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
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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?)
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.
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
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.
Crystal data top
2[InCl3(NH3)3] | Z = 1 |
Mr = 544.54 | F(000) = 260 |
Triclinic, P1 | Dx = 2.327 Mg m−3 |
a = 5.8652 (15) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 6.8130 (18) Å | Cell parameters from 1719 reflections |
c = 9.794 (2) Å | θ = 1.9–26° |
α = 86.14 (3)° | µ = 3.98 mm−1 |
β = 86.68 (3)° | T = 293 K |
γ = 85.26 (3)° | Irregular, colourless |
V = 388.59 (17) Å3 | 0.25 × 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 tube | Rint = 0.023 |
Graphite monochromator | θmax = 26.0°, θmin = 3.5° |
φ scans | h = −6→7 |
1719 measured reflections | k = −8→7 |
1234 independent reflections | l = −12→12 |
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)] = 0.028 | H-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 reflections | Δρmax = 0.81 e Å−3 |
68 parameters | Δρmin = −0.75 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction 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 | x | y | z | Uiso*/Ueq | |
In1 | 0.0000 | 0.5000 | 0.0000 | 0.02408 (19) | |
In2 | 0.5000 | 0.0000 | 0.5000 | 0.02292 (18) | |
Cl1 | −0.2706 (2) | 0.00305 (19) | 0.27341 (11) | 0.0342 (3) | |
Cl2 | −0.2624 (2) | 0.69134 (17) | 0.58217 (13) | 0.0361 (3) | |
Cl3 | 0.28373 (19) | 0.70997 (17) | 0.08736 (12) | 0.0326 (3) | |
N1 | 0.7470 (7) | 0.1896 (6) | 0.5817 (4) | 0.0301 (8) | |
H1A | 0.7116 | 0.3152 | 0.5545 | 0.045* | |
H1B | 0.8884 | 0.1528 | 0.5502 | 0.045* | |
H1C | 0.7395 | 0.1763 | 0.6728 | 0.045* | |
N2 | 0.7969 (7) | 0.7762 (6) | 0.9238 (5) | 0.0342 (8) | |
H2A | 0.7155 | 0.7495 | 0.8544 | 0.051* | |
H2B | 0.8920 | 0.8676 | 0.8956 | 0.051* | |
H2C | 0.7027 | 0.8209 | 0.9914 | 0.051* | |
N3 | 0.1954 (7) | 0.4972 (6) | 0.7946 (4) | 0.0333 (8) | |
H3A | 0.2994 | 0.5857 | 0.7905 | 0.050* | |
H3B | 0.0986 | 0.5271 | 0.7282 | 0.050* | |
H3C | 0.2652 | 0.3777 | 0.7841 | 0.050* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
In1 | 0.0245 (2) | 0.0224 (3) | 0.0253 (3) | −0.00095 (17) | −0.00252 (15) | −0.00183 (16) |
In2 | 0.0231 (2) | 0.0210 (2) | 0.0250 (3) | −0.00240 (16) | −0.00260 (15) | −0.00150 (16) |
Cl1 | 0.0376 (6) | 0.0348 (6) | 0.0299 (5) | −0.0048 (5) | 0.0052 (4) | −0.0026 (5) |
Cl2 | 0.0360 (6) | 0.0267 (5) | 0.0448 (6) | 0.0026 (5) | −0.0098 (5) | 0.0024 (5) |
Cl3 | 0.0313 (5) | 0.0334 (6) | 0.0351 (5) | −0.0077 (5) | −0.0045 (4) | −0.0071 (4) |
N1 | 0.0292 (18) | 0.0283 (19) | 0.0341 (18) | −0.0049 (16) | −0.0037 (15) | −0.0067 (16) |
N2 | 0.0328 (19) | 0.0251 (18) | 0.043 (2) | 0.0031 (17) | −0.0014 (17) | −0.0001 (17) |
N3 | 0.0342 (19) | 0.032 (2) | 0.0326 (19) | 0.0001 (17) | 0.0031 (16) | −0.0048 (17) |
Geometric parameters (Å, º) top
In1—N2i | 2.250 (4) | Cl2—In2xi | 2.5355 (15) |
In1—N2ii | 2.250 (4) | N1—H1A | 0.8900 |
In1—N3iii | 2.258 (4) | N1—H1B | 0.8900 |
In1—N3iv | 2.258 (4) | N1—H1C | 0.8900 |
In1—Cl3v | 2.5043 (12) | N2—In1xii | 2.250 (4) |
In1—Cl3 | 2.5043 (12) | N2—H2A | 0.8900 |
In2—N1vi | 2.234 (3) | N2—H2B | 0.8900 |
In2—N1 | 2.234 (3) | N2—H2C | 0.8900 |
In2—Cl1vii | 2.5276 (14) | N3—In1xiii | 2.258 (4) |
In2—Cl1viii | 2.5276 (14) | N3—H3A | 0.8900 |
In2—Cl2ix | 2.5355 (15) | N3—H3B | 0.8900 |
In2—Cl2iv | 2.5355 (15) | N3—H3C | 0.8900 |
Cl1—In2x | 2.5276 (14) | | |
| | | |
N2i—In1—N2ii | 180.0 | Cl1viii—In2—Cl2ix | 90.12 (5) |
N2i—In1—N3iii | 88.70 (17) | N1vi—In2—Cl2iv | 90.69 (12) |
N2ii—In1—N3iii | 91.30 (17) | N1—In2—Cl2iv | 89.31 (12) |
N2i—In1—N3iv | 91.30 (17) | Cl1vii—In2—Cl2iv | 90.12 (5) |
N2ii—In1—N3iv | 88.70 (17) | Cl1viii—In2—Cl2iv | 89.88 (5) |
N3iii—In1—N3iv | 180.0 (2) | Cl2ix—In2—Cl2iv | 180.00 (6) |
N2i—In1—Cl3v | 90.97 (11) | In2—N1—H1A | 109.5 |
N2ii—In1—Cl3v | 89.03 (11) | In2—N1—H1B | 109.5 |
N3iii—In1—Cl3v | 89.59 (11) | H1A—N1—H1B | 109.5 |
N3iv—In1—Cl3v | 90.41 (11) | In2—N1—H1C | 109.5 |
N2i—In1—Cl3 | 89.03 (11) | H1A—N1—H1C | 109.5 |
N2ii—In1—Cl3 | 90.97 (11) | H1B—N1—H1C | 109.5 |
N3iii—In1—Cl3 | 90.41 (11) | In1xii—N2—H2A | 109.5 |
N3iv—In1—Cl3 | 89.59 (11) | In1xii—N2—H2B | 109.5 |
Cl3v—In1—Cl3 | 180.00 (5) | H2A—N2—H2B | 109.5 |
N1vi—In2—N1 | 180.000 (1) | In1xii—N2—H2C | 109.5 |
N1vi—In2—Cl1vii | 90.33 (11) | H2A—N2—H2C | 109.5 |
N1—In2—Cl1vii | 89.67 (11) | H2B—N2—H2C | 109.5 |
N1vi—In2—Cl1viii | 89.67 (11) | In1xiii—N3—H3A | 109.5 |
N1—In2—Cl1viii | 90.33 (11) | In1xiii—N3—H3B | 109.5 |
Cl1vii—In2—Cl1viii | 180.0 | H3A—N3—H3B | 109.5 |
N1vi—In2—Cl2ix | 89.31 (12) | In1xiii—N3—H3C | 109.5 |
N1—In2—Cl2ix | 90.69 (12) | H3A—N3—H3C | 109.5 |
Cl1vii—In2—Cl2ix | 89.88 (5) | H3B—N3—H3C | 109.5 |
Symmetry codes: (i) x−1, y, z−1; (ii) −x+1, −y+1, −z+1; (iii) x, y, z−1; (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, y−1, z; (x) x−1, y, z; (xi) x−1, y+1, z; (xii) x+1, y, z+1; (xiii) x, y, z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···Cl2vii | 0.89 | 2.61 | 3.415 (4) | 150 |
N1—H1B···Cl2ii | 0.89 | 2.74 | 3.470 (4) | 141 |
N1—H1C···Cl3ii | 0.89 | 2.52 | 3.349 (4) | 156 |
N2—H2A···Cl2vii | 0.89 | 2.72 | 3.476 (5) | 144 |
N2—H2B···Cl1ii | 0.89 | 2.85 | 3.659 (5) | 151 |
N2—H2C···Cl3xiii | 0.89 | 2.73 | 3.376 (5) | 131 |
N3—H3A···Cl1iv | 0.89 | 2.82 | 3.484 (5) | 132 |
N3—H3B···Cl2 | 0.89 | 2.74 | 3.602 (4) | 163 |
N3—H3C···Cl1viii | 0.89 | 2.69 | 3.504 (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. |