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Barium oxide iodide, Ba4OI6, has been prepared by a solid-state reaction and shown to be isostructural with both A4OCl6, where A is Ba or Sr, and Sr4OI6.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801006614/br6008sup1.cif
Contains datablocks I, Ba4OI6

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801006614/br6008Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](O-Ba) = 0.008 Å
  • R factor = 0.022
  • wR factor = 0.051
  • Data-to-parameter ratio = 31.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
CELLV_02 Alert C The supplied cell volume s.u. differs from that calculated from the cell parameter s.u.'s by > 2 Calculated cell volume su = 5.41 Cell volume su given = 9.00 General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 28.81 From the CIF: _reflns_number_total 842 Count of symmetry unique reflns 462 Completeness (_total/calc) 182.25% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 380 Fraction of Friedel pairs measured 0.823 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
1 Alert Level C = Please check

Computing details top

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: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2001).

(I) top
Crystal data top
Ba4OI6Dx = 5.150 Mg m3
Mr = 1326.72Mo Kα radiation, λ = 0.71069 Å
Hexagonal, P63mcCell parameters from 802 reflections
a = 10.838 (4) Åθ = 4.3–27.8°
c = 8.410 (3) ŵ = 19.87 mm1
V = 855.5 (9) Å3T = 150 K
Z = 2Block, colourless
F(000) = 11000.18 × 0.12 × 0.10 mm
Data collection top
Bruker SMART1000 CCD area-detector
diffractometer
842 independent reflections
Radiation source: fine-focus sealed tube732 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
ω scansθmax = 28.8°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Bruker, 1996)
h = 1412
Tmin = 0.077, Tmax = 0.137k = 1414
4900 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)] = 0.022 w = 1/[σ2(Fo2) + (0.0263P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.051(Δ/σ)max = 0.001
S = 1.09Δρmax = 0.82 e Å3
782 reflectionsΔρmin = 1.20 e Å3
25 parametersAbsolute structure: Flack (1983)
1 restraintAbsolute structure parameter: 0.06 (10)
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*/Ueq
Ba10.33330.66670.02342 (13)0.0133 (2)
Ba20.20359 (3)0.40719 (6)0.62927 (8)0.01196 (14)
I10.53228 (3)0.46772 (3)0.82627 (8)0.01280 (15)
I20.13667 (3)0.27334 (6)0.01355 (8)0.01651 (16)
O0.33330.66670.7212 (15)0.010 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba10.0142 (3)0.0142 (3)0.0113 (5)0.00711 (15)0.0000.000
Ba20.0109 (2)0.0100 (3)0.0147 (3)0.00499 (14)0.00039 (13)0.0008 (3)
I10.0127 (2)0.0127 (2)0.0130 (3)0.0064 (3)0.00047 (14)0.00047 (14)
I20.0126 (2)0.0184 (3)0.0204 (3)0.00919 (17)0.00145 (15)0.0029 (3)
O0.008 (3)0.008 (3)0.013 (6)0.0041 (16)0.0000.000
Geometric parameters (Å, º) top
Ba1—Oi2.542 (12)Ba2—I1v3.6781 (15)
Ba1—I1ii3.5848 (17)Ba2—I13.6781 (15)
Ba1—I1iii3.5848 (17)Ba2—Ba1ix4.113 (2)
Ba1—I1iv3.5848 (17)Ba2—Ba2vi4.218 (2)
Ba1—I2v3.6927 (18)Ba2—Ba2v4.218 (2)
Ba1—I2vi3.6927 (18)I1—Ba2x3.5560 (15)
Ba1—I23.6927 (18)I1—Ba2xii3.5560 (15)
Ba1—Ba2vii4.113 (2)I1—Ba1xii3.5848 (17)
Ba1—Ba2i4.113 (2)I1—Ba2vi3.6781 (15)
Ba1—Ba2viii4.113 (2)I2—Ba2i3.467 (2)
Ba2—O2.555 (4)I2—Ba2iii3.5115 (16)
Ba2—I2ix3.467 (2)I2—Ba2xiii3.5115 (16)
Ba2—I2x3.5115 (16)O—Ba1ix2.542 (12)
Ba2—I2xi3.5115 (16)O—Ba2v2.555 (4)
Ba2—I1iii3.5560 (15)O—Ba2vi2.555 (4)
Ba2—I1iv3.5560 (15)
Oi—Ba1—I1ii135.27 (3)I2ix—Ba2—I1v68.66 (2)
Oi—Ba1—I1iii135.27 (3)I2x—Ba2—I1v142.459 (19)
I1ii—Ba1—I1iii75.10 (4)I2xi—Ba2—I1v71.35 (2)
Oi—Ba1—I1iv135.27 (3)I1iii—Ba2—I1v74.43 (4)
I1ii—Ba1—I1iv75.10 (4)I1iv—Ba2—I1v144.294 (19)
I1iii—Ba1—I1iv75.10 (4)O—Ba2—I173.53 (11)
Oi—Ba1—I2v88.71 (2)I2ix—Ba2—I168.66 (2)
I1ii—Ba1—I2v70.379 (15)I2x—Ba2—I171.35 (2)
I1iii—Ba1—I2v70.379 (16)I2xi—Ba2—I1142.459 (19)
I1iv—Ba1—I2v136.01 (4)I1iii—Ba2—I1144.29 (2)
Oi—Ba1—I2vi88.71 (2)I1iv—Ba2—I174.43 (4)
I1ii—Ba1—I2vi70.379 (16)I1v—Ba2—I1123.13 (4)
I1iii—Ba1—I2vi136.01 (4)O—Ba2—Ba1ix36.1 (3)
I1iv—Ba1—I2vi70.379 (16)I2ix—Ba2—Ba1ix57.55 (4)
I2v—Ba1—I2vi119.950 (2)I2x—Ba2—Ba1ix130.653 (17)
Oi—Ba1—I288.71 (2)I2xi—Ba2—Ba1ix130.653 (17)
I1ii—Ba1—I2136.01 (4)I1iii—Ba2—Ba1ix112.46 (4)
I1iii—Ba1—I270.379 (16)I1iv—Ba2—Ba1ix112.46 (4)
I1iv—Ba1—I270.379 (16)I1v—Ba2—Ba1ix62.97 (2)
I2v—Ba1—I2119.950 (2)I1—Ba2—Ba1ix62.97 (2)
I2vi—Ba1—I2119.950 (2)O—Ba2—Ba2vi34.36 (12)
Oi—Ba1—Ba2vii36.31 (2)I2ix—Ba2—Ba2vi108.287 (17)
I1ii—Ba1—Ba2vii111.36 (4)I2x—Ba2—Ba2vi108.049 (12)
I1iii—Ba1—Ba2vii111.36 (4)I2xi—Ba2—Ba2vi160.488 (17)
I1iv—Ba1—Ba2vii171.58 (2)I1iii—Ba2—Ba2vi91.216 (11)
I2v—Ba1—Ba2vii52.41 (3)I1iv—Ba2—Ba2vi53.62 (2)
I2vi—Ba1—Ba2vii106.13 (2)I1v—Ba2—Ba2vi107.812 (11)
I2—Ba1—Ba2vii106.13 (2)I1—Ba2—Ba2vi55.009 (12)
Oi—Ba1—Ba2i36.31 (2)Ba1ix—Ba2—Ba2vi59.152 (19)
I1ii—Ba1—Ba2i171.58 (2)O—Ba2—Ba2v34.36 (12)
I1iii—Ba1—Ba2i111.36 (4)I2ix—Ba2—Ba2v108.287 (17)
I1iv—Ba1—Ba2i111.36 (4)I2x—Ba2—Ba2v160.488 (17)
I2v—Ba1—Ba2i106.13 (2)I2xi—Ba2—Ba2v108.049 (12)
I2vi—Ba1—Ba2i106.13 (2)I1iii—Ba2—Ba2v53.62 (2)
I2—Ba1—Ba2i52.41 (3)I1iv—Ba2—Ba2v91.216 (11)
Ba2vii—Ba1—Ba2i61.70 (4)I1v—Ba2—Ba2v55.009 (12)
Oi—Ba1—Ba2viii36.31 (2)I1—Ba2—Ba2v107.812 (11)
I1ii—Ba1—Ba2viii111.36 (4)Ba1ix—Ba2—Ba2v59.152 (19)
I1iii—Ba1—Ba2viii171.58 (2)Ba2vi—Ba2—Ba2v60.0
I1iv—Ba1—Ba2viii111.36 (4)Ba2x—I1—Ba2xii72.76 (4)
I2v—Ba1—Ba2viii106.13 (2)Ba2x—I1—Ba1xii104.53 (4)
I2vi—Ba1—Ba2viii52.41 (3)Ba2xii—I1—Ba1xii104.53 (4)
I2—Ba1—Ba2viii106.13 (2)Ba2x—I1—Ba2vi156.07 (2)
Ba2vii—Ba1—Ba2viii61.70 (4)Ba2xii—I1—Ba2vi103.52 (3)
Ba2i—Ba1—Ba2viii61.70 (4)Ba1xii—I1—Ba2vi99.29 (4)
O—Ba2—I2ix93.6 (3)Ba2x—I1—Ba2103.52 (3)
O—Ba2—I2x140.63 (2)Ba2xii—I1—Ba2156.07 (2)
I2ix—Ba2—I2x89.79 (3)Ba1xii—I1—Ba299.29 (4)
O—Ba2—I2xi140.63 (2)Ba2vi—I1—Ba269.98 (2)
I2ix—Ba2—I2xi89.79 (3)Ba2i—I2—Ba2iii109.018 (17)
I2x—Ba2—I2xi78.50 (2)Ba2i—I2—Ba2xiii109.018 (17)
O—Ba2—I1iii84.4 (2)Ba2iii—I2—Ba2xiii140.98 (3)
I2ix—Ba2—I1iii141.96 (2)Ba2i—I2—Ba170.05 (3)
I2x—Ba2—I1iii115.40 (4)Ba2iii—I2—Ba1100.378 (13)
I2xi—Ba2—I1iii69.600 (17)Ba2xiii—I2—Ba1100.378 (13)
O—Ba2—I1iv84.4 (2)Ba1ix—O—Ba2v107.6 (3)
I2ix—Ba2—I1iv141.96 (2)Ba1ix—O—Ba2107.6 (3)
I2x—Ba2—I1iv69.600 (17)Ba2v—O—Ba2111.3 (2)
I2xi—Ba2—I1iv115.40 (4)Ba1ix—O—Ba2vi107.6 (3)
I1iii—Ba2—I1iv75.81 (4)Ba2v—O—Ba2vi111.3 (2)
O—Ba2—I1v73.53 (11)Ba2—O—Ba2vi111.3 (2)
Symmetry codes: (i) x, y, z1; (ii) y, x+y+1, z1/2; (iii) xy, x, z1/2; (iv) x+1, y+1, z1/2; (v) x+y, x+1, z; (vi) y+1, xy+1, z; (vii) x+y, x+1, z1; (viii) y+1, xy+1, z1; (ix) x, y, z+1; (x) y, x+y, z+1/2; (xi) xy, x, z+1/2; (xii) x+1, y+1, z+1/2; (xiii) y, x+y, z1/2.
 

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