Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680401075X/wm6017sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680401075X/wm6017Isup2.hkl |
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 1999); program(s) used to solve structure: SHELXTL (Sheldrick, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXTL.
EuBrI | F(000) = 604 |
Mr = 358.77 | Dx = 6.128 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 4924 reflections |
a = 8.3723 (18) Å | θ = 3.2–28.4° |
b = 4.7404 (11) Å | µ = 34.08 mm−1 |
c = 9.799 (2) Å | T = 293 K |
V = 388.89 (15) Å3 | Block, pink |
Z = 4 | 0.08 × 0.06 × 0.03 mm |
Bruker AXS APEX CCD diffractometer | 546 independent reflections |
Radiation source: fine-focus sealed tube | 429 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.072 |
ω scans | θmax = 28.4°, θmin = 3.2° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.100, Tmax = 0.360 | k = −6→6 |
4924 measured reflections | l = −13→13 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: isomorphous structure methods |
R[F2 > 2σ(F2)] = 0.038 | w = 1/[σ2(Fo2) + (0.0239P)2 + 11.5746P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.080 | (Δ/σ)max < 0.001 |
S = 1.08 | Δρmax = 1.58 e Å−3 |
546 reflections | Δρmin = −2.17 e Å−3 |
19 parameters |
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. PLAT731 Type_1 Test for consistency of Bond su's and Coordinate su's in CIF A large ratio of the reported and calculated bond s.u.'s is found. The use of a DFIX instruction might cause such a warning since calculated s.u.'s are based on reported variances only. Note_1: su's on the unitcell dimensions are taken into account in the calculation of expected su's. This may result in large differences between expected and reported su's when this contribution is not included in the reported su's, in particular for inaccurate unitcells. Note_2: Another source for the discrepancy between calculated and reported su's can be that the validation software has access only to the variances of the refined parameters as opposed to the full co-variance matrix used by e.g. SHELXL for the calculation of derived parameters with associated su's. Constrained/restrained refinement may cause largei co-variances. |
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 | ||
Eu | 0.72653 (10) | 0.7500 | 0.37198 (9) | 0.0242 (2) | |
I | 1.02693 (14) | 0.2500 | 0.33271 (11) | 0.0243 (3) | |
Br | 0.6442 (2) | 0.2500 | 0.5642 (2) | 0.0312 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Eu | 0.0240 (5) | 0.0219 (4) | 0.0267 (4) | 0.000 | 0.0028 (4) | 0.000 |
I | 0.0247 (6) | 0.0238 (5) | 0.0245 (5) | 0.000 | −0.0005 (4) | 0.000 |
Br | 0.0285 (10) | 0.0315 (9) | 0.0337 (9) | 0.000 | 0.0014 (7) | 0.000 |
Eu—Bri | 3.1049 (15) | Eu—Ivi | 3.5544 (15) |
Eu—Br | 3.1049 (15) | I—Euvii | 3.4772 (12) |
Eu—Brii | 3.166 (2) | I—Euviii | 3.5261 (12) |
Eu—Briii | 3.204 (2) | I—Euix | 3.5261 (12) |
Eu—Ii | 3.4772 (12) | I—Euvi | 3.5544 (15) |
Eu—I | 3.4772 (12) | Br—Euvii | 3.1049 (15) |
Eu—Iiv | 3.5261 (12) | Br—Euii | 3.166 (2) |
Eu—Iv | 3.5261 (12) | Br—Eux | 3.204 (2) |
Bri—Eu—Br | 99.52 (6) | I—Eu—Iv | 137.56 (3) |
Bri—Eu—Brii | 70.27 (5) | Iiv—Eu—Iv | 84.47 (3) |
Br—Eu—Brii | 70.27 (5) | Bri—Eu—Ivi | 68.60 (4) |
Bri—Eu—Briii | 130.24 (3) | Br—Eu—Ivi | 68.60 (4) |
Br—Eu—Briii | 130.24 (3) | Brii—Eu—Ivi | 114.11 (5) |
Brii—Eu—Briii | 121.14 (5) | Briii—Eu—Ivi | 124.75 (5) |
Bri—Eu—Ii | 72.99 (4) | Ii—Eu—Ivi | 70.74 (3) |
Br—Eu—Ii | 138.42 (5) | I—Eu—Ivi | 70.74 (3) |
Brii—Eu—Ii | 136.960 (18) | Iiv—Eu—Ivi | 137.587 (19) |
Briii—Eu—Ii | 69.61 (3) | Iv—Eu—Ivi | 137.587 (19) |
Bri—Eu—I | 138.42 (5) | Euvii—I—Eu | 85.94 (4) |
Br—Eu—I | 72.99 (4) | Euvii—I—Euviii | 86.99 (2) |
Brii—Eu—I | 136.960 (18) | Eu—I—Euviii | 149.76 (4) |
Briii—Eu—I | 69.61 (3) | Euvii—I—Euix | 149.76 (4) |
Ii—Eu—I | 85.94 (4) | Eu—I—Euix | 86.99 (2) |
Bri—Eu—Iiv | 138.84 (5) | Euviii—I—Euix | 84.47 (3) |
Br—Eu—Iiv | 74.14 (4) | Euvii—I—Euvi | 109.26 (3) |
Brii—Eu—Iiv | 69.38 (3) | Eu—I—Euvi | 109.26 (3) |
Briii—Eu—Iiv | 67.96 (3) | Euviii—I—Euvi | 100.83 (3) |
Ii—Eu—Iiv | 137.56 (3) | Euix—I—Euvi | 100.83 (3) |
I—Eu—Iiv | 79.73 (2) | Euvii—Br—Eu | 99.52 (6) |
Bri—Eu—Iv | 74.14 (4) | Euvii—Br—Euii | 109.73 (5) |
Br—Eu—Iv | 138.84 (5) | Eu—Br—Euii | 109.73 (5) |
Brii—Eu—Iv | 69.38 (3) | Euvii—Br—Eux | 119.73 (4) |
Briii—Eu—Iv | 67.96 (3) | Eu—Br—Eux | 119.73 (4) |
Ii—Eu—Iv | 79.73 (2) | Euii—Br—Eux | 98.35 (5) |
Symmetry codes: (i) x, y+1, z; (ii) −x+1, −y+1, −z+1; (iii) −x+3/2, −y+1, z−1/2; (iv) x−1/2, y, −z+1/2; (v) x−1/2, y+1, −z+1/2; (vi) −x+2, −y+1, −z+1; (vii) x, y−1, z; (viii) x+1/2, y−1, −z+1/2; (ix) x+1/2, y, −z+1/2; (x) −x+3/2, −y+1, z+1/2. |