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Single crystals of YI
3 were obtained by high-vacuum sublimation of the crude product at 1213 K. The crystal structure is that of the BiI
3 structure type. Two-thirds of the octahedral voids between every second hexagonally closest-packed layer of I
− ions are occupied by Y
3+ ions. Thereby, the YI
6 octahedra share common edges within
Bγ
2/3A slabs in the stacking sequence
γ
2/3A□
Bγ
2/3A□
Bγ
2/3A□
Bγ
2/3.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (I-Y) = 0.001 Å
- R factor = 0.032
- wR factor = 0.090
- Data-to-parameter ratio = 32.0
checkCIF/PLATON results
No syntax errors found
Alert level C
RINTA01_ALERT_3_C The value of Rint is greater than 0.10
Rint given 0.122
PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.12
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-RED (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97.
Crystal data top
YI3 | Dx = 4.617 Mg m−3 |
Mr = 469.61 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, R3 | Cell parameters from 6289 reflections |
Hall symbol: -R 3 | θ = 2.9–29.3° |
a = 7.4864 (12) Å | µ = 22.20 mm−1 |
c = 20.880 (6) Å | T = 293 K |
V = 1013.5 (4) Å3 | Plate, colourless |
Z = 6 | 0.20 × 0.10 × 0.05 mm |
F(000) = 1188 | |
Data collection top
Stoe IPDS-I diffractometer | 448 independent reflections |
Radiation source: fine-focus sealed tube | 409 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.122 |
φ scans | θmax = 26.0°, θmin = 2.9° |
Absorption correction: numerical [X-RED (Stoe & Cie, 2001), after optimizing the crystal shape using
X-SHAPE (Stoe & Cie, 1999)] | h = −9→9 |
Tmin = 0.023, Tmax = 0.204 | k = −9→9 |
3717 measured reflections | l = −25→25 |
Refinement top
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)] = 0.032 | w = 1/[σ2(Fo2) + (0.0446P)2 + 2.737P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.090 | (Δ/σ)max < 0.001 |
S = 1.08 | Δρmax = 1.16 e Å−3 |
448 reflections | Δρmin = −1.05 e Å−3 |
14 parameters | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.022 (3) |
Special details top
Experimental. A suitable single-crystal was carefully selected under a polarizing microscope
and mounted in a glass capillary. The scattering intensities were collected
with an imaging-plate diffractometer (IPDS I, Stoe & Cie) equipped with
a fine-focus sealed-tube X-ray source (Mo Kα, λ = 0.71073 Å) operating at
50 kV and 40 mA. Intensity data for YI3 were collected at 293 K by φ scans
in 142 frames in the 2θ range 2.93–52.00°. Structure solution and
refinement were carried out using the program SHELXL97 (Sheldrick,
1997). A numerical absorption correction (X-RED (Stoe & Cie, 2001) was
applied after optimization of the crystal shape (X-SHAPE (Stoe & Cie,
1999)). The final difference maps were free of any chemically significant
features. The refinement was based on F2 for ALL reflections. |
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 | x | y | z | Uiso*/Ueq | |
I | −0.01189 (6) | 0.66558 (5) | 0.08312 (2) | 0.0317 (3) | |
Y | 0.0000 | 1.0000 | 0.16627 (4) | 0.0264 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
I | 0.0342 (4) | 0.0257 (4) | 0.0326 (4) | 0.0130 (2) | 0.00833 (14) | 0.00020 (14) |
Y | 0.0238 (4) | 0.0238 (4) | 0.0315 (6) | 0.0119 (2) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
I—Yi | 3.0108 (7) | Y—Iiii | 3.0108 (7) |
I—Y | 3.0112 (7) | Y—Iiv | 3.0112 (7) |
Y—Iii | 3.0108 (7) | Y—Iv | 3.0112 (7) |
Y—Ii | 3.0108 (7) | | |
| | | |
Yi—I—Y | 91.739 (17) | Ii—Y—Iiv | 92.21 (2) |
Iii—Y—Ii | 89.52 (2) | Iiii—Y—Iiv | 88.260 (17) |
Iii—Y—Iiii | 89.52 (2) | I—Y—Iiv | 90.08 (2) |
Ii—Y—Iiii | 89.52 (2) | Iii—Y—Iv | 88.260 (17) |
Iii—Y—I | 92.21 (2) | Ii—Y—Iv | 177.172 (15) |
Ii—Y—I | 88.261 (17) | Iiii—Y—Iv | 92.21 (2) |
Iiii—Y—I | 177.171 (15) | I—Y—Iv | 90.08 (2) |
Iii—Y—Iiv | 177.171 (15) | Iiv—Y—Iv | 90.08 (2) |
Symmetry codes: (i) −x−1/3, −y+4/3, −z+1/3; (ii) y−1/3, −x+y+1/3, −z+1/3; (iii) x−y+2/3, x+4/3, −z+1/3; (iv) −x+y−1, −x+1, z; (v) −y+1, x−y+2, z. |
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