Tri­ammonium nona­iodo­diantimonate(III), (NH4)3[Sb2I9]

Zhang, H.; Fang, L.; Yuan, R.-Z.

doi:10.1107/S1600536805011098

Triammonium nonaiododiantimonate(III), (NH₄)₃[Sb₂I₉]

The crystal structure of the title compound, (NH₄)₃[Sb₂I₉], which crystallizes in the monoclinic space group P2₁/n, resembles that of hexagonal Cs₃[Sb₂I₉], which crystallizes in space group P $\overline 3$ m1. The title compound consists of double layers parallel to (001). Each layer is made up of distorted corner-sharing SbI₆ octahedra. One-third of the ammonium cations reside within six-membered rings formed by corner-sharing SbI₆ octahedra within the layers. The other ammonium cations are situated within three-membered rings built from corner-sharing SbI₆ octahedra near the edges of the layers.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805011098/wm6059sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536805011098/wm6059Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 223 K
Mean (I-Sb) = 0.001 Å
H-atom completeness 1%
R factor = 0.041
wR factor = 0.089
Data-to-parameter ratio = 46.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         I5

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:H12 I9 N3 Sb2
            Atom count from the _atom_site data:  I9 N3 Sb2
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    4
           From the CIF: _chemical_formula_sum  H12 I9 N3 Sb2
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           H         48.00      0.00   48.00
           I         36.00     36.00    0.00
           N         12.00     12.00    0.00
           Sb         8.00      8.00    0.00

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   3 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 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: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 2002) and DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97).

Triammonium nonaiododiantimonate(III) top

Crystal data top

(NH₄)₃[Sb₂I₉]	F(000) = 2448
M_r = 1439.75	D_x = 4.016 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 5949 reflections
a = 14.394 (3) Å	θ = 1.7–28.4°
b = 8.0685 (18) Å	µ = 13.92 mm⁻¹
c = 20.505 (5) Å	T = 223 K
β = 90.530 (4)°	Prism, red
V = 2381.4 (9) Å³	0.15 × 0.12 × 0.10 mm
Z = 4

Data collection top

Bruker SMART Apex CCD diffractometer	5949 independent reflections
Radiation source: fine-focus sealed tube	4013 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.067
ω scan	θ_max = 28.4°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Bruker, 1998)	h = −19→19
T_min = 0.151, T_max = 0.251	k = −10→10
31497 measured reflections	l = −27→27

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.041	H-atom parameters not refined
wR(F²) = 0.089	w = 1/[σ²(F_o²) + (0.0263P)² + 6.8306P] where P = (F_o² + 2F_c²)/3
S = 1.01	(Δ/σ)_max < 0.001
5949 reflections	Δρ_max = 1.09 e Å⁻³
127 parameters	Δρ_min = −0.98 e Å⁻³
0 restraints

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	U_iso*/U_eq
Sb1	0.16664 (4)	0.00860 (6)	0.34432 (3)	0.02174 (13)
Sb2	−0.16322 (4)	0.00890 (6)	0.15384 (3)	0.02196 (13)
I1	0.04655 (4)	0.20488 (7)	0.42306 (3)	0.03198 (15)
I2	0.12331 (4)	−0.28781 (7)	0.41543 (3)	0.03279 (15)
I3	0.30075 (4)	−0.17702 (7)	0.24474 (3)	0.03158 (15)
I5	0.00464 (4)	−0.08553 (8)	0.24624 (4)	0.03950 (16)
I4	0.32819 (4)	0.07776 (8)	0.42179 (3)	0.03589 (17)
I6	−0.24153 (4)	0.19363 (7)	0.28128 (3)	0.03102 (15)
I7	−0.07208 (4)	0.30328 (7)	0.11033 (3)	0.03199 (15)
I8	−0.08585 (4)	−0.19324 (7)	0.05466 (3)	0.03291 (15)
I9	−0.32917 (4)	0.06904 (8)	0.07921 (3)	0.03696 (17)
N1	0.5345 (5)	−0.0243 (10)	0.2242 (4)	0.039 (2)
N2	0.1488 (6)	0.0288 (11)	0.1100 (4)	0.049 (2)
N3	0.1876 (6)	0.9815 (11)	0.5630 (5)	0.053 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sb1	0.0202 (3)	0.0235 (3)	0.0215 (3)	0.0013 (2)	0.0011 (2)	−0.0001 (3)
Sb2	0.0213 (3)	0.0229 (3)	0.0217 (3)	−0.0011 (2)	0.0007 (2)	−0.0005 (3)
I1	0.0306 (3)	0.0321 (3)	0.0333 (4)	0.0051 (2)	0.0076 (3)	−0.0054 (3)
I2	0.0361 (3)	0.0274 (3)	0.0350 (4)	−0.0012 (2)	0.0056 (3)	0.0080 (3)
I3	0.0295 (3)	0.0293 (3)	0.0360 (4)	0.0019 (2)	0.0074 (3)	−0.0083 (3)
I5	0.0291 (3)	0.0475 (4)	0.0415 (4)	−0.0066 (3)	−0.0151 (3)	0.0081 (3)
I4	0.0266 (3)	0.0450 (4)	0.0359 (4)	−0.0034 (3)	−0.0098 (3)	0.0003 (3)
I6	0.0345 (3)	0.0272 (3)	0.0315 (4)	0.0048 (2)	0.0058 (3)	−0.0055 (2)
I7	0.0347 (3)	0.0265 (3)	0.0348 (4)	−0.0072 (2)	0.0046 (3)	0.0048 (2)
I8	0.0380 (3)	0.0322 (3)	0.0286 (3)	0.0032 (3)	0.0064 (3)	−0.0061 (3)
I9	0.0283 (3)	0.0450 (4)	0.0373 (4)	−0.0011 (3)	−0.0106 (3)	0.0056 (3)
N1	0.034 (4)	0.039 (5)	0.045 (5)	0.000 (4)	0.003 (4)	0.008 (4)
N2	0.049 (5)	0.056 (6)	0.042 (6)	−0.005 (4)	−0.003 (4)	0.010 (5)
N3	0.054 (5)	0.054 (6)	0.050 (6)	−0.012 (5)	−0.006 (5)	0.014 (5)

Geometric parameters (Å, º) top

Sb1—I1	2.8556 (8)	Sb2—I8	2.8422 (9)
Sb1—I4	2.8591 (9)	Sb2—I7	2.8602 (9)
Sb1—I2	2.8725 (9)	Sb2—I9	2.8664 (9)
Sb1—I5	3.1579 (10)	Sb2—I5	3.1501 (10)
Sb1—I3ⁱ	3.1633 (9)	Sb2—I6ⁱⁱ	3.1865 (9)
Sb1—I3	3.1956 (9)	Sb2—I6	3.2211 (9)

I1—Sb1—I4	94.08 (3)	I7—Sb2—I9	94.32 (3)
I1—Sb1—I2	92.26 (3)	I8—Sb2—I5	89.32 (3)
I4—Sb1—I2	93.42 (3)	I7—Sb2—I5	92.12 (2)
I1—Sb1—I5	92.65 (3)	I9—Sb2—I5	173.14 (3)
I4—Sb1—I5	173.12 (3)	I8—Sb2—I6ⁱⁱ	90.78 (3)
I2—Sb1—I5	87.74 (2)	I7—Sb2—I6ⁱⁱ	173.49 (3)
I1—Sb1—I3ⁱ	88.60 (3)	I9—Sb2—I6ⁱⁱ	89.90 (2)
I4—Sb1—I3ⁱ	92.29 (2)	I5—Sb2—I6ⁱⁱ	83.48 (2)
I2—Sb1—I3ⁱ	174.15 (3)	I8—Sb2—I6	171.27 (3)
I5—Sb1—I3ⁱ	86.44 (2)	I7—Sb2—I6	91.94 (2)
I1—Sb1—I3	173.51 (3)	I9—Sb2—I6	93.36 (3)
I4—Sb1—I3	87.33 (3)	I5—Sb2—I6	84.04 (3)
I2—Sb1—I3	93.98 (3)	I6ⁱⁱ—Sb2—I6	82.85 (2)
I5—Sb1—I3	85.83 (3)	Sb1ⁱⁱⁱ—I3—Sb1	146.98 (2)
I3ⁱ—Sb1—I3	85.02 (2)	Sb2—I5—Sb1	151.96 (3)
I8—Sb2—I7	93.98 (3)	Sb2^iv—I6—Sb2	149.68 (2)
I8—Sb2—I9	92.59 (3)

Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x−1/2, y−1/2, −z+1/2; (iii) −x+1/2, y−1/2, −z+1/2; (iv) −x−1/2, y+1/2, −z+1/2.

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Tri­ammonium nona­iodo­diantimonate(III), (NH4)3[Sb2I9]

Supporting information

Key indicators

checkCIF/PLATON results

Triammonium nonaiododiantimonate(III), (NH₄)₃[Sb₂I₉]