Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807015899/bi2165sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807015899/bi2165Isup2.hkl |
Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED; program(s) used to solve structure: SIR2002 (Burla et al., 2003); program(s) used to refine structure: JANA2000 (Petříček et al., 2000); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: JANA2000.
Cs3ZnCl5 | Dx = 3.440 Mg m−3 |
Mr = 641.4 | Mo Kα radiation, λ = 0.71069 Å |
Tetragonal, I4/mcm | Cell parameters from 6777 reflections |
Hall symbol: -I 4 2c | θ = 2.6–26.5° |
a = 9.2421 (18) Å | µ = 11.69 mm−1 |
c = 14.4928 (15) Å | T = 292 K |
V = 1237.9 (4) Å3 | Prism, colourless |
Z = 4 | 0.20 × 0.12 × 0.05 mm |
F(000) = 1120 |
Oxford XCalibur2 CCD area-detector diffractometer | 374 independent reflections |
Radiation source: X-ray tube | 349 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.023 |
ω scans | θmax = 26.6°, θmin = 2.8° |
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2006) | h = −11→11 |
Tmin = 0.103, Tmax = 0.290 | k = −11→11 |
7208 measured reflections | l = −18→18 |
Refinement on F2 | 0 constraints |
R[F > 3σ(F)] = 0.010 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0009I2] |
wR(F) = 0.035 | (Δ/σ)max = 0.008 |
S = 1.01 | Δρmax = 0.17 e Å−3 |
374 reflections | Δρmin = −0.22 e Å−3 |
18 parameters | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
0 restraints | Extinction coefficient: 0.0061 (2) |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors are based on F, with F set to zero for negative F2. The threshold expression of F2 > n*σ(F2) is used only for calculating R-factors etc. and is not relevant to the choice of reflections for refinement. The program used for refinement, Jana2000, uses the weighting scheme based on the experimental expectations, see _refine_ls_weighting_details, that does not force S to be one. Therefore the values of S are usually larger then the ones from the SHELX program. |
x | y | z | Uiso*/Ueq | ||
Cs1 | 0.334245 (15) | 0.165755 (15) | 1 | 0.03014 (9) | |
Cs2 | 1 | 0 | 0.75 | 0.04073 (11) | |
Zn1 | 0.5 | 0 | 0.75 | 0.02556 (13) | |
Cl1 | 0.5 | 0.5 | 1 | 0.0340 (3) | |
Cl2 | 0.63920 (6) | 0.13920 (6) | 0.84233 (5) | 0.04076 (16) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cs1 | 0.02764 (15) | 0.02764 (15) | 0.03515 (18) | 0.00189 (6) | 0 | 0 |
Cs2 | 0.04327 (17) | 0.04327 (17) | 0.0356 (2) | 0 | 0 | 0 |
Zn1 | 0.0280 (2) | 0.0280 (2) | 0.0206 (3) | 0 | 0 | 0 |
Cl1 | 0.0294 (3) | 0.0294 (3) | 0.0431 (6) | 0 | 0 | 0 |
Cl2 | 0.0429 (2) | 0.0429 (2) | 0.0364 (3) | −0.0125 (3) | −0.0061 (2) | −0.0061 (2) |
Zn1—Cl2 | 2.2584 (6) | Cs1—Cl2viii | 3.4236 (6) |
Zn1—Cl2i | 2.2584 (6) | Cs2—Cl1ix | 3.6232 (7) |
Zn1—Cl2ii | 2.2584 (6) | Cs2—Cl1x | 3.6232 (7) |
Zn1—Cl2iii | 2.2584 (6) | Cs2—Cl2 | 3.8164 (6) |
Cs1—Cl1 | 3.4481 (7) | Cs2—Cl2xi | 3.8164 (6) |
Cs1—Cl1iv | 3.4481 (7) | Cs2—Cl2xii | 3.8164 (6) |
Cs1—Cl2 | 3.6367 (6) | Cs2—Cl2i | 3.8164 (6) |
Cs1—Cl2v | 3.6367 (6) | Cs2—Cl2xiii | 3.8164 (6) |
Cs1—Cl2vi | 3.4236 (6) | Cs2—Cl2xiv | 3.8164 (6) |
Cs1—Cl2ii | 3.6367 (6) | Cs2—Cl2xv | 3.8164 (6) |
Cs1—Cl2vii | 3.6367 (6) | Cs2—Cl2xvi | 3.8164 (6) |
Cl2—Zn1—Cl2i | 110.55 (2) | Cl2ii—Zn1—Cl2 | 107.33 (2) |
Cl2—Zn1—Cl2ii | 107.33 (2) | Cl2ii—Zn1—Cl2i | 110.55 (2) |
Cl2—Zn1—Cl2iii | 110.55 (2) | Cl2ii—Zn1—Cl2iii | 110.55 (2) |
Cl2i—Zn1—Cl2 | 110.55 (2) | Cl2iii—Zn1—Cl2 | 110.55 (2) |
Cl2i—Zn1—Cl2ii | 110.55 (2) | Cl2iii—Zn1—Cl2i | 107.33 (2) |
Cl2i—Zn1—Cl2iii | 107.33 (2) | Cl2iii—Zn1—Cl2ii | 110.55 (2) |
Symmetry codes: (i) y+1/2, −x+1/2, −z+3/2; (ii) −x+1, −y, z; (iii) −y+1/2, x−1/2, −z+3/2; (iv) −x+1/2, y−1/2, z; (v) −x+1, −y, −z+2; (vi) y, −x+1, −z+2; (vii) x, y, −z+2; (viii) y, −x+1, z; (ix) x+1/2, y−1/2, z−1/2; (x) −x+3/2, y−1/2, z; (xi) −x+3/2, −y+1/2, −z+3/2; (xii) −y+1, x−1, z; (xiii) −x+2, −y, z; (xiv) x+1/2, y−1/2, −z+3/2; (xv) y+1, −x+1, z; (xvi) −y+3/2, x−1/2, −z+3/2. |