The title compound, [Sc2Br6(NH3)4], was obtained by the reaction of ammonium bromide, (NH4)Br, with scandium metal in a sealed tantalum container. The crystal structure contains isolated dimers of bromide edge-connected [Sc-mer-(NH3)3Br3] and [Sc(NH3)Br5] octahedra. Sc(NH3)2Br3 is isotypic with Sc(NH3)2Cl3.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Sc-N) = 0.010 Å
- R factor = 0.039
- wR factor = 0.081
- Data-to-parameter ratio = 26.5
checkCIF/PLATON results
No syntax errors found
Alert level C
GOODF01_ALERT_2_C The least squares goodness of fit parameter lies
outside the range 0.80 <> 2.00
Goodness of fit given = 0.700
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT420_ALERT_2_C D-H Without Acceptor N11 - H11B ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N11 - H11C ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N12 - H12A ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N13 - H13A ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N13 - H13B ... ?
PLAT431_ALERT_2_C Short Inter HL..A Contact Br1 .. Br2 = 3.60 Ang.
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
9 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
7 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996); software used to prepare material for publication: SHELXL97.
Tetraamminehexabromodiscandium(III)
top
Crystal data top
[Sc2Br6(NH3)4] | Z = 2 |
Mr = 637.52 | F(000) = 584 |
Triclinic, P1 | Dx = 2.827 Mg m−3 |
Hall symbol: -P 1 | Melting point: unknown K |
a = 7.211 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.157 (3) Å | Cell parameters from 2678 reflections |
c = 11.350 (3) Å | θ = 1.9–29.7° |
α = 105.39 (2)° | µ = 16.88 mm−1 |
β = 90.76 (2)° | T = 293 K |
γ = 109.85 (2)° | Column, colourless |
V = 749.0 (4) Å3 | 0.2 × 0.1 × 0.1 mm |
Data collection top
Stoe IPDS II diffractometer | 2938 independent reflections |
Radiation source: fine-focus sealed tube | 1237 reflections with I > 2s(I) |
Graphite monochromator | Rint = 0.077 |
Detector resolution: not measured pixels mm-1 | θmax = 26.0°, θmin = 1.9° |
ω and φ scans | h = −8→8 |
Absorption correction: numerical the absorption correction (X-RED; Stoe & Cie, 2001) was performed after
optimizing the crystal shape using X-SHAPE (Stoe & Cie, 1999) | k = −12→12 |
Tmin = 0.100, Tmax = 0.148 | l = −13→13 |
6953 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.039 | H-atom parameters constrained |
wR(F2) = 0.081 | w = 1/[σ2(Fo2) + (0.0201P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.70 | (Δ/σ)max < 0.001 |
2938 reflections | Δρmax = 0.66 e Å−3 |
111 parameters | Δρmin = −0.70 e Å−3 |
0 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: 0.00190 (15) |
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 | |
Br21 | 0.1258 (2) | 0.40251 (16) | 0.34540 (12) | 0.0546 (4) | |
Br11 | −0.14637 (19) | −0.42322 (15) | 0.13769 (11) | 0.0521 (4) | |
Br1 | −0.0130 (2) | −0.01176 (15) | 0.24330 (12) | 0.0481 (3) | |
Br2 | 0.5115 (2) | 0.02968 (14) | 0.25850 (12) | 0.0486 (4) | |
Br23 | 0.33607 (19) | 0.22062 (15) | 0.53367 (11) | 0.0511 (4) | |
Br22 | 0.3424 (2) | 0.22896 (17) | 0.07698 (11) | 0.0558 (4) | |
Sc1 | 0.1727 (3) | −0.2021 (3) | 0.1969 (2) | 0.0415 (5) | |
Sc2 | 0.3187 (3) | 0.2260 (3) | 0.3042 (2) | 0.0394 (5) | |
N13 | 0.1770 (14) | −0.1951 (11) | 0.3998 (8) | 0.052 (3) | |
H13A | 0.2940 | −0.1334 | 0.4400 | 0.117 (16)* | |
H13B | 0.1576 | −0.2840 | 0.4066 | 0.117 (16)* | |
H13C | 0.0812 | −0.1653 | 0.4317 | 0.117 (16)* | |
N11 | 0.1814 (14) | −0.1890 (11) | 0.0005 (8) | 0.051 (3) | |
H11A | 0.3022 | −0.1796 | −0.0215 | 0.117 (16)* | |
H11B | 0.1524 | −0.1121 | −0.0047 | 0.117 (16)* | |
H11C | 0.0930 | −0.2701 | −0.0494 | 0.117 (16)* | |
N21 | 0.6158 (15) | 0.3995 (11) | 0.3506 (9) | 0.052 (3) | |
H21A | 0.6266 | 0.4603 | 0.3051 | 0.117 (16)* | |
H21B | 0.7083 | 0.3593 | 0.3356 | 0.117 (16)* | |
H21C | 0.6320 | 0.4487 | 0.4299 | 0.117 (16)* | |
N12 | 0.3669 (15) | −0.3404 (11) | 0.1667 (8) | 0.053 (3) | |
H12A | 0.2912 | −0.4341 | 0.1522 | 0.117 (16)* | |
H12B | 0.4524 | −0.3132 | 0.2335 | 0.117 (16)* | |
H12C | 0.4334 | −0.3283 | 0.1025 | 0.117 (16)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Br21 | 0.0542 (9) | 0.0524 (9) | 0.0616 (8) | 0.0289 (7) | 0.0031 (6) | 0.0107 (7) |
Br11 | 0.0482 (8) | 0.0467 (8) | 0.0525 (7) | 0.0078 (7) | 0.0048 (6) | 0.0116 (6) |
Br1 | 0.0359 (6) | 0.0443 (8) | 0.0604 (8) | 0.0142 (6) | 0.0044 (5) | 0.0090 (6) |
Br2 | 0.0362 (6) | 0.0433 (8) | 0.0626 (8) | 0.0160 (6) | 0.0046 (5) | 0.0068 (6) |
Br23 | 0.0578 (8) | 0.0577 (9) | 0.0392 (6) | 0.0215 (7) | 0.0062 (6) | 0.0148 (6) |
Br22 | 0.0556 (8) | 0.0706 (10) | 0.0404 (7) | 0.0194 (7) | 0.0068 (6) | 0.0185 (6) |
Sc1 | 0.0406 (12) | 0.0385 (13) | 0.0446 (10) | 0.0144 (10) | 0.0057 (9) | 0.0101 (10) |
Sc2 | 0.0378 (11) | 0.0396 (13) | 0.0396 (10) | 0.0141 (10) | 0.0045 (8) | 0.0090 (9) |
N13 | 0.044 (6) | 0.059 (7) | 0.054 (6) | 0.017 (5) | 0.006 (5) | 0.019 (5) |
N11 | 0.050 (6) | 0.049 (7) | 0.047 (6) | 0.012 (5) | 0.004 (4) | 0.010 (5) |
N21 | 0.052 (7) | 0.047 (6) | 0.054 (6) | 0.014 (5) | 0.012 (5) | 0.011 (5) |
N12 | 0.067 (7) | 0.045 (6) | 0.058 (6) | 0.035 (5) | 0.013 (5) | 0.013 (5) |
Geometric parameters (Å, º) top
Br21—Sc2 | 2.575 (3) | N13—H13A | 0.8900 |
Br11—Sc1 | 2.538 (3) | N13—H13B | 0.8900 |
Br1—Sc1 | 2.654 (3) | N13—H13C | 0.8900 |
Br1—Sc2 | 2.679 (3) | N11—H11A | 0.8900 |
Br2—Sc1 | 2.679 (3) | N11—H11B | 0.8900 |
Br2—Sc2 | 2.745 (3) | N11—H11C | 0.8900 |
Br23—Sc2 | 2.622 (3) | N21—H21A | 0.8900 |
Br22—Sc2 | 2.594 (3) | N21—H21B | 0.8900 |
Sc1—N11 | 2.269 (9) | N21—H21C | 0.8900 |
Sc1—N12 | 2.269 (9) | N12—H12A | 0.8900 |
Sc1—N13 | 2.284 (10) | N12—H12B | 0.8900 |
Sc2—N21 | 2.211 (10) | N12—H12C | 0.8900 |
| | | |
Sc1—Br1—Sc2 | 95.35 (9) | Br21—Sc2—Br2 | 177.95 (11) |
Sc1—Br2—Sc2 | 93.25 (8) | Br22—Sc2—Br2 | 87.55 (8) |
N11—Sc1—N12 | 91.6 (4) | Br23—Sc2—Br2 | 87.06 (8) |
N11—Sc1—N13 | 175.3 (4) | Br1—Sc2—Br2 | 84.79 (9) |
N12—Sc1—N13 | 90.5 (3) | Sc1—N13—H13A | 109.5 |
N11—Sc1—Br11 | 91.6 (3) | Sc1—N13—H13B | 109.5 |
N12—Sc1—Br11 | 93.2 (3) | H13A—N13—H13B | 109.5 |
N13—Sc1—Br11 | 92.4 (3) | Sc1—N13—H13C | 109.5 |
N11—Sc1—Br1 | 89.0 (3) | H13A—N13—H13C | 109.5 |
N12—Sc1—Br1 | 172.8 (3) | H13B—N13—H13C | 109.5 |
N13—Sc1—Br1 | 88.4 (3) | Sc1—N11—H11A | 109.5 |
Br11—Sc1—Br1 | 93.95 (9) | Sc1—N11—H11B | 109.5 |
N11—Sc1—Br2 | 88.2 (3) | H11A—N11—H11B | 109.5 |
N12—Sc1—Br2 | 86.3 (3) | Sc1—N11—H11C | 109.5 |
N13—Sc1—Br2 | 87.7 (3) | H11A—N11—H11C | 109.5 |
Br11—Sc1—Br2 | 179.43 (12) | H11B—N11—H11C | 109.5 |
Br1—Sc1—Br2 | 86.61 (9) | Sc2—N21—H21A | 109.5 |
N21—Sc2—Br21 | 95.2 (3) | Sc2—N21—H21B | 109.5 |
N21—Sc2—Br22 | 87.9 (3) | H21A—N21—H21B | 109.5 |
Br21—Sc2—Br22 | 92.64 (9) | Sc2—N21—H21C | 109.5 |
N21—Sc2—Br23 | 87.8 (3) | H21A—N21—H21C | 109.5 |
Br21—Sc2—Br23 | 92.89 (8) | H21B—N21—H21C | 109.5 |
Br22—Sc2—Br23 | 173.27 (10) | Sc1—N12—H12A | 109.5 |
N21—Sc2—Br1 | 171.6 (3) | Sc1—N12—H12B | 109.5 |
Br21—Sc2—Br1 | 93.17 (9) | H12A—N12—H12B | 109.5 |
Br22—Sc2—Br1 | 92.17 (9) | Sc1—N12—H12C | 109.5 |
Br23—Sc2—Br1 | 91.35 (9) | H12A—N12—H12C | 109.5 |
N21—Sc2—Br2 | 86.8 (3) | H12B—N12—H12C | 109.5 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N13—H13A···Br23i | 0.89 | 3.12 | 3.690 (10) | 124 |
N13—H13B···Br21ii | 0.89 | 3.00 | 3.854 (11) | 161 |
N13—H13C···Br23iii | 0.89 | 2.92 | 3.722 (9) | 151 |
N11—H11A···Br22iv | 0.89 | 2.82 | 3.684 (9) | 163 |
N11—H11B···Br22 | 0.89 | 3.13 | 3.846 (11) | 139 |
N21—H21A···Br11v | 0.89 | 2.77 | 3.514 (10) | 143 |
N21—H21B···Br21vi | 0.89 | 2.89 | 3.669 (10) | 148 |
N21—H21C···Br21vii | 0.89 | 2.81 | 3.609 (10) | 151 |
N12—H12A···Br21ii | 0.89 | 3.11 | 3.712 (10) | 127 |
N12—H12B···Br23i | 0.89 | 2.79 | 3.671 (10) | 170 |
N12—H12C···Br22iv | 0.89 | 2.80 | 3.678 (9) | 168 |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x, y−1, z; (iii) −x, −y, −z+1; (iv) −x+1, −y, −z; (v) x+1, y+1, z; (vi) x+1, y, z; (vii) −x+1, −y+1, −z+1. |