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The title compound, [Sc2Br6(NH3)2], was obtained by the reaction of ammonium bromide, (NH4)Br, with scandium metal in a sealed tantalum metal container. The crystal structure contains zigzag chains of edge-connected [Sc(NH3)Br5] octahedra according to the formulation [Sc(NH3)1/1Br1/1Br4/2]. Sc(NH3)Br3 is isotypic with Sc(NH3)Cl3.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803021536/bt6360sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803021536/bt6360Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](Sc-N) = 0.008 Å
  • R factor = 0.040
  • wR factor = 0.096
  • Data-to-parameter ratio = 37.3

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.99
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 = 0.789 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT155_ALERT_4_C The Triclinic Unitcell is NOT Reduced .......... ? PLAT156_ALERT_4_C Axial System Input Cell not Standard ........... ? PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1A ... ? PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2A ... ?
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 7 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 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 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: Details?.

Diamminehexabromodiscandium(III) top
Crystal data top
[Sc2Br6(NH3)2]Z = 2
Mr = 603.45F(000) = 544
Triclinic, P1Dx = 3.192 Mg m3
Hall symbol: -P 1Melting point: unknown K
a = 7.392 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.578 (2) ÅCell parameters from 3629 reflections
c = 9.551 (2) Åθ = 1.3–29.8°
α = 73.07 (2)°µ = 20.12 mm1
β = 80.04 (2)°T = 293 K
γ = 77.82 (2)°Column, colourless
V = 627.8 (3) Å30.25 × 0.1 × 0.1 mm
Data collection top
Stoe IPDS II
diffractometer
3470 independent reflections
Radiation source: fine-focus sealed tube1750 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.072
Detector resolution: not measured pixels mm-1θmax = 29.6°, θmin = 2.3°
ω and φ scansh = 1010
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 = 1313
Tmin = 0.052, Tmax = 0.155l = 1313
9270 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)] = 0.040H-atom parameters constrained
wR(F2) = 0.096 w = 1/[σ2(Fo2) + (0.043P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.79(Δ/σ)max = 0.001
3470 reflectionsΔρmax = 1.06 e Å3
93 parametersΔρmin = 1.19 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: 0.0021 (3)
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
Sc10.0800 (2)0.94111 (15)0.69559 (16)0.0309 (3)
Br110.21509 (14)1.06539 (10)0.81959 (11)0.0490 (2)
Br120.09954 (11)1.16842 (9)0.45800 (9)0.0363 (2)
Br10.08889 (10)0.69948 (9)0.91996 (9)0.0350 (2)
Br20.40163 (10)0.79309 (8)0.58317 (9)0.0370 (2)
Sc20.4011 (2)0.55114 (15)0.80663 (16)0.0315 (3)
Br210.41246 (11)0.32866 (9)1.04857 (10)0.0366 (2)
Br220.23220 (14)0.42413 (10)0.68373 (11)0.0479 (2)
N10.2690 (11)1.0360 (8)0.7911 (9)0.0495 (19)
H1A0.38721.00480.76010.115 (19)*
H1B0.25041.00630.88900.115 (19)*
H1C0.24421.13450.76180.115 (19)*
N20.6822 (10)0.4583 (8)0.7072 (9)0.0471 (18)
H2A0.77030.48990.73670.115 (19)*
H2B0.68860.48830.60940.115 (19)*
H2C0.69900.35980.73620.115 (19)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sc10.0288 (6)0.0323 (7)0.0310 (7)0.0000 (5)0.0082 (5)0.0085 (6)
Br110.0474 (5)0.0466 (5)0.0440 (5)0.0099 (4)0.0007 (4)0.0140 (4)
Br120.0387 (4)0.0343 (4)0.0369 (5)0.0102 (3)0.0139 (3)0.0027 (3)
Br10.0280 (4)0.0367 (4)0.0328 (4)0.0000 (3)0.0024 (3)0.0022 (3)
Br20.0287 (4)0.0386 (5)0.0337 (5)0.0007 (3)0.0019 (3)0.0001 (4)
Sc20.0300 (6)0.0308 (7)0.0313 (7)0.0003 (5)0.0078 (5)0.0055 (6)
Br210.0360 (4)0.0341 (4)0.0383 (5)0.0083 (3)0.0144 (3)0.0003 (3)
Br220.0609 (6)0.0459 (5)0.0434 (5)0.0131 (4)0.0148 (4)0.0141 (4)
N10.060 (5)0.044 (4)0.050 (5)0.012 (3)0.021 (4)0.011 (3)
N20.043 (4)0.045 (4)0.044 (4)0.009 (3)0.004 (3)0.010 (3)
Geometric parameters (Å, º) top
Sc1—N12.252 (7)Sc2—Br222.5293 (18)
Sc1—Br112.5316 (18)Sc2—Br212.6477 (18)
Sc1—Br12.6548 (18)Sc2—Br21ii2.7190 (18)
Sc1—Br122.6555 (19)Br21—Sc2ii2.7190 (18)
Sc1—Br12i2.6779 (17)N1—H1A0.8900
Sc1—Br22.7197 (17)N1—H1B0.8900
Br12—Sc1i2.6779 (17)N1—H1C0.8900
Br1—Sc22.6769 (18)N2—H2A0.8900
Br2—Sc22.6542 (18)N2—H2B0.8900
Sc2—N22.244 (7)N2—H2C0.8900
N1—Sc1—Br1193.8 (2)Br21—Sc2—Br2172.99 (6)
N1—Sc1—Br192.4 (2)N2—Sc2—Br1171.1 (2)
Br11—Sc1—Br191.10 (6)Br22—Sc2—Br194.51 (6)
N1—Sc1—Br1287.8 (2)Br21—Sc2—Br192.25 (6)
Br11—Sc1—Br1294.50 (6)Br2—Sc2—Br185.59 (5)
Br1—Sc1—Br12174.38 (6)N2—Sc2—Br21ii86.6 (2)
N1—Sc1—Br12i170.1 (2)Br22—Sc2—Br21ii176.44 (7)
Br11—Sc1—Br12i94.49 (6)Br21—Sc2—Br21ii84.05 (5)
Br1—Sc1—Br12i92.78 (6)Br2—Sc2—Br21ii89.16 (6)
Br12—Sc1—Br12i86.30 (5)Br1—Sc2—Br21ii86.49 (5)
N1—Sc1—Br284.9 (2)Sc2—Br21—Sc2ii95.95 (5)
Br11—Sc1—Br2175.57 (7)Sc1—N1—H1A109.5
Br1—Sc1—Br284.73 (5)Sc1—N1—H1B109.5
Br12—Sc1—Br289.69 (6)H1A—N1—H1B109.5
Br12i—Sc1—Br287.21 (5)Sc1—N1—H1C109.5
Sc1—Br12—Sc1i93.70 (5)H1A—N1—H1C109.5
Sc1—Br1—Sc295.32 (6)H1B—N1—H1C109.5
Sc2—Br2—Sc194.33 (6)Sc2—N2—H2A109.5
N2—Sc2—Br2292.8 (2)Sc2—N2—H2B109.5
N2—Sc2—Br2192.6 (2)H2A—N2—H2B109.5
Br22—Sc2—Br2192.49 (6)Sc2—N2—H2C109.5
N2—Sc2—Br288.7 (2)H2A—N2—H2C109.5
Br22—Sc2—Br294.32 (6)H2B—N2—H2C109.5
Symmetry codes: (i) x, y+2, z+1; (ii) x+1, y+1, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1B···Br11iii0.892.643.532 (8)175
N1—H1C···Br22iv0.892.643.520 (8)170
N2—H2B···Br22v0.892.683.556 (8)171
N2—H2C···Br11vi0.892.663.551 (7)174
Symmetry codes: (iii) x, y+2, z+2; (iv) x, y+1, z; (v) x+1, y+1, z+1; (vi) x+1, y1, z.
 

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