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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803021524/bt6359sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803021524/bt6359Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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

Computing details top

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 = 637.52F(000) = 584
Triclinic, P1Dx = 2.827 Mg m3
Hall symbol: -P 1Melting point: unknown K
a = 7.211 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.157 (3) ÅCell parameters from 2678 reflections
c = 11.350 (3) Åθ = 1.9–29.7°
α = 105.39 (2)°µ = 16.88 mm1
β = 90.76 (2)°T = 293 K
γ = 109.85 (2)°Column, colourless
V = 749.0 (4) Å30.2 × 0.1 × 0.1 mm
Data collection top
Stoe IPDS II
diffractometer
2938 independent reflections
Radiation source: fine-focus sealed tube1237 reflections with I > 2s(I)
Graphite monochromatorRint = 0.077
Detector resolution: not measured pixels mm-1θmax = 26.0°, θmin = 1.9°
ω and φ scansh = 88
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 = 1212
Tmin = 0.100, Tmax = 0.148l = 1313
6953 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.039H-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 reflectionsΔρmax = 0.66 e Å3
111 parametersΔρmin = 0.70 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction 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
xyzUiso*/Ueq
Br210.1258 (2)0.40251 (16)0.34540 (12)0.0546 (4)
Br110.14637 (19)0.42322 (15)0.13769 (11)0.0521 (4)
Br10.0130 (2)0.01176 (15)0.24330 (12)0.0481 (3)
Br20.5115 (2)0.02968 (14)0.25850 (12)0.0486 (4)
Br230.33607 (19)0.22062 (15)0.53367 (11)0.0511 (4)
Br220.3424 (2)0.22896 (17)0.07698 (11)0.0558 (4)
Sc10.1727 (3)0.2021 (3)0.1969 (2)0.0415 (5)
Sc20.3187 (3)0.2260 (3)0.3042 (2)0.0394 (5)
N130.1770 (14)0.1951 (11)0.3998 (8)0.052 (3)
H13A0.29400.13340.44000.117 (16)*
H13B0.15760.28400.40660.117 (16)*
H13C0.08120.16530.43170.117 (16)*
N110.1814 (14)0.1890 (11)0.0005 (8)0.051 (3)
H11A0.30220.17960.02150.117 (16)*
H11B0.15240.11210.00470.117 (16)*
H11C0.09300.27010.04940.117 (16)*
N210.6158 (15)0.3995 (11)0.3506 (9)0.052 (3)
H21A0.62660.46030.30510.117 (16)*
H21B0.70830.35930.33560.117 (16)*
H21C0.63200.44870.42990.117 (16)*
N120.3669 (15)0.3404 (11)0.1667 (8)0.053 (3)
H12A0.29120.43410.15220.117 (16)*
H12B0.45240.31320.23350.117 (16)*
H12C0.43340.32830.10250.117 (16)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br210.0542 (9)0.0524 (9)0.0616 (8)0.0289 (7)0.0031 (6)0.0107 (7)
Br110.0482 (8)0.0467 (8)0.0525 (7)0.0078 (7)0.0048 (6)0.0116 (6)
Br10.0359 (6)0.0443 (8)0.0604 (8)0.0142 (6)0.0044 (5)0.0090 (6)
Br20.0362 (6)0.0433 (8)0.0626 (8)0.0160 (6)0.0046 (5)0.0068 (6)
Br230.0578 (8)0.0577 (9)0.0392 (6)0.0215 (7)0.0062 (6)0.0148 (6)
Br220.0556 (8)0.0706 (10)0.0404 (7)0.0194 (7)0.0068 (6)0.0185 (6)
Sc10.0406 (12)0.0385 (13)0.0446 (10)0.0144 (10)0.0057 (9)0.0101 (10)
Sc20.0378 (11)0.0396 (13)0.0396 (10)0.0141 (10)0.0045 (8)0.0090 (9)
N130.044 (6)0.059 (7)0.054 (6)0.017 (5)0.006 (5)0.019 (5)
N110.050 (6)0.049 (7)0.047 (6)0.012 (5)0.004 (4)0.010 (5)
N210.052 (7)0.047 (6)0.054 (6)0.014 (5)0.012 (5)0.011 (5)
N120.067 (7)0.045 (6)0.058 (6)0.035 (5)0.013 (5)0.013 (5)
Geometric parameters (Å, º) top
Br21—Sc22.575 (3)N13—H13A0.8900
Br11—Sc12.538 (3)N13—H13B0.8900
Br1—Sc12.654 (3)N13—H13C0.8900
Br1—Sc22.679 (3)N11—H11A0.8900
Br2—Sc12.679 (3)N11—H11B0.8900
Br2—Sc22.745 (3)N11—H11C0.8900
Br23—Sc22.622 (3)N21—H21A0.8900
Br22—Sc22.594 (3)N21—H21B0.8900
Sc1—N112.269 (9)N21—H21C0.8900
Sc1—N122.269 (9)N12—H12A0.8900
Sc1—N132.284 (10)N12—H12B0.8900
Sc2—N212.211 (10)N12—H12C0.8900
Sc1—Br1—Sc295.35 (9)Br21—Sc2—Br2177.95 (11)
Sc1—Br2—Sc293.25 (8)Br22—Sc2—Br287.55 (8)
N11—Sc1—N1291.6 (4)Br23—Sc2—Br287.06 (8)
N11—Sc1—N13175.3 (4)Br1—Sc2—Br284.79 (9)
N12—Sc1—N1390.5 (3)Sc1—N13—H13A109.5
N11—Sc1—Br1191.6 (3)Sc1—N13—H13B109.5
N12—Sc1—Br1193.2 (3)H13A—N13—H13B109.5
N13—Sc1—Br1192.4 (3)Sc1—N13—H13C109.5
N11—Sc1—Br189.0 (3)H13A—N13—H13C109.5
N12—Sc1—Br1172.8 (3)H13B—N13—H13C109.5
N13—Sc1—Br188.4 (3)Sc1—N11—H11A109.5
Br11—Sc1—Br193.95 (9)Sc1—N11—H11B109.5
N11—Sc1—Br288.2 (3)H11A—N11—H11B109.5
N12—Sc1—Br286.3 (3)Sc1—N11—H11C109.5
N13—Sc1—Br287.7 (3)H11A—N11—H11C109.5
Br11—Sc1—Br2179.43 (12)H11B—N11—H11C109.5
Br1—Sc1—Br286.61 (9)Sc2—N21—H21A109.5
N21—Sc2—Br2195.2 (3)Sc2—N21—H21B109.5
N21—Sc2—Br2287.9 (3)H21A—N21—H21B109.5
Br21—Sc2—Br2292.64 (9)Sc2—N21—H21C109.5
N21—Sc2—Br2387.8 (3)H21A—N21—H21C109.5
Br21—Sc2—Br2392.89 (8)H21B—N21—H21C109.5
Br22—Sc2—Br23173.27 (10)Sc1—N12—H12A109.5
N21—Sc2—Br1171.6 (3)Sc1—N12—H12B109.5
Br21—Sc2—Br193.17 (9)H12A—N12—H12B109.5
Br22—Sc2—Br192.17 (9)Sc1—N12—H12C109.5
Br23—Sc2—Br191.35 (9)H12A—N12—H12C109.5
N21—Sc2—Br286.8 (3)H12B—N12—H12C109.5
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N13—H13A···Br23i0.893.123.690 (10)124
N13—H13B···Br21ii0.893.003.854 (11)161
N13—H13C···Br23iii0.892.923.722 (9)151
N11—H11A···Br22iv0.892.823.684 (9)163
N11—H11B···Br220.893.133.846 (11)139
N21—H21A···Br11v0.892.773.514 (10)143
N21—H21B···Br21vi0.892.893.669 (10)148
N21—H21C···Br21vii0.892.813.609 (10)151
N12—H12A···Br21ii0.893.113.712 (10)127
N12—H12B···Br23i0.892.793.671 (10)170
N12—H12C···Br22iv0.892.803.678 (9)168
Symmetry codes: (i) x+1, y, z+1; (ii) x, y1, 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.
 

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