[Sc(H
2O)
5(OH)]Br
2 is a scandium(III) halide compound that contains centrosymmetric [Sc(H
2O)
5(OH)]
24+ dimeric cationic units built from two edge-sharing (hydroxo-bridged) symmetrically equivalent Sc(H
2O)
5(OH)
2 polyhedra. The mean Sc—O bond length is 2.156 Å. The hydrogen bonds (O
Br) are of low strength. All atoms are in general positions.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (c-O) = 0.002 Å
- R factor = 0.030
- wR factor = 0.073
- Data-to-parameter ratio = 32.1
checkCIF/PLATON results
No syntax errors found
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
Tmin and Tmax reported: 0.301 0.457
Tmin and Tmax expected: 0.221 0.395
RR = 1.179
Please check that your absorption correction is appropriate.
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.16
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.86
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Sc - O6 .. 5.19 su
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Sc
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.53
PLAT731_ALERT_1_C Bond Calc 0.87(4), Rep 0.866(18) ...... 2.22 su-Rat
O2 -H2 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.88(4), Rep 0.883(18) ...... 2.22 su-Rat
O4 -H7 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.86(4), Rep 0.859(19) ...... 2.11 su-Rat
O5 -H9 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.87(4), Rep 0.871(19) ...... 2.11 su-Rat
O6 -H11 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.87(4), Rep 0.866(18) ...... 2.22 su-Rat
O2 -H2 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.88(4), Rep 0.883(18) ...... 2.22 su-Rat
O4 -H7 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.86(4), Rep 0.859(19) ...... 2.11 su-Rat
O5 -H9 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.87(4), Rep 0.871(19) ...... 2.11 su-Rat
O6 -H11 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 2.40(4), Rep 2.401(19) ...... 2.11 su-Rat
H7 -BR2 1.555 2.656
Alert level G
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 0.864
Tmax scaled 0.395 Tmin scaled 0.260
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
19 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
13 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 2004); cell refinement: SCALEPACK (Otwinowski et al., 2003); data reduction: SCALEPACK and DENZO (Otwinowski et al., 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 1999) and ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
Pentaaquahydroxoscandium(III) dibromide
top
Crystal data top
[Sc(H2O)5(OH)]Br2 | Z = 2 |
Mr = 311.87 | F(000) = 300 |
Triclinic, P1 | Dx = 2.212 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.412 (1) Å | Cell parameters from 4082 reflections |
b = 8.368 (2) Å | θ = 2.0–35.0° |
c = 8.627 (2) Å | µ = 9.29 mm−1 |
α = 95.12 (3)° | T = 293 K |
β = 114.56 (3)° | Fragment, colourless |
γ = 101.33 (3)° | 0.17 × 0.15 × 0.10 mm |
V = 468.3 (2) Å3 | |
Data collection top
Nonius KappaCCD area-detector diffractometer | 4082 independent reflections |
Radiation source: fine-focus sealed tube | 3219 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
φ and ω scans | θmax = 34.9°, θmin = 2.5° |
Absorption correction: multi-scan (SCALEPACK; Otwinowski et al., 2003) | h = −11→11 |
Tmin = 0.301, Tmax = 0.457 | k = −13→13 |
8112 measured reflections | l = −13→13 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.030 | All H-atom parameters refined |
wR(F2) = 0.073 | w = 1/[σ2(Fo2) + (0.034P)2 + 0.15P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.001 |
4082 reflections | Δρmax = 0.98 e Å−3 |
127 parameters | Δρmin = −0.87 e Å−3 |
11 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0166 (13) |
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 | |
Sc | 0.87962 (5) | −0.15841 (4) | 0.32614 (4) | 0.02076 (7) | |
Br1 | 0.86413 (3) | 0.31138 (2) | 0.08405 (3) | 0.03305 (7) | |
Br2 | 0.46366 (3) | 0.24920 (3) | 0.30388 (3) | 0.03492 (7) | |
O1 | 1.0337 (2) | −0.09827 (16) | 0.59158 (16) | 0.0285 (3) | |
O2 | 1.0504 (4) | −0.0777 (2) | 0.1840 (3) | 0.0604 (6) | |
O3 | 0.5988 (3) | −0.0878 (2) | 0.1780 (3) | 0.0517 (5) | |
O4 | 0.6694 (3) | −0.3377 (2) | 0.3869 (3) | 0.0561 (6) | |
O5 | 1.0651 (3) | −0.3407 (3) | 0.3758 (2) | 0.0576 (6) | |
O6 | 0.7160 (2) | −0.34896 (19) | 0.08302 (18) | 0.0327 (3) | |
H1 | 1.057 (4) | −0.168 (3) | 0.659 (3) | 0.052 (8)* | |
H2 | 1.094 (5) | −0.140 (4) | 0.129 (5) | 0.082 (12)* | |
H3 | 1.136 (4) | 0.020 (3) | 0.211 (5) | 0.067 (10)* | |
H4 | 0.471 (3) | −0.152 (4) | 0.114 (4) | 0.084 (12)* | |
H5 | 0.589 (6) | 0.010 (3) | 0.219 (5) | 0.073 (11)* | |
H6 | 0.603 (5) | −0.442 (3) | 0.339 (4) | 0.071 (11)* | |
H7 | 0.636 (6) | −0.321 (5) | 0.473 (4) | 0.082 (12)* | |
H8 | 1.186 (4) | −0.329 (5) | 0.464 (4) | 0.089 (13)* | |
H9 | 1.046 (6) | −0.429 (4) | 0.306 (5) | 0.097 (14)* | |
H10 | 0.663 (5) | −0.328 (5) | −0.024 (3) | 0.074 (11)* | |
H11 | 0.727 (7) | −0.447 (3) | 0.051 (6) | 0.113 (16)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sc | 0.02461 (16) | 0.01590 (14) | 0.01799 (13) | 0.00331 (11) | 0.00755 (11) | −0.00107 (10) |
Br1 | 0.04039 (12) | 0.02452 (10) | 0.03456 (11) | 0.00948 (8) | 0.01708 (9) | 0.00238 (7) |
Br2 | 0.03351 (12) | 0.03616 (12) | 0.03264 (11) | 0.00742 (8) | 0.01359 (8) | 0.00380 (8) |
O1 | 0.0444 (8) | 0.0154 (6) | 0.0186 (5) | 0.0057 (5) | 0.0084 (5) | 0.0017 (4) |
O2 | 0.0841 (15) | 0.0335 (10) | 0.0798 (14) | −0.0117 (9) | 0.0683 (13) | −0.0146 (9) |
O3 | 0.0320 (8) | 0.0289 (9) | 0.0679 (12) | 0.0117 (7) | −0.0008 (8) | −0.0099 (8) |
O4 | 0.0762 (14) | 0.0370 (10) | 0.0501 (11) | −0.0208 (9) | 0.0423 (11) | −0.0095 (8) |
O5 | 0.0561 (11) | 0.0486 (11) | 0.0402 (9) | 0.0329 (9) | −0.0085 (8) | −0.0169 (8) |
O6 | 0.0403 (8) | 0.0248 (7) | 0.0236 (6) | 0.0099 (6) | 0.0061 (6) | −0.0037 (5) |
Geometric parameters (Å, º) top
Sc—O1 | 2.0485 (15) | Br2—O5i | 3.312 (2) |
Sc—O1i | 2.0824 (15) | Br2—O4iii | 3.371 (2) |
Sc—O2 | 2.1591 (19) | Br2—O2vii | 3.392 (2) |
Sc—O3 | 2.1724 (19) | Br2—O3 | 3.407 (2) |
Sc—O5 | 2.2024 (19) | Br2—O1i | 3.9428 (18) |
Sc—O4 | 2.2032 (19) | Br2—O3iv | 4.059 (3) |
Sc—O6 | 2.2228 (18) | Br2—O1vi | 4.1398 (18) |
Br1—O2ii | 3.236 (2) | O1—H1 | 0.853 (17) |
Br1—O6iii | 3.2413 (18) | O2—H2 | 0.866 (18) |
Br1—O3iv | 3.265 (2) | O2—H3 | 0.879 (18) |
Br1—O5iii | 3.302 (2) | O3—H4 | 0.894 (18) |
Br1—O1i | 3.3532 (17) | O3—H5 | 0.890 (18) |
Br1—O2 | 3.812 (3) | O4—H6 | 0.877 (18) |
Br1—O3 | 3.862 (2) | O4—H7 | 0.883 (18) |
Br1—O6ii | 3.9096 (18) | O5—H8 | 0.880 (18) |
Br1—O6iv | 4.0159 (18) | O5—H9 | 0.859 (19) |
Br1—Br1v | 4.1076 (13) | O6—H10 | 0.888 (18) |
Br2—O4vi | 3.280 (2) | O6—H11 | 0.871 (19) |
Br2—O6iv | 3.2940 (18) | | |
| | | |
O1—Sc—O1i | 69.77 (7) | O2—Sc—O6 | 78.53 (8) |
O1—Sc—O2 | 116.94 (8) | O3—Sc—O6 | 75.36 (7) |
O1i—Sc—O2 | 78.21 (7) | O5—Sc—O6 | 76.73 (7) |
O1—Sc—O3 | 122.77 (8) | O4—Sc—O6 | 77.78 (7) |
O1i—Sc—O3 | 77.34 (7) | Sc—O1—Sci | 110.23 (7) |
O2—Sc—O3 | 99.66 (10) | Sc—O1—H1 | 125 (2) |
O1—Sc—O5 | 80.16 (7) | Sci—O1—H1 | 124 (2) |
O1i—Sc—O5 | 130.56 (7) | Sc—O2—H2 | 126 (3) |
O2—Sc—O5 | 81.97 (10) | Sc—O2—H3 | 124 (2) |
O3—Sc—O5 | 151.08 (7) | Sc—O3—H4 | 129 (3) |
O1—Sc—O4 | 81.42 (8) | Sc—O3—H5 | 117 (2) |
O1i—Sc—O4 | 125.90 (7) | Sc—O4—H6 | 131 (2) |
O2—Sc—O4 | 155.04 (7) | Sc—O4—H7 | 127 (3) |
O3—Sc—O4 | 81.82 (9) | Sc—O5—H8 | 127 (3) |
O5—Sc—O4 | 85.07 (10) | Sc—O5—H9 | 128 (3) |
O1—Sc—O6 | 149.98 (6) | Sc—O6—H10 | 125 (2) |
O1i—Sc—O6 | 140.25 (6) | Sc—O6—H11 | 134 (3) |
Symmetry codes: (i) −x+2, −y, −z+1; (ii) −x+2, −y, −z; (iii) x, y+1, z; (iv) −x+1, −y, −z; (v) −x+2, −y+1, −z; (vi) −x+1, −y, −z+1; (vii) x−1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···Br1i | 0.85 (2) | 2.52 (2) | 3.3532 (17) | 165 (3) |
O2—H2···Br1ii | 0.87 (2) | 2.39 (2) | 3.236 (2) | 165 (3) |
O2—H3···Br2viii | 0.88 (2) | 2.54 (2) | 3.392 (2) | 162 (3) |
O3—H4···Br1iv | 0.89 (2) | 2.38 (2) | 3.265 (2) | 173 (3) |
O3—H5···Br2 | 0.89 (2) | 2.54 (2) | 3.407 (2) | 165 (3) |
O4—H6···Br2ix | 0.88 (2) | 2.53 (2) | 3.371 (2) | 161 (3) |
O4—H7···Br2vi | 0.88 (2) | 2.40 (2) | 3.280 (2) | 174 (4) |
O5—H8···Br2i | 0.88 (2) | 2.44 (2) | 3.312 (2) | 170 (4) |
O5—H9···Br1ix | 0.86 (2) | 2.48 (2) | 3.302 (2) | 160 (4) |
O6—H10···Br2iv | 0.89 (2) | 2.41 (2) | 3.2940 (18) | 175 (3) |
O6—H11···Br1ix | 0.87 (2) | 2.42 (3) | 3.2413 (18) | 156 (4) |
Symmetry codes: (i) −x+2, −y, −z+1; (ii) −x+2, −y, −z; (iv) −x+1, −y, −z; (vi) −x+1, −y, −z+1; (viii) x+1, y, z; (ix) x, y−1, z. |