Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801006626/br6009sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801006626/br6009Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (Sr-O) = 0.01 Å
- R factor = 0.030
- wR factor = 0.055
- Data-to-parameter ratio = 28.8
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_731 Alert C Bond Calc 3.8305(9), Rep 3.830(2) .... 2.22 s.u-Ratio SR1 -I2 1.555 6.565 PLAT_731 Alert C Bond Calc 3.8305(9), Rep 3.830(2) .... 2.22 s.u-Ratio SR1 -I2 1.555 5.555 PLAT_732 Alert C Angle Calc 144.65(4), Rep 144.65(2) .... 2.22 s.u-Ratio O -SR2 -I2 1.555 1.555 1.555 General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.58 From the CIF: _reflns_number_total 776 From the CIF: _diffrn_reflns_limit_ max hkl 6. 4. 10. From the CIF: _diffrn_reflns_limit_ min hkl -13. -10. -9. TEST1: Expected hkl limits for theta max Calculated maximum hkl 14. 14. 10. Calculated minimum hkl -14. -14. -10. ALERT: Expected hkl max differ from CIF values REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.58 From the CIF: _reflns_number_total 776 Count of symmetry unique reflns 382 Completeness (_total/calc) 203.14% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 394 Fraction of Friedel pairs measured 1.031 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
3 Alert Level C = Please check
Data collection: SMART Bruker, 1998); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT and SHELXL97 (Sheldrick, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 and WinGX (Farrugia, 1999); molecular graphics: ATOMS (Dowty, 1998) and ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2001).
Sr4OI6 | Dx = 4.760 Mg m−3 |
Mr = 1127.88 | Mo Kα radiation, λ = 0.71069 Å |
Hexagonal, P63mc | Cell parameters from 841 reflections |
a = 10.747 (1) Å | θ = 5.9–27.6° |
c = 7.8678 (9) Å | µ = 25.21 mm−1 |
V = 787.0 (3) Å3 | T = 150 K |
Z = 2 | Block, colourless |
F(000) = 956 | 0.05 × 0.04 × 0.04 mm |
Bruker SMART1000 CCD area-detector diffractometer | 776 independent reflections |
Radiation source: fine-focus sealed tube | 586 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.054 |
ω scans | θmax = 27.6°, θmin = 5.9° |
Absorption correction: multi-scan (SADABS; Bruker, 1996) | h = −13→6 |
Tmin = 0.272, Tmax = 0.365 | k = −10→4 |
3527 measured reflections | l = −9→10 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.030 | w = 1/[σ2(Fo2) + (0.0206P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.055 | (Δ/σ)max < 0.001 |
S = 0.94 | Δρmax = 1.27 e Å−3 |
721 reflections | Δρmin = −0.99 e Å−3 |
25 parameters | Absolute structure: Flack (1983) |
1 restraint | Absolute structure parameter: 0.064 (18) |
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. |
x | y | z | Uiso*/Ueq | ||
Sr1 | 0.3333 | 0.6667 | 0.8847 (3) | 0.0290 (6) | |
Sr2 | 0.21157 (7) | 0.42313 (14) | 0.48599 (16) | 0.0172 (3) | |
I1 | 0.46542 (5) | 0.53458 (5) | 0.17690 (10) | 0.0174 (2) | |
I2 | 0.25533 (9) | 0.12766 (5) | 0.36865 (10) | 0.0175 (2) | |
O | 0.3333 | 0.6667 | 0.584 (3) | 0.031 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sr1 | 0.0391 (10) | 0.0391 (10) | 0.0088 (12) | 0.0196 (5) | 0.000 | 0.000 |
Sr2 | 0.0181 (5) | 0.0200 (7) | 0.0142 (7) | 0.0100 (4) | −0.0004 (3) | −0.0008 (6) |
I1 | 0.0187 (3) | 0.0187 (3) | 0.0129 (4) | 0.0078 (4) | 0.0015 (2) | −0.0015 (2) |
I2 | 0.0195 (5) | 0.0166 (3) | 0.0174 (5) | 0.0098 (2) | 0.0008 (5) | 0.0004 (2) |
O | 0.027 (7) | 0.027 (7) | 0.038 (12) | 0.014 (4) | 0.000 | 0.000 |
Sr1—O | 2.37 (2) | Sr2—I2 | 3.5567 (19) |
Sr1—I1i | 3.366 (2) | Sr2—I1vi | 3.5967 (17) |
Sr1—I1ii | 3.366 (2) | Sr2—I1v | 3.5967 (17) |
Sr1—I1iii | 3.366 (2) | Sr2—Sr2viii | 3.926 (3) |
Sr1—I2iv | 3.830 (2) | Sr2—Sr2vii | 3.926 (3) |
Sr1—I2v | 3.830 (2) | I1—Sr1x | 3.366 (2) |
Sr1—I2vi | 3.830 (2) | I1—Sr2viii | 3.3947 (18) |
Sr1—Sr2vii | 3.870 (3) | I1—Sr2xi | 3.5967 (17) |
Sr1—Sr2 | 3.870 (3) | I1—Sr2xii | 3.5967 (17) |
Sr1—Sr2viii | 3.870 (3) | I2—Sr2xi | 3.392 (2) |
Sr2—O | 2.393 (6) | I2—Sr2xiii | 3.5567 (19) |
Sr2—I2v | 3.392 (2) | I2—Sr1xii | 3.830 (2) |
Sr2—I1vii | 3.3947 (18) | O—Sr2vii | 2.393 (6) |
Sr2—I1 | 3.3947 (18) | O—Sr2viii | 2.393 (6) |
Sr2—I2ix | 3.5567 (19) | ||
O—Sr1—I1i | 133.08 (4) | I2v—Sr2—I1vi | 71.32 (3) |
O—Sr1—I1ii | 133.08 (4) | I1vii—Sr2—I1vi | 146.26 (4) |
I1i—Sr1—I1ii | 78.48 (6) | I1—Sr2—I1vi | 72.54 (4) |
O—Sr1—I1iii | 133.08 (4) | I2ix—Sr2—I1vi | 135.64 (4) |
I1i—Sr1—I1iii | 78.48 (6) | I2—Sr2—I1vi | 70.80 (3) |
I1ii—Sr1—I1iii | 78.48 (6) | O—Sr2—I1v | 76.25 (17) |
O—Sr1—I2iv | 88.11 (4) | I2v—Sr2—I1v | 71.32 (3) |
I1i—Sr1—I2iv | 69.97 (2) | I1vii—Sr2—I1v | 72.54 (4) |
I1ii—Sr1—I2iv | 69.97 (2) | I1—Sr2—I1v | 146.26 (4) |
I1iii—Sr1—I2iv | 138.80 (8) | I2ix—Sr2—I1v | 70.80 (3) |
O—Sr1—I2v | 88.11 (4) | I2—Sr2—I1v | 135.64 (4) |
I1i—Sr1—I2v | 138.80 (8) | I1vi—Sr2—I1v | 128.84 (6) |
I1ii—Sr1—I2v | 69.97 (2) | O—Sr2—Sr1 | 35.4 (5) |
I1iii—Sr1—I2v | 69.97 (2) | I2v—Sr2—Sr1 | 63.27 (5) |
I2iv—Sr1—I2v | 119.893 (5) | I1vii—Sr2—Sr1 | 113.68 (5) |
O—Sr1—I2vi | 88.11 (4) | I1—Sr2—Sr1 | 113.68 (5) |
I1i—Sr1—I2vi | 69.97 (2) | I2ix—Sr2—Sr1 | 131.55 (3) |
I1ii—Sr1—I2vi | 138.80 (8) | I2—Sr2—Sr1 | 131.55 (3) |
I1iii—Sr1—I2vi | 69.97 (2) | I1vi—Sr2—Sr1 | 66.26 (3) |
I2iv—Sr1—I2vi | 119.893 (5) | I1v—Sr2—Sr1 | 66.26 (3) |
I2v—Sr1—I2vi | 119.893 (5) | O—Sr2—Sr2viii | 34.9 (2) |
O—Sr1—Sr2vii | 35.85 (4) | I2v—Sr2—Sr2viii | 113.50 (3) |
I1i—Sr1—Sr2vii | 109.86 (4) | I1vii—Sr2—Sr2viii | 92.81 (2) |
I1ii—Sr1—Sr2vii | 109.86 (4) | I1—Sr2—Sr2viii | 54.67 (3) |
I1iii—Sr1—Sr2vii | 168.93 (6) | I2ix—Sr2—Sr2viii | 163.52 (2) |
I2iv—Sr1—Sr2vii | 52.26 (3) | I2—Sr2—Sr2viii | 112.351 (18) |
I2v—Sr1—Sr2vii | 105.43 (5) | I1vi—Sr2—Sr2viii | 56.92 (2) |
I2vi—Sr1—Sr2vii | 105.43 (5) | I1v—Sr2—Sr2viii | 110.87 (2) |
O—Sr1—Sr2 | 35.85 (4) | Sr1—Sr2—Sr2viii | 59.52 (3) |
I1i—Sr1—Sr2 | 168.93 (6) | O—Sr2—Sr2vii | 34.9 (2) |
I1ii—Sr1—Sr2 | 109.86 (4) | I2v—Sr2—Sr2vii | 113.50 (3) |
I1iii—Sr1—Sr2 | 109.86 (4) | I1vii—Sr2—Sr2vii | 54.67 (3) |
I2iv—Sr1—Sr2 | 105.43 (5) | I1—Sr2—Sr2vii | 92.81 (2) |
I2v—Sr1—Sr2 | 52.26 (3) | I2ix—Sr2—Sr2vii | 112.351 (18) |
I2vi—Sr1—Sr2 | 105.43 (5) | I2—Sr2—Sr2vii | 163.52 (2) |
Sr2vii—Sr1—Sr2 | 60.96 (6) | I1vi—Sr2—Sr2vii | 110.87 (2) |
O—Sr1—Sr2viii | 35.85 (4) | I1v—Sr2—Sr2vii | 56.92 (2) |
I1i—Sr1—Sr2viii | 109.86 (4) | Sr1—Sr2—Sr2vii | 59.52 (3) |
I1ii—Sr1—Sr2viii | 168.93 (6) | Sr2viii—Sr2—Sr2vii | 60.0 |
I1iii—Sr1—Sr2viii | 109.86 (4) | Sr1x—I1—Sr2viii | 101.78 (5) |
I2iv—Sr1—Sr2viii | 105.43 (5) | Sr1x—I1—Sr2 | 101.78 (5) |
I2v—Sr1—Sr2viii | 105.43 (5) | Sr2viii—I1—Sr2 | 70.65 (6) |
I2vi—Sr1—Sr2viii | 52.26 (3) | Sr1x—I1—Sr2xi | 104.20 (5) |
Sr2vii—Sr1—Sr2viii | 60.96 (6) | Sr2viii—I1—Sr2xi | 153.95 (4) |
Sr2—Sr1—Sr2viii | 60.96 (6) | Sr2—I1—Sr2xi | 105.50 (4) |
O—Sr2—I2v | 98.7 (5) | Sr1x—I1—Sr2xii | 104.20 (5) |
O—Sr2—I1vii | 86.6 (4) | Sr2viii—I1—Sr2xii | 105.50 (4) |
I2v—Sr2—I1vii | 140.95 (3) | Sr2—I1—Sr2xii | 153.95 (4) |
O—Sr2—I1 | 86.6 (4) | Sr2xi—I1—Sr2xii | 66.15 (4) |
I2v—Sr2—I1 | 140.95 (3) | Sr2xi—I2—Sr2 | 106.45 (2) |
I1vii—Sr2—I1 | 77.69 (5) | Sr2xi—I2—Sr2xiii | 106.45 (2) |
O—Sr2—I2ix | 144.645 (17) | Sr2—I2—Sr2xiii | 147.04 (5) |
I2v—Sr2—I2ix | 82.78 (4) | Sr2xi—I2—Sr1xii | 64.47 (5) |
I1vii—Sr2—I2ix | 71.78 (3) | Sr2—I2—Sr1xii | 96.08 (2) |
I1—Sr2—I2ix | 114.41 (5) | Sr2xiii—I2—Sr1xii | 96.08 (2) |
O—Sr2—I2 | 144.645 (18) | Sr1—O—Sr2vii | 108.7 (5) |
I2v—Sr2—I2 | 82.78 (4) | Sr1—O—Sr2 | 108.7 (5) |
I1vii—Sr2—I2 | 114.41 (5) | Sr2vii—O—Sr2 | 110.2 (4) |
I1—Sr2—I2 | 71.78 (3) | Sr1—O—Sr2viii | 108.7 (5) |
I2ix—Sr2—I2 | 70.71 (3) | Sr2vii—O—Sr2viii | 110.2 (4) |
O—Sr2—I1vi | 76.25 (17) | Sr2—O—Sr2viii | 110.2 (4) |
Symmetry codes: (i) −y+1, x−y+1, z+1; (ii) −x+y, −x+1, z+1; (iii) x, y, z+1; (iv) y, −x+y+1, z+1/2; (v) x−y, x, z+1/2; (vi) −x+1, −y+1, z+1/2; (vii) −x+y, −x+1, z; (viii) −y+1, x−y+1, z; (ix) −y, x−y, z; (x) x, y, z−1; (xi) y, −x+y, z−1/2; (xii) −x+1, −y+1, z−1/2; (xiii) −x+y, −x, z. |
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