Download citation
Download citation
link to html
The triammoniate of indium(III) chloride has been obtained as single crystals from the reaction of indium metal and ammonium chloride in a sealed Monel metal container. It crystallizes as a salt with [In(NH3)4Cl2]+ and [In(NH3)2Cl4]- ions, both of which lie on inversion centers.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803013539/bt6243sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803013539/bt6243Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](In-N) = 0.004 Å
  • R factor = 0.028
  • wR factor = 0.073
  • Data-to-parameter ratio = 18.1

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
ABSTM_02 Alert A The ratio of Tmax/Tmin expected RT(exp) is > 1.30 An absorption correction should be applied. Tmin and Tmax expected: 0.498 0.672 RT(exp) = 1.349 REFLT_03 From the CIF: _diffrn_reflns_theta_max 25.99 From the CIF: _reflns_number_total 1234 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 1530 Completeness (_total/calc) 80.65% Alert A: < 85% complete (theta max?)
Amber Alert Alert Level B:
CHEMS_01 Alert B The sum formula contains elements in the wrong order. H precedes Cl Sequence must be C, H, then alphabetical.
Yellow Alert Alert Level C:
PLAT_420 Alert C D-H Without Acceptor N2 - H2B ... ? General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: H18 Cl6 In2 N6 Atom count from _chemical_formula_moiety:
2 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Data collection: IPDS (Stoe & Cie, 1996-1997); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
2[InCl3(NH3)3]Z = 1
Mr = 544.54F(000) = 260
Triclinic, P1Dx = 2.327 Mg m3
a = 5.8652 (15) ÅMo Kα radiation, λ = 0.71073 Å
b = 6.8130 (18) ÅCell parameters from 1719 reflections
c = 9.794 (2) Åθ = 1.9–26°
α = 86.14 (3)°µ = 3.98 mm1
β = 86.68 (3)°T = 293 K
γ = 85.26 (3)°Irregular, colourless
V = 388.59 (17) Å30.25 × 0.15 × 0.1 mm
Data collection top
Stoe Imaging Plate Diffraction System
diffractometer
1049 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.023
Graphite monochromatorθmax = 26.0°, θmin = 3.5°
φ scansh = 67
1719 measured reflectionsk = 87
1234 independent reflectionsl = 1212
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)] = 0.028H-atom parameters constrained
wR(F2) = 0.073 w = 1/[σ2(Fo2) + (0.0559P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.96(Δ/σ)max < 0.001
1234 reflectionsΔρmax = 0.81 e Å3
68 parametersΔρmin = 0.75 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.023 (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
In10.00000.50000.00000.02408 (19)
In20.50000.00000.50000.02292 (18)
Cl10.2706 (2)0.00305 (19)0.27341 (11)0.0342 (3)
Cl20.2624 (2)0.69134 (17)0.58217 (13)0.0361 (3)
Cl30.28373 (19)0.70997 (17)0.08736 (12)0.0326 (3)
N10.7470 (7)0.1896 (6)0.5817 (4)0.0301 (8)
H1A0.71160.31520.55450.045*
H1B0.88840.15280.55020.045*
H1C0.73950.17630.67280.045*
N20.7969 (7)0.7762 (6)0.9238 (5)0.0342 (8)
H2A0.71550.74950.85440.051*
H2B0.89200.86760.89560.051*
H2C0.70270.82090.99140.051*
N30.1954 (7)0.4972 (6)0.7946 (4)0.0333 (8)
H3A0.29940.58570.79050.050*
H3B0.09860.52710.72820.050*
H3C0.26520.37770.78410.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
In10.0245 (2)0.0224 (3)0.0253 (3)0.00095 (17)0.00252 (15)0.00183 (16)
In20.0231 (2)0.0210 (2)0.0250 (3)0.00240 (16)0.00260 (15)0.00150 (16)
Cl10.0376 (6)0.0348 (6)0.0299 (5)0.0048 (5)0.0052 (4)0.0026 (5)
Cl20.0360 (6)0.0267 (5)0.0448 (6)0.0026 (5)0.0098 (5)0.0024 (5)
Cl30.0313 (5)0.0334 (6)0.0351 (5)0.0077 (5)0.0045 (4)0.0071 (4)
N10.0292 (18)0.0283 (19)0.0341 (18)0.0049 (16)0.0037 (15)0.0067 (16)
N20.0328 (19)0.0251 (18)0.043 (2)0.0031 (17)0.0014 (17)0.0001 (17)
N30.0342 (19)0.032 (2)0.0326 (19)0.0001 (17)0.0031 (16)0.0048 (17)
Geometric parameters (Å, º) top
In1—N2i2.250 (4)Cl2—In2xi2.5355 (15)
In1—N2ii2.250 (4)N1—H1A0.8900
In1—N3iii2.258 (4)N1—H1B0.8900
In1—N3iv2.258 (4)N1—H1C0.8900
In1—Cl3v2.5043 (12)N2—In1xii2.250 (4)
In1—Cl32.5043 (12)N2—H2A0.8900
In2—N1vi2.234 (3)N2—H2B0.8900
In2—N12.234 (3)N2—H2C0.8900
In2—Cl1vii2.5276 (14)N3—In1xiii2.258 (4)
In2—Cl1viii2.5276 (14)N3—H3A0.8900
In2—Cl2ix2.5355 (15)N3—H3B0.8900
In2—Cl2iv2.5355 (15)N3—H3C0.8900
Cl1—In2x2.5276 (14)
N2i—In1—N2ii180.0Cl1viii—In2—Cl2ix90.12 (5)
N2i—In1—N3iii88.70 (17)N1vi—In2—Cl2iv90.69 (12)
N2ii—In1—N3iii91.30 (17)N1—In2—Cl2iv89.31 (12)
N2i—In1—N3iv91.30 (17)Cl1vii—In2—Cl2iv90.12 (5)
N2ii—In1—N3iv88.70 (17)Cl1viii—In2—Cl2iv89.88 (5)
N3iii—In1—N3iv180.0 (2)Cl2ix—In2—Cl2iv180.00 (6)
N2i—In1—Cl3v90.97 (11)In2—N1—H1A109.5
N2ii—In1—Cl3v89.03 (11)In2—N1—H1B109.5
N3iii—In1—Cl3v89.59 (11)H1A—N1—H1B109.5
N3iv—In1—Cl3v90.41 (11)In2—N1—H1C109.5
N2i—In1—Cl389.03 (11)H1A—N1—H1C109.5
N2ii—In1—Cl390.97 (11)H1B—N1—H1C109.5
N3iii—In1—Cl390.41 (11)In1xii—N2—H2A109.5
N3iv—In1—Cl389.59 (11)In1xii—N2—H2B109.5
Cl3v—In1—Cl3180.00 (5)H2A—N2—H2B109.5
N1vi—In2—N1180.000 (1)In1xii—N2—H2C109.5
N1vi—In2—Cl1vii90.33 (11)H2A—N2—H2C109.5
N1—In2—Cl1vii89.67 (11)H2B—N2—H2C109.5
N1vi—In2—Cl1viii89.67 (11)In1xiii—N3—H3A109.5
N1—In2—Cl1viii90.33 (11)In1xiii—N3—H3B109.5
Cl1vii—In2—Cl1viii180.0H3A—N3—H3B109.5
N1vi—In2—Cl2ix89.31 (12)In1xiii—N3—H3C109.5
N1—In2—Cl2ix90.69 (12)H3A—N3—H3C109.5
Cl1vii—In2—Cl2ix89.88 (5)H3B—N3—H3C109.5
Symmetry codes: (i) x1, y, z1; (ii) x+1, y+1, z+1; (iii) x, y, z1; (iv) x, y+1, z+1; (v) x, y+1, z; (vi) x+1, y, z+1; (vii) x+1, y, z; (viii) x, y, z+1; (ix) x+1, y1, z; (x) x1, y, z; (xi) x1, y+1, z; (xii) x+1, y, z+1; (xiii) x, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···Cl2vii0.892.613.415 (4)150
N1—H1B···Cl2ii0.892.743.470 (4)141
N1—H1C···Cl3ii0.892.523.349 (4)156
N2—H2A···Cl2vii0.892.723.476 (5)144
N2—H2B···Cl1ii0.892.853.659 (5)151
N2—H2C···Cl3xiii0.892.733.376 (5)131
N3—H3A···Cl1iv0.892.823.484 (5)132
N3—H3B···Cl20.892.743.602 (4)163
N3—H3C···Cl1viii0.892.693.504 (5)153
Symmetry codes: (ii) x+1, y+1, z+1; (iv) x, y+1, z+1; (vii) x+1, y, z; (viii) x, y, z+1; (xiii) x, y, z+1.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds