The respective rotatory powers were found to be 17 (1), 24 (2) and 19 (2)° mm−1. The absolute chirality has been established by comparing Bijvoet differences, {hkl} and {k\bar{h}l}, on the same crystal on which OR was measured. Atomic positions and electron density Fourier peak heights were exploited as input for semi-empirical calculations of refractive indices and OR, using WinOPTACT [Glazer (2002). J. Appl. Cryst. 35, 652] with only one free parameter fitted to match the average refractive index.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889805009908/aj5030sup1.cif
Contains datablock shelxl

Computing details top

Data collection: KappaCCD; cell refinement: HKL SCALEPACK (Otwinowski & Minor 1997); data reduction: HKL SCALEPACK (Otwinowski & Minor 1997); program(s) used to solve structure: SIR97; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: maXus, ZORTEP; software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

'CLBO' top
Crystal data top
B12O20·2(Cs)·2(Li)F(000) = 672
Mr = 729.42Dx = 2.478 Mg m3
Tetragonal, I42dMo Kα radiation, λ = 0.71070 Å
Hall symbol: I -4 2bwCell parameters from 135 reflections
a = 10.4670 (9) ŵ = 3.83 mm1
c = 8.9220 (6) ÅT = 295 K
V = 977.48 (14) Å3Cut block, colorless
Z = 20.58 × 0.55 × 0.54 mm
Data collection top
Nonius KappaCCD
diffractometer
477 independent reflections
Radiation source: fine-focus sealed tube466 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
φ and ω scansθmax = 26.3°, θmin = 3.0°
Absorption correction: multi-scan
HKL2000
h = 1313
Tmin = 0.130, Tmax = 0.132k = 1313
477 measured reflectionsl = 1111
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)] = 0.055 w = 1/[σ2(Fo2) + (0.0963P)2 + 6.8411P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.144(Δ/σ)max < 0.001
S = 1.24Δρmax = 0.70 e Å3
477 reflectionsΔρmin = 1.52 e Å3
43 parametersAbsolute structure: Flack (1983), 172 Friedel pairs
0 restraintsAbsolute structure parameter: 0.28 (24)
Special details top

Experimental. Data was collected with ω and φ scans in 2° increments with 15 second exposures per degree. Crystal-to-detector distance was 30 mm. 16894 full and partial reflection were integrated.

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
Li10.00000.00000.50000.010 (4)
B10.2326 (7)0.1484 (7)0.5601 (9)0.0095 (15)
B20.25000.0244 (8)0.37500.005 (2)
O10.1022 (5)0.1444 (5)0.5703 (7)0.0127 (11)
O20.2994 (7)0.25000.62500.026 (2)
O30.3020 (5)0.0575 (5)0.4948 (7)0.0125 (10)
Cs10.00000.00000.00000.0277 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Li10.006 (6)0.006 (6)0.019 (12)0.0000.0000.000
B10.010 (4)0.009 (3)0.010 (4)0.001 (3)0.004 (3)0.002 (3)
B20.009 (4)0.006 (5)0.002 (5)0.0000.000 (3)0.000
O10.008 (2)0.012 (3)0.018 (3)0.0016 (18)0.002 (2)0.009 (2)
O20.012 (3)0.023 (3)0.029 (4)0.0000.0000.016 (3)
O30.013 (2)0.011 (2)0.013 (2)0.0023 (17)0.001 (2)0.006 (2)
Cs10.0291 (5)0.0291 (5)0.0250 (7)0.0000.0000.000
Geometric parameters (Å, º) top
Li1—O1i1.954 (5)O2—Cs1x3.536 (5)
Li1—O1ii1.954 (5)O2—Cs1v3.536 (5)
Li1—O11.954 (5)O3—Cs1v3.137 (5)
Li1—O1iii1.954 (5)Cs1—O3xi3.137 (5)
Li1—Cs1iv4.4610 (3)Cs1—O3vii3.137 (5)
Li1—Cs14.4610 (3)Cs1—O3xii3.137 (5)
B1—O31.331 (9)Cs1—O3xiii3.137 (5)
B1—O11.369 (9)Cs1—O2xiv3.536 (5)
B1—O21.398 (8)Cs1—O2xi3.536 (5)
B1—Cs1v3.622 (7)Cs1—O2xiii3.536 (5)
B2—O1ii1.457 (7)Cs1—O2xv3.536 (5)
B2—O1vi1.457 (7)Cs1—B1xi3.622 (7)
B2—O3vii1.474 (7)Cs1—B1vii3.622 (7)
B2—O31.474 (7)Cs1—B1xii3.622 (7)
O1—B2viii1.457 (6)Cs1—B1xiii3.622 (7)
O2—B1ix1.398 (8)
O1i—Li1—O1ii142.6 (4)O2xiv—Cs1—O2xi95.711 (15)
O1i—Li1—O195.91 (12)O3xi—Cs1—O2xiii107.78 (12)
O1ii—Li1—O195.90 (12)O3vii—Cs1—O2xiii81.60 (11)
O1i—Li1—O1iii95.90 (12)O3xii—Cs1—O2xiii127.16 (13)
O1ii—Li1—O1iii95.90 (12)O3xiii—Cs1—O2xiii40.25 (10)
O1—Li1—O1iii142.6 (4)O2xiv—Cs1—O2xiii95.710 (15)
O1i—Li1—Cs1iv108.71 (19)O2xi—Cs1—O2xiii143.23 (5)
O1ii—Li1—Cs1iv108.71 (19)O3xi—Cs1—O2xv127.16 (13)
O1—Li1—Cs1iv71.29 (19)O3vii—Cs1—O2xv107.78 (12)
O1iii—Li1—Cs1iv71.29 (19)O3xii—Cs1—O2xv40.25 (10)
O1i—Li1—Cs171.29 (19)O3xiii—Cs1—O2xv81.60 (11)
O1ii—Li1—Cs171.29 (19)O2xiv—Cs1—O2xv143.23 (5)
O1—Li1—Cs1108.71 (19)O2xi—Cs1—O2xv95.710 (15)
O1iii—Li1—Cs1108.71 (19)O2xiii—Cs1—O2xv95.709 (15)
Cs1iv—Li1—Cs1180.0O3xi—Cs1—B1xi21.20 (15)
O3—B1—O1123.4 (6)O3vii—Cs1—B1xi118.35 (15)
O3—B1—O2116.9 (6)O3xii—Cs1—B1xi101.79 (16)
O1—B1—O2119.6 (7)O3xiii—Cs1—B1xi104.66 (17)
O3—B1—Cs1v58.5 (4)O2xiv—Cs1—B1xi80.24 (13)
O1—B1—Cs1v136.6 (5)O2xi—Cs1—B1xi22.49 (12)
O2—B1—Cs1v75.3 (3)O2xiii—Cs1—B1xi128.96 (13)
O1ii—B2—O1vi112.1 (7)O2xv—Cs1—B1xi117.69 (14)
O1ii—B2—O3vii106.7 (3)O3xi—Cs1—B1vii101.79 (16)
O1vi—B2—O3vii111.2 (4)O3vii—Cs1—B1vii21.20 (15)
O1ii—B2—O3111.2 (4)O3xii—Cs1—B1vii104.66 (17)
O1vi—B2—O3106.7 (3)O3xiii—Cs1—B1vii118.35 (15)
O3vii—B2—O3108.9 (7)O2xiv—Cs1—B1vii22.49 (12)
B1—O1—B2viii123.8 (6)O2xi—Cs1—B1vii117.69 (14)
B1—O1—Li1123.3 (4)O2xiii—Cs1—B1vii80.24 (13)
B2viii—O1—Li1112.9 (4)O2xv—Cs1—B1vii128.96 (13)
B1ix—O2—B1120.0 (8)B1xi—Cs1—B1vii102.65 (10)
B1ix—O2—Cs1x82.2 (3)O3xi—Cs1—B1xii118.35 (15)
B1—O2—Cs1x136.8 (3)O3vii—Cs1—B1xii104.66 (17)
B1ix—O2—Cs1v136.8 (3)O3xii—Cs1—B1xii21.20 (15)
B1—O2—Cs1v82.2 (3)O3xiii—Cs1—B1xii101.79 (16)
Cs1x—O2—Cs1v107.1 (2)O2xiv—Cs1—B1xii128.96 (13)
B1—O3—B2122.1 (5)O2xi—Cs1—B1xii80.24 (13)
B1—O3—Cs1v100.3 (4)O2xiii—Cs1—B1xii117.69 (14)
B2—O3—Cs1v131.2 (4)O2xv—Cs1—B1xii22.49 (12)
O3xi—Cs1—O3vii121.79 (13)B1xi—Cs1—B1xii102.65 (10)
O3xi—Cs1—O3xii121.79 (13)B1vii—Cs1—B1xii124.2 (2)
O3vii—Cs1—O3xii86.9 (2)O3xi—Cs1—B1xiii104.66 (17)
O3xi—Cs1—O3xiii86.9 (2)O3vii—Cs1—B1xiii101.79 (16)
O3vii—Cs1—O3xiii121.79 (13)O3xii—Cs1—B1xiii118.35 (15)
O3xii—Cs1—O3xiii121.79 (13)O3xiii—Cs1—B1xiii21.20 (15)
O3xi—Cs1—O2xiv81.60 (11)O2xiv—Cs1—B1xiii117.69 (14)
O3vii—Cs1—O2xiv40.25 (10)O2xi—Cs1—B1xiii128.96 (13)
O3xii—Cs1—O2xiv107.78 (12)O2xiii—Cs1—B1xiii22.49 (12)
O3xiii—Cs1—O2xiv127.16 (13)O2xv—Cs1—B1xiii80.24 (13)
O3xi—Cs1—O2xi40.25 (10)B1xi—Cs1—B1xiii124.2 (2)
O3vii—Cs1—O2xi127.16 (13)B1vii—Cs1—B1xiii102.65 (10)
O3xii—Cs1—O2xi81.60 (11)B1xii—Cs1—B1xiii102.65 (11)
O3xiii—Cs1—O2xi107.78 (12)
Symmetry codes: (i) y, x, z+1; (ii) y, x, z+1; (iii) x, y, z; (iv) x, y, z+1; (v) x+1/2, y, z+3/4; (vi) y+1/2, x, z1/4; (vii) x+1/2, y, z+3/4; (viii) y, x+1/2, z+1/4; (ix) x, y+1/2, z+5/4; (x) x+1/2, y+1/2, z+1/2; (xi) y, x+1/2, z3/4; (xii) x1/2, y, z+3/4; (xiii) y, x1/2, z3/4; (xiv) x+1/2, y+1/2, z1/2; (xv) x1/2, y1/2, z1/2.
 

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