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Bis­(diiso­propyl­ammonium) hexa­chloro­iridate(IV), [{(H3C)2CH}2NH2]2[IrCl6], crystallizes in the monoclinic centrosymmetric space group P21/c with two crystallographically independent [IrCl6]2- anions, each located on a center of symmetry, and two crystallographically independent diiso­propyl­ammonium cations in general positions. Weak hydrogen bonding occurs between the cations and anions to form layers parallel to the bc plane. Each layer is built by annealed 24-membered rings that can be classified according to Etter's nomenclature as R88(24). The structural relationship between K3[IrCl6] and the title compound shows that a replacement of three potassium cations by two diiso­propyl­ammonium cations leads to a layered structure. The hydro­philic layers that are dominated by hexa­chloro­iridate(IV) anions are separated by lipophilic regions in the planes at x = 1/4 and x = 3/4.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802000417/tk6045sup1.cif
Contains datablocks I, iridip

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802000417/tk6045Isup2.hkl
Contains datablock I

CCDC reference: 180757

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.034
  • wR factor = 0.094
  • Data-to-parameter ratio = 19.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Computing details top

Data collection: CrysAlis (Kuma, 2000); cell refinement: CrysAlis RED (Kuma, 2000); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

bis(diisopropylammonium) hexachloroiridate(IV) top
Crystal data top
(C6H16N)2[IrCl6]F(000) = 1188
Mr = 609.30Dx = 1.802 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 693 reflections
a = 16.0939 (14) Åθ = 5–20°
b = 10.3961 (12) ŵ = 6.66 mm1
c = 13.6382 (13) ÅT = 293 K
β = 100.196 (9)°Plate, dark red
V = 2245.8 (4) Å30.20 × 0.10 × 0.05 mm
Z = 4
Data collection top
Stoe CCD
diffractometer
3932 independent reflections
Radiation source: fine-focus sealed tube2977 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.073
ω scansθmax = 25.0°, θmin = 4.1°
Absorption correction: numerical
(XRED; Stoe & Cie, 1999)
h = 1919
Tmin = 0.294, Tmax = 0.712k = 1212
25279 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.094H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.04P)2 + 4P]
where P = (Fo2 + 2Fc2)/3
3932 reflections(Δ/σ)max = 0.001
205 parametersΔρmax = 0.89 e Å3
0 restraintsΔρmin = 0.83 e Å3
Special details top

Experimental. A thin dark-red platelet of the title compound was mounted on Stoe four-circle diffractometer equipped with a CCD-detector. For the data collection 21 omega-scans (0.7°) with different chi, phi and 2theta settings and a detector to crystal distance of 80 mm were performed. Integration procedures using variable integration masks and integration width of 0.75° yielded a data completeness of 99.3%.

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
Ir10.00000.00000.00000.04074 (11)
Cl10.06553 (10)0.16306 (14)0.10171 (12)0.0679 (4)
Cl20.12510 (9)0.04463 (15)0.05546 (13)0.0694 (4)
Cl30.03607 (11)0.14831 (15)0.12684 (12)0.0719 (4)
Ir20.50000.00000.50000.03860 (11)
Cl40.45159 (9)0.15270 (14)0.37918 (11)0.0617 (4)
Cl50.36823 (8)0.09812 (13)0.47392 (10)0.0569 (3)
Cl60.53933 (9)0.13088 (15)0.37709 (11)0.0649 (4)
N10.1171 (3)0.1428 (4)0.3486 (4)0.0573 (11)
H10.08860.21300.36270.073 (19)*
H20.10380.13020.28240.055 (16)*
C110.0840 (4)0.0300 (6)0.3986 (5)0.0618 (16)
H110.08910.05040.46960.074*
C120.0091 (4)0.0153 (6)0.3562 (6)0.077 (2)
H12A0.01640.00450.28520.116*
H12B0.03890.09070.37120.116*
H12C0.03090.05870.38520.116*
C130.1332 (4)0.0902 (6)0.3899 (5)0.0766 (18)
H13A0.13280.10870.32090.115*
H13B0.10800.16040.41980.115*
H13C0.19030.07860.42360.115*
C210.2101 (3)0.1741 (5)0.3727 (4)0.0565 (13)
H210.24160.09800.35790.068*
C220.2275 (4)0.2814 (6)0.3043 (5)0.0725 (17)
H22A0.19940.35830.31960.109*
H22B0.20700.25730.23630.109*
H22C0.28720.29670.31330.109*
C230.2366 (4)0.2051 (7)0.4810 (4)0.0753 (18)
H23A0.20810.28150.49670.113*
H23B0.29650.21890.49540.113*
H23C0.22210.13480.52040.113*
N20.3739 (3)0.2199 (4)0.1947 (3)0.0536 (11)
H30.41470.18830.24230.066 (17)*
H40.39870.27660.15910.072 (18)*
C310.3131 (4)0.2939 (6)0.2459 (4)0.0594 (14)
H310.28890.23420.28880.071*
C320.3627 (4)0.3946 (6)0.3110 (5)0.0798 (19)
H32A0.38560.45550.27000.120*
H32B0.32630.43830.34870.120*
H32C0.40800.35420.35570.120*
C330.2414 (4)0.3510 (7)0.1712 (5)0.082 (2)
H33A0.26390.41080.12900.122*
H33B0.21210.28350.13130.122*
H33C0.20290.39490.20610.122*
C410.3408 (4)0.1097 (6)0.1259 (4)0.0597 (15)
H410.30360.14510.06740.072*
C420.2905 (5)0.0175 (6)0.1774 (5)0.0749 (19)
H42A0.24200.06090.19360.112*
H42B0.27230.05370.13410.112*
H42C0.32500.01350.23740.112*
C430.4147 (5)0.0459 (7)0.0920 (6)0.0806 (19)
H43A0.39470.02100.04520.121*
H43B0.44530.10850.06070.121*
H43C0.45120.00950.14840.121*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ir10.03911 (19)0.03179 (17)0.04803 (19)0.00652 (10)0.00129 (13)0.00310 (10)
Cl10.0682 (10)0.0534 (8)0.0771 (10)0.0201 (7)0.0006 (7)0.0157 (7)
Cl20.0547 (9)0.0601 (8)0.0943 (11)0.0056 (7)0.0154 (8)0.0026 (8)
Cl30.0744 (10)0.0597 (9)0.0754 (10)0.0014 (7)0.0036 (8)0.0276 (7)
Ir20.03071 (18)0.04358 (19)0.03962 (18)0.00631 (10)0.00109 (12)0.00257 (10)
Cl40.0489 (8)0.0665 (9)0.0652 (8)0.0060 (6)0.0024 (6)0.0240 (7)
Cl50.0370 (7)0.0630 (8)0.0685 (8)0.0126 (6)0.0031 (6)0.0038 (6)
Cl60.0526 (8)0.0771 (10)0.0643 (8)0.0015 (7)0.0085 (6)0.0142 (7)
N10.052 (3)0.055 (3)0.067 (3)0.008 (2)0.018 (2)0.005 (2)
C110.067 (4)0.057 (3)0.063 (4)0.003 (3)0.016 (3)0.005 (3)
C120.059 (4)0.061 (4)0.120 (6)0.003 (3)0.037 (4)0.007 (3)
C130.071 (4)0.063 (4)0.091 (5)0.004 (3)0.001 (4)0.010 (3)
C210.043 (3)0.054 (3)0.072 (4)0.005 (2)0.011 (3)0.006 (3)
C220.049 (4)0.065 (4)0.104 (5)0.009 (3)0.014 (3)0.003 (4)
C230.073 (4)0.080 (4)0.070 (4)0.018 (3)0.004 (3)0.020 (3)
N20.043 (2)0.056 (3)0.059 (3)0.005 (2)0.001 (2)0.009 (2)
C310.051 (3)0.067 (4)0.061 (3)0.001 (3)0.014 (3)0.008 (3)
C320.084 (5)0.064 (4)0.087 (5)0.006 (3)0.006 (4)0.002 (3)
C330.057 (4)0.106 (5)0.079 (4)0.022 (4)0.004 (3)0.015 (4)
C410.057 (4)0.060 (4)0.057 (3)0.011 (3)0.004 (3)0.007 (3)
C420.079 (5)0.071 (4)0.071 (4)0.025 (3)0.002 (4)0.010 (3)
C430.092 (6)0.072 (4)0.078 (5)0.003 (4)0.016 (4)0.002 (4)
Geometric parameters (Å, º) top
Ir1—Cl32.3133 (14)C11—C131.495 (9)
Ir1—Cl12.3221 (13)C21—C231.499 (8)
Ir1—Cl22.3194 (15)C21—C221.512 (8)
Ir2—Cl42.3212 (13)N2—C411.517 (7)
Ir2—Cl52.3232 (12)N2—C311.510 (7)
Ir2—Cl62.3319 (14)N2—H30.9000
N1—C111.501 (7)N2—H40.9000
N1—C211.510 (7)C31—C321.508 (8)
N1—H10.9000C31—C331.518 (8)
N1—H20.9000C41—C421.507 (8)
C11—C121.514 (10)C41—C431.504 (9)
Cl1—Ir1—Cl289.30 (6)C23—C21—C22113.5 (5)
Cl1—Ir1—Cl390.72 (6)N1—C21—C22108.0 (4)
Cl2—Ir1—Cl390.40 (6)C23—C21—H21108.0
Cl4—Ir2—Cl590.52 (5)N1—C21—H21108.0
Cl4—Ir2—Cl689.34 (6)C41—N2—C31119.0 (4)
Cl5—Ir2—Cl689.45 (5)C41—N2—H3107.6
C11—N1—C21119.2 (5)C31—N2—H3107.6
C11—N1—H1107.5C41—N2—H4107.6
C21—N1—H1107.5C31—N2—H4107.6
C11—N1—H2107.5H3—N2—H4107.0
C21—N1—H2107.5C32—C31—N2107.8 (5)
H1—N1—H2107.0C32—C31—C33112.6 (5)
C12—C11—N1108.2 (5)N2—C31—C33111.5 (5)
C12—C11—C13112.8 (6)C42—C41—C43112.5 (6)
N1—C11—C13112.4 (5)C42—C41—N2110.6 (5)
C23—C21—N1111.0 (5)C43—C41—N2108.2 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···Cl3i0.902.503.346 (5)158
N1—H2···Cl10.902.463.329 (5)164
N2—H3···Cl60.902.543.434 (4)172
N2—H4···Cl4ii0.902.663.414 (5)142
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x+1, y1/2, z+1/2.
 

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