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[Sc(H2O)5(OH)]Br2 is a scand­ium(III) halide compound that contains centrosymmetric [Sc(H2O)5(OH)]24+ dimeric cationic units built from two edge-sharing (hydroxo-bridged) symmetrically equivalent Sc(H2O)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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806013328/wm2011sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806013328/wm2011Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](c-O) = 0.002 Å
  • R factor = 0.030
  • wR factor = 0.073
  • Data-to-parameter ratio = 32.1

checkCIF/PLATON results

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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

Computing details top

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)]Br2Z = 2
Mr = 311.87F(000) = 300
Triclinic, P1Dx = 2.212 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.412 (1) ÅCell parameters from 4082 reflections
b = 8.368 (2) Åθ = 2.0–35.0°
c = 8.627 (2) ŵ = 9.29 mm1
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 tube3219 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
φ and ω scansθmax = 34.9°, θmin = 2.5°
Absorption correction: multi-scan
(SCALEPACK; Otwinowski et al., 2003)
h = 1111
Tmin = 0.301, Tmax = 0.457k = 1313
8112 measured reflectionsl = 1313
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030All 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 reflectionsΔρmax = 0.98 e Å3
127 parametersΔρmin = 0.87 e Å3
11 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction 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
xyzUiso*/Ueq
Sc0.87962 (5)0.15841 (4)0.32614 (4)0.02076 (7)
Br10.86413 (3)0.31138 (2)0.08405 (3)0.03305 (7)
Br20.46366 (3)0.24920 (3)0.30388 (3)0.03492 (7)
O11.0337 (2)0.09827 (16)0.59158 (16)0.0285 (3)
O21.0504 (4)0.0777 (2)0.1840 (3)0.0604 (6)
O30.5988 (3)0.0878 (2)0.1780 (3)0.0517 (5)
O40.6694 (3)0.3377 (2)0.3869 (3)0.0561 (6)
O51.0651 (3)0.3407 (3)0.3758 (2)0.0576 (6)
O60.7160 (2)0.34896 (19)0.08302 (18)0.0327 (3)
H11.057 (4)0.168 (3)0.659 (3)0.052 (8)*
H21.094 (5)0.140 (4)0.129 (5)0.082 (12)*
H31.136 (4)0.020 (3)0.211 (5)0.067 (10)*
H40.471 (3)0.152 (4)0.114 (4)0.084 (12)*
H50.589 (6)0.010 (3)0.219 (5)0.073 (11)*
H60.603 (5)0.442 (3)0.339 (4)0.071 (11)*
H70.636 (6)0.321 (5)0.473 (4)0.082 (12)*
H81.186 (4)0.329 (5)0.464 (4)0.089 (13)*
H91.046 (6)0.429 (4)0.306 (5)0.097 (14)*
H100.663 (5)0.328 (5)0.024 (3)0.074 (11)*
H110.727 (7)0.447 (3)0.051 (6)0.113 (16)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sc0.02461 (16)0.01590 (14)0.01799 (13)0.00331 (11)0.00755 (11)0.00107 (10)
Br10.04039 (12)0.02452 (10)0.03456 (11)0.00948 (8)0.01708 (9)0.00238 (7)
Br20.03351 (12)0.03616 (12)0.03264 (11)0.00742 (8)0.01359 (8)0.00380 (8)
O10.0444 (8)0.0154 (6)0.0186 (5)0.0057 (5)0.0084 (5)0.0017 (4)
O20.0841 (15)0.0335 (10)0.0798 (14)0.0117 (9)0.0683 (13)0.0146 (9)
O30.0320 (8)0.0289 (9)0.0679 (12)0.0117 (7)0.0008 (8)0.0099 (8)
O40.0762 (14)0.0370 (10)0.0501 (11)0.0208 (9)0.0423 (11)0.0095 (8)
O50.0561 (11)0.0486 (11)0.0402 (9)0.0329 (9)0.0085 (8)0.0169 (8)
O60.0403 (8)0.0248 (7)0.0236 (6)0.0099 (6)0.0061 (6)0.0037 (5)
Geometric parameters (Å, º) top
Sc—O12.0485 (15)Br2—O5i3.312 (2)
Sc—O1i2.0824 (15)Br2—O4iii3.371 (2)
Sc—O22.1591 (19)Br2—O2vii3.392 (2)
Sc—O32.1724 (19)Br2—O33.407 (2)
Sc—O52.2024 (19)Br2—O1i3.9428 (18)
Sc—O42.2032 (19)Br2—O3iv4.059 (3)
Sc—O62.2228 (18)Br2—O1vi4.1398 (18)
Br1—O2ii3.236 (2)O1—H10.853 (17)
Br1—O6iii3.2413 (18)O2—H20.866 (18)
Br1—O3iv3.265 (2)O2—H30.879 (18)
Br1—O5iii3.302 (2)O3—H40.894 (18)
Br1—O1i3.3532 (17)O3—H50.890 (18)
Br1—O23.812 (3)O4—H60.877 (18)
Br1—O33.862 (2)O4—H70.883 (18)
Br1—O6ii3.9096 (18)O5—H80.880 (18)
Br1—O6iv4.0159 (18)O5—H90.859 (19)
Br1—Br1v4.1076 (13)O6—H100.888 (18)
Br2—O4vi3.280 (2)O6—H110.871 (19)
Br2—O6iv3.2940 (18)
O1—Sc—O1i69.77 (7)O2—Sc—O678.53 (8)
O1—Sc—O2116.94 (8)O3—Sc—O675.36 (7)
O1i—Sc—O278.21 (7)O5—Sc—O676.73 (7)
O1—Sc—O3122.77 (8)O4—Sc—O677.78 (7)
O1i—Sc—O377.34 (7)Sc—O1—Sci110.23 (7)
O2—Sc—O399.66 (10)Sc—O1—H1125 (2)
O1—Sc—O580.16 (7)Sci—O1—H1124 (2)
O1i—Sc—O5130.56 (7)Sc—O2—H2126 (3)
O2—Sc—O581.97 (10)Sc—O2—H3124 (2)
O3—Sc—O5151.08 (7)Sc—O3—H4129 (3)
O1—Sc—O481.42 (8)Sc—O3—H5117 (2)
O1i—Sc—O4125.90 (7)Sc—O4—H6131 (2)
O2—Sc—O4155.04 (7)Sc—O4—H7127 (3)
O3—Sc—O481.82 (9)Sc—O5—H8127 (3)
O5—Sc—O485.07 (10)Sc—O5—H9128 (3)
O1—Sc—O6149.98 (6)Sc—O6—H10125 (2)
O1i—Sc—O6140.25 (6)Sc—O6—H11134 (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) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···Br1i0.85 (2)2.52 (2)3.3532 (17)165 (3)
O2—H2···Br1ii0.87 (2)2.39 (2)3.236 (2)165 (3)
O2—H3···Br2viii0.88 (2)2.54 (2)3.392 (2)162 (3)
O3—H4···Br1iv0.89 (2)2.38 (2)3.265 (2)173 (3)
O3—H5···Br20.89 (2)2.54 (2)3.407 (2)165 (3)
O4—H6···Br2ix0.88 (2)2.53 (2)3.371 (2)161 (3)
O4—H7···Br2vi0.88 (2)2.40 (2)3.280 (2)174 (4)
O5—H8···Br2i0.88 (2)2.44 (2)3.312 (2)170 (4)
O5—H9···Br1ix0.86 (2)2.48 (2)3.302 (2)160 (4)
O6—H10···Br2iv0.89 (2)2.41 (2)3.2940 (18)175 (3)
O6—H11···Br1ix0.87 (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, y1, z.
 

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