In the structure of the title compound, [Y(H
2O)
9](BrO
3)
3, the yttrium(III) ion is surrounded by six equidistant water molecules forming a trigonal prism, which is capped by three more distant water molecules. The Y
III ion lies on a special position (2
c) with crystallographically imposed
m2 symmetry. The title compound is isotypic with other [Ln(H
2O)
9](BrO
3)
3 (Ln = Pr, Sm, Tb and Yb) compounds, and the bromate anions are disordered in these structures. Relatively strong hydrogen bonds between the bromate anions and the water molecules stabilize the trigonal prism.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 291 K
- Mean (r-O) = 0.005 Å
- Disorder in main residue
- R factor = 0.029
- wR factor = 0.089
- Data-to-parameter ratio = 9.9
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT430_ALERT_2_A Short Inter D...A Contact O4 .. O4 .. 2.04 Ang.
| Author Response: This is explained in text
|
PLAT430_ALERT_2_A Short Inter D...A Contact O4 .. O4 .. 2.04 Ang.
| Author Response: This is explained in text
|
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . O4
PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.88
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.62 Ratio
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Y
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Br
PLAT301_ALERT_3_C Main Residue Disorder ......................... 7.00 Perc.
PLAT431_ALERT_2_C Short Inter HL..A Contact Br .. O4 .. 3.09 Ang.
PLAT431_ALERT_2_C Short Inter HL..A Contact Br .. O4 .. 3.09 Ang.
PLAT431_ALERT_2_C Short Inter HL..A Contact Br .. O4 .. 3.09 Ang.
PLAT431_ALERT_2_C Short Inter HL..A Contact Br .. O4 .. 3.09 Ang.
2 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
11 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
9 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: EXPOSE in IPDS (Stoe & Cie, 1997); cell refinement: CELL in IPDS; data reduction: INTEGRATE in IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.
Nonaaquayttrium(III) tris[bromate(V)]
top
Crystal data top
[Y(H2O)9](BrO3)3 | Dx = 2.649 Mg m−3 |
Mr = 634.78 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63/mmc | Cell parameters from 1421 reflections |
Hall symbol: -P 6c 2c | θ = 5.1–25.8° |
a = 11.7237 (16) Å | µ = 11.28 mm−1 |
c = 6.6855 (9) Å | T = 291 K |
V = 795.78 (19) Å3 | Needle, colourless |
Z = 2 | 0.40 × 0.10 × 0.08 mm |
F(000) = 612 | |
Data collection top
Stoe IPDS diffractometer | 336 independent reflections |
Radiation source: fine-focus sealed tube | 311 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.085 |
Detector resolution: 6.7 pixels mm-1 | θmax = 26.2°, θmin = 2.0° |
area–detector φ scans | h = −14→14 |
Absorption correction: numerical (X-RED; Stoe & Cie, 1997) | k = −14→14 |
Tmin = 0.01, Tmax = 0.40 | l = −8→8 |
12059 measured reflections | |
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)] = 0.029 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.089 | Only H-atom coordinates refined |
S = 1.23 | w = 1/[σ2(Fo2) + (0.0398P)2 + 3.0946P] where P = (Fo2 + 2Fc2)/3 |
336 reflections | (Δ/σ)max < 0.001 |
34 parameters | Δρmax = 0.70 e Å−3 |
0 restraints | Δρmin = −0.62 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y | 0.3333 | 0.6667 | 0.2500 | 0.0179 (4) | |
O1 | 0.2135 (3) | 0.4269 (6) | 0.2500 | 0.0365 (17) | |
H1 | 0.142 (7) | 0.383 (8) | 0.2500 | 0.044* | |
O2 | 0.4194 (2) | 0.8388 (5) | 0.0103 (7) | 0.0321 (10) | |
H2 | 0.486 (4) | 0.867 (5) | −0.048 (8) | 0.039* | |
Br | 0.13043 (4) | 0.26086 (8) | 0.7500 | 0.0355 (4) | |
O3 | 0.2919 (4) | 0.3609 (4) | 0.7500 | 0.0303 (10) | |
O4 | 0.0960 (7) | 0.1920 (13) | 0.954 (3) | 0.079 (5) | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y | 0.0170 (4) | 0.0170 (4) | 0.0199 (6) | 0.0085 (2) | 0.000 | 0.000 |
O1 | 0.024 (2) | 0.016 (3) | 0.067 (5) | 0.0081 (15) | 0.000 | 0.000 |
O2 | 0.0275 (15) | 0.037 (2) | 0.035 (2) | 0.0184 (12) | 0.0080 (10) | 0.016 (2) |
Br | 0.0202 (4) | 0.0230 (5) | 0.0641 (7) | 0.0115 (3) | 0.000 | 0.000 |
O3 | 0.019 (2) | 0.031 (2) | 0.039 (2) | 0.0113 (17) | 0.000 | 0.000 |
O4 | 0.048 (4) | 0.070 (8) | 0.126 (13) | 0.035 (4) | 0.035 (5) | 0.069 (9) |
Geometric parameters (Å, º) top
Y—O1i | 2.434 (7) | Y—O2i | 2.371 (4) |
Y—O1 | 2.434 (7) | O1—H1 | 0.73 (8) |
Y—O1ii | 2.434 (7) | O2—H2 | 0.78 (5) |
Y—O2iii | 2.371 (4) | Br—O4vi | 1.533 (15) |
Y—O2ii | 2.371 (4) | Br—O4 | 1.533 (15) |
Y—O2iv | 2.371 (4) | Br—O3vii | 1.655 (4) |
Y—O2 | 2.371 (4) | Br—O3 | 1.655 (4) |
Y—O2v | 2.371 (4) | | |
| | | |
O2iii—Y—O2ii | 136.76 (9) | O2ii—Y—O1 | 68.38 (4) |
O2iii—Y—O2iv | 79.31 (18) | O2iv—Y—O1 | 68.38 (4) |
O2ii—Y—O2iv | 85.1 (2) | O2—Y—O1 | 137.47 (12) |
O2iii—Y—O2 | 85.1 (2) | O2v—Y—O1 | 68.38 (4) |
O2ii—Y—O2 | 79.31 (18) | O2i—Y—O1 | 68.38 (4) |
O2iv—Y—O2 | 136.76 (9) | O1i—Y—O1 | 120.0 |
O2iii—Y—O2v | 79.31 (18) | O2iii—Y—O1ii | 68.38 (4) |
O2ii—Y—O2v | 136.76 (9) | O2ii—Y—O1ii | 137.47 (12) |
O2iv—Y—O2v | 79.31 (18) | O2iv—Y—O1ii | 137.47 (12) |
O2—Y—O2v | 136.76 (9) | O2—Y—O1ii | 68.38 (4) |
O2iii—Y—O2i | 136.76 (9) | O2v—Y—O1ii | 68.38 (4) |
O2ii—Y—O2i | 79.31 (18) | O2i—Y—O1ii | 68.38 (4) |
O2iv—Y—O2i | 136.76 (9) | O1i—Y—O1ii | 120.000 (1) |
O2—Y—O2i | 79.31 (18) | O1—Y—O1ii | 120.0 |
O2v—Y—O2i | 85.1 (2) | Y—O1—H1 | 128 (6) |
O2iii—Y—O1i | 68.38 (4) | Y—O2—H2 | 127 (4) |
O2ii—Y—O1i | 68.38 (4) | O4vi—Br—O4 | 125.7 (13) |
O2iv—Y—O1i | 68.38 (4) | O4vi—Br—O3vii | 106.3 (4) |
O2—Y—O1i | 68.38 (4) | O4—Br—O3vii | 106.3 (4) |
O2v—Y—O1i | 137.47 (12) | O4vi—Br—O3 | 106.3 (4) |
O2i—Y—O1i | 137.47 (12) | O4—Br—O3 | 106.3 (4) |
O2iii—Y—O1 | 137.47 (12) | O3vii—Br—O3 | 104.3 (3) |
Symmetry codes: (i) −x+y, −x+1, z; (ii) −y+1, x−y+1, z; (iii) x, y, −z+1/2; (iv) −y+1, x−y+1, −z+1/2; (v) −x+y, −x+1, −z+1/2; (vi) x, y, −z+3/2; (vii) −x+y, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O3viii | 0.73 (9) | 2.15 (9) | 2.869 (8) | 168 |
O2—H2···O3ix | 0.78 (5) | 2.06 (5) | 2.837 (6) | 169 |
Symmetry codes: (viii) x−y, x, −z+1; (ix) −y+1, x−y+1, z−1. |