Penta­aqua­hydroxoscandium(III) dibromide, [Sc(H₂O)₅(OH)]Br₂

[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.

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

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

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Computing details

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

Crystal data

[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) Å^3

Data collection

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

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.030	All H-atom parameters refined
wR(F^2) = 0.073	w = 1/[σ^2(Fo^2) + (0.034P)^2 + 0.15P] where P = (Fo^2 + 2Fc^2)/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+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0166 (13)

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Sc—O1	2.0485 (15)	Br2—O5^i	3.312 (2)
Sc—O1^i	2.0824 (15)	Br2—O4^iii	3.371 (2)
Sc—O2	2.1591 (19)	Br2—O2^vii	3.392 (2)
Sc—O3	2.1724 (19)	Br2—O3	3.407 (2)
Sc—O5	2.2024 (19)	Br2—O1^i	3.9428 (18)
Sc—O4	2.2032 (19)	Br2—O3^iv	4.059 (3)
Sc—O6	2.2228 (18)	Br2—O1^vi	4.1398 (18)
Br1—O2^ii	3.236 (2)	O1—H1	0.853 (17)
Br1—O6^iii	3.2413 (18)	O2—H2	0.866 (18)
Br1—O3^iv	3.265 (2)	O2—H3	0.879 (18)
Br1—O5^iii	3.302 (2)	O3—H4	0.894 (18)
Br1—O1^i	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—O6^ii	3.9096 (18)	O5—H8	0.880 (18)
Br1—O6^iv	4.0159 (18)	O5—H9	0.859 (19)
Br1—Br1^v	4.1076 (13)	O6—H10	0.888 (18)
Br2—O4^vi	3.280 (2)	O6—H11	0.871 (19)
Br2—O6^iv	3.2940 (18)
O1—Sc—O1^i	69.77 (7)	O2—Sc—O6	78.53 (8)
O1—Sc—O2	116.94 (8)	O3—Sc—O6	75.36 (7)
O1^i—Sc—O2	78.21 (7)	O5—Sc—O6	76.73 (7)
O1—Sc—O3	122.77 (8)	O4—Sc—O6	77.78 (7)
O1^i—Sc—O3	77.34 (7)	Sc—O1—Sc^i	110.23 (7)
O2—Sc—O3	99.66 (10)	Sc—O1—H1	125 (2)
O1—Sc—O5	80.16 (7)	Sc^i—O1—H1	124 (2)
O1^i—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)
O1^i—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)
O1^i—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)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···Br1^i	0.85 (2)	2.52 (2)	3.3532 (17)	165 (3)
O2—H2···Br1^ii	0.87 (2)	2.39 (2)	3.236 (2)	165 (3)
O2—H3···Br2^viii	0.88 (2)	2.54 (2)	3.392 (2)	162 (3)
O3—H4···Br1^iv	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···Br2^ix	0.88 (2)	2.53 (2)	3.371 (2)	161 (3)
O4—H7···Br2^vi	0.88 (2)	2.40 (2)	3.280 (2)	174 (4)
O5—H8···Br2^i	0.88 (2)	2.44 (2)	3.312 (2)	170 (4)
O5—H9···Br1^ix	0.86 (2)	2.48 (2)	3.302 (2)	160 (4)
O6—H10···Br2^iv	0.89 (2)	2.41 (2)	3.2940 (18)	175 (3)
O6—H11···Br1^ix	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.