metal-organic compounds
Bis(hydroxyammonium) hexachloridoplatinate(IV)–18-crown-6 (1/2)
aDepartment of Chemistry, Saint Petersburg State University, Universitetsky Pr. 26, 198504 Stary Petergof, Russian Federation, and bDepartment of Chemistry, University of Jyvaskyla, PO Box 35 FI-40014 Jyvaskyla, Finland
*Correspondence e-mail: tgc@mail.ru
In the title complex, (NH3OH)2[PtCl6]·2C12H24O6, the PtIV atom is coordinated by six chloride anions in a slightly distorted octahedral geometry. The Pt—Cl bond lengths are comparable to those reported for other hexachloridoplatinate(IV) species. The hydroxyammonium groups act as linkers between the [PtCl6]2− anion and the crown ether molecules. The anion is linked to two hydroxyammonium cations via O—H⋯Cl hydrogen bonds and each hydroxyammonium moiety is linked to a crown ether molecule by hydrogen bonds between ammonium H atoms and 18-crown-6 O atoms. The crown ether molecules have the classic crown shape in which all O atoms are located in the inner part of the crown ether ring and all –CH2– groups are turned to the outside.
CCDC reference: 968918
Related literature
For general background to supramolecular assemblies, see: Saalfrank & Demleitner (1999). For crystal structures of related compounds based on platinum complexes and crown ether molecules, see: Bulatov et al. (2012).
Experimental
Crystal data
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Data collection: APEX2 (Bruker, 2009); cell SAINT (Bruker, 2009); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008b); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.
Supporting information
CCDC reference: 968918
https://doi.org/10.1107/S1600536813032649/pk2505sup1.cif
contains datablock I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536813032649/pk2505Isup2.hkl
Supporting information file. DOI: https://doi.org/10.1107/S1600536813032649/pk2505Isup3.cdx
A mixture of cis-[PtCl2(HON=C(CH3)2)2] (0.045 mmol, 0.019 g) and N,N-dichlorotosylamide (0.090 mmol, 0.022 g) in chloroform (5 mL) was refluxed for 2 h, whereupon the reaction mixture was passed through a silica gel (60 Å; Merck) column using chloroform as the
The resulting yellow solid was co-crystallized with 18-crown-6 in a 1:2 molar ratio from an acetone:chloroform (2:3, v/v) solution at 20–25 °C to give yellow crystals (yield 46%).The OH hydrogen atom was located in a difference Fourier map but refined with fixed distances and angles (O—H = 0.84 Å and N—O—H = 109.47°) using a riding model with Uiso = 1.5Ueq of the parent atom. The NH3 hydrogen atoms were also found in a difference Fourier map, but were subsequently constrained to ride on their parent atom, with N—H = 0.91 Å and Uiso = 1.5Ueq (parent atom). The other hydrogen atoms were positioned geometrically and constrained to ride on their parent atoms, with C—H = 0.99 and Uiso = 1.2Ueq(parent atom).
The
of the title complex contains one Pt atom coordinated by six Cl atoms in an octahedral geometry (Fig. 1). The Pt—Cl1, Pt—Cl3, and Pt—Cl4 distances are 2.328 (3), 2.3202 (10), and 2.3184 (10) Å, respectively. The hydroxyammonium ions act as linkers between the [PtCl6]2- moieties and the crown ether molecules. The O—H···Cl and N—H···O hydrogen bond parameters are given in Table 1. Association with the platinum complexes changes the conformation of the crown ether. Thus, the cavity of the free 18-crown-6 has two inward-turned CH2 groups and two oxygens with the electron pairs facing outward and away from the center. In other words, the free crown ether does not display the true crown shape or cavity. However, in the presence of (NH3OH)2[PtCl6], reorganization of the crown occurs to give the classic crown shape in which all oxygen atoms are located in the inner part of the crown ring and all CH2 groups are turned to the outside.For general background to supramolecular assemblies, see: Saalfrank & Demleitner (1999). For crystal structures of related compounds based on platinum complexes and crown ether molecules, see: Bulatov et al. (2012).
Data collection: APEX2 (Bruker, 2009); cell
SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008b); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008b).Fig. 1. The molecular structure of the title compound with displacement ellipsoids drawn at the 50% probability level. |
(NH4O)2[PtCl6](C12H24O6)2 | F(000) = 4048 |
Mr = 1004.50 | Dx = 1.733 Mg m−3 |
Orthorhombic, Fdd2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: F 2 -2d | Cell parameters from 9098 reflections |
a = 29.6079 (10) Å | θ = 2.6–30.0° |
b = 30.5302 (10) Å | µ = 4.12 mm−1 |
c = 8.5175 (3) Å | T = 100 K |
V = 7699.3 (5) Å3 | Needle, yellow |
Z = 8 | 0.48 × 0.12 × 0.11 mm |
Bruker Kappa APEXII DUO CCD diffractometer | 4628 independent reflections |
Radiation source: fine-focus sealed tube | 4037 reflections with I > 2σ(I) |
Curved graphite crystal monochromator | Rint = 0.067 |
Detector resolution: 16 pixels mm-1 | θmax = 28.3°, θmin = 1.9° |
φ scans and ω scans with κ offset | h = −39→39 |
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a) | k = −40→40 |
Tmin = 0.241, Tmax = 0.664 | l = −10→11 |
29930 measured reflections |
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)] = 0.033 | H-atom parameters constrained |
wR(F2) = 0.054 | w = 1/[σ2(Fo2) + 25.8438P] where P = (Fo2 + 2Fc2)/3 |
S = 1.13 | (Δ/σ)max = 0.001 |
4628 reflections | Δρmax = 1.49 e Å−3 |
215 parameters | Δρmin = −1.23 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 2066 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.035 (6) |
(NH4O)2[PtCl6](C12H24O6)2 | V = 7699.3 (5) Å3 |
Mr = 1004.50 | Z = 8 |
Orthorhombic, Fdd2 | Mo Kα radiation |
a = 29.6079 (10) Å | µ = 4.12 mm−1 |
b = 30.5302 (10) Å | T = 100 K |
c = 8.5175 (3) Å | 0.48 × 0.12 × 0.11 mm |
Bruker Kappa APEXII DUO CCD diffractometer | 4628 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a) | 4037 reflections with I > 2σ(I) |
Tmin = 0.241, Tmax = 0.664 | Rint = 0.067 |
29930 measured reflections |
R[F2 > 2σ(F2)] = 0.033 | H-atom parameters constrained |
wR(F2) = 0.054 | w = 1/[σ2(Fo2) + 25.8438P] where P = (Fo2 + 2Fc2)/3 |
S = 1.13 | Δρmax = 1.49 e Å−3 |
4628 reflections | Δρmin = −1.23 e Å−3 |
215 parameters | Absolute structure: Flack (1983), 2066 Friedel pairs |
1 restraint | Absolute structure parameter: 0.035 (6) |
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. |
x | y | z | Uiso*/Ueq | ||
Pt1 | 0.2500 | 0.2500 | 0.34985 (5) | 0.01233 (5) | |
Cl1 | 0.2500 | 0.2500 | 0.0765 (3) | 0.0260 (7) | |
Cl2 | 0.2500 | 0.2500 | 0.6231 (3) | 0.0178 (6) | |
Cl3 | 0.22293 (3) | 0.32131 (3) | 0.35338 (17) | 0.0194 (2) | |
Cl4 | 0.17574 (3) | 0.22593 (3) | 0.34620 (17) | 0.0196 (2) | |
O1 | 0.11462 (11) | 0.22413 (11) | −0.1142 (4) | 0.0191 (7) | |
O2 | 0.09346 (12) | 0.30857 (12) | −0.2258 (4) | 0.0204 (9) | |
O3 | 0.05499 (11) | 0.36586 (11) | −0.0014 (4) | 0.0176 (7) | |
O4 | 0.01529 (11) | 0.33464 (11) | 0.2718 (4) | 0.0152 (7) | |
O5 | 0.04401 (9) | 0.24907 (13) | 0.3768 (5) | 0.0154 (10) | |
O6 | 0.06925 (10) | 0.18918 (10) | 0.1471 (3) | 0.0159 (7) | |
O7 | 0.13001 (12) | 0.30883 (12) | 0.1706 (4) | 0.0322 (9) | |
H7O | 0.1485 | 0.2909 | 0.2091 | 0.048* | |
C1 | 0.1225 (2) | 0.23742 (17) | −0.2727 (6) | 0.0288 (13) | |
H1A | 0.0953 | 0.2314 | −0.3372 | 0.035* | |
H1B | 0.1481 | 0.2207 | −0.3172 | 0.035* | |
C2 | 0.13288 (19) | 0.28539 (18) | −0.2750 (7) | 0.0298 (13) | |
H2A | 0.1583 | 0.2918 | −0.2032 | 0.036* | |
H2B | 0.1416 | 0.2946 | −0.3823 | 0.036* | |
C3 | 0.10008 (17) | 0.35477 (16) | −0.2288 (6) | 0.0222 (11) | |
H3A | 0.1054 | 0.3646 | −0.3380 | 0.027* | |
H3B | 0.1269 | 0.3625 | −0.1652 | 0.027* | |
C4 | 0.05936 (15) | 0.37703 (15) | −0.1643 (6) | 0.0194 (10) | |
H4A | 0.0624 | 0.4092 | −0.1760 | 0.023* | |
H4B | 0.0321 | 0.3675 | −0.2225 | 0.023* | |
C5 | 0.02007 (16) | 0.39000 (15) | 0.0749 (5) | 0.0196 (11) | |
H5A | −0.0098 | 0.3813 | 0.0328 | 0.024* | |
H5B | 0.0242 | 0.4218 | 0.0564 | 0.024* | |
C6 | 0.02242 (17) | 0.38033 (15) | 0.2473 (6) | 0.0193 (10) | |
H6A | 0.0524 | 0.3889 | 0.2888 | 0.023* | |
H6B | −0.0009 | 0.3974 | 0.3037 | 0.023* | |
C7 | 0.02376 (18) | 0.32346 (16) | 0.4320 (6) | 0.0200 (11) | |
H7A | 0.0053 | 0.3422 | 0.5019 | 0.024* | |
H7B | 0.0560 | 0.3284 | 0.4572 | 0.024* | |
C8 | 0.01196 (16) | 0.27634 (16) | 0.4571 (6) | 0.0204 (11) | |
H8A | 0.0123 | 0.2696 | 0.5708 | 0.025* | |
H8B | −0.0188 | 0.2705 | 0.4167 | 0.025* | |
C9 | 0.03121 (15) | 0.20407 (14) | 0.3860 (5) | 0.0166 (10) | |
H9A | 0.0018 | 0.1996 | 0.3330 | 0.020* | |
H9B | 0.0280 | 0.1952 | 0.4973 | 0.020* | |
C10 | 0.06677 (15) | 0.17702 (15) | 0.3083 (5) | 0.0159 (10) | |
H10A | 0.0963 | 0.1820 | 0.3598 | 0.019* | |
H10B | 0.0592 | 0.1455 | 0.3175 | 0.019* | |
C11 | 0.10475 (15) | 0.16589 (16) | 0.0690 (5) | 0.0191 (11) | |
H11A | 0.1000 | 0.1339 | 0.0802 | 0.023* | |
H11B | 0.1342 | 0.1734 | 0.1168 | 0.023* | |
C12 | 0.10464 (18) | 0.17826 (17) | −0.1014 (6) | 0.0194 (12) | |
H12A | 0.1276 | 0.1610 | −0.1587 | 0.023* | |
H12B | 0.0747 | 0.1720 | −0.1480 | 0.023* | |
N1 | 0.09142 (12) | 0.28600 (12) | 0.1164 (5) | 0.0180 (8) | |
H1C | 0.0998 | 0.2660 | 0.0429 | 0.027* | |
H1D | 0.0716 | 0.3053 | 0.0732 | 0.027* | |
H1E | 0.0780 | 0.2720 | 0.1985 | 0.027* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.01615 (9) | 0.00846 (9) | 0.01239 (9) | −0.00288 (16) | 0.000 | 0.000 |
Cl1 | 0.0447 (18) | 0.0187 (15) | 0.0145 (16) | −0.0078 (8) | 0.000 | 0.000 |
Cl2 | 0.0220 (14) | 0.0191 (14) | 0.0123 (14) | −0.0011 (7) | 0.000 | 0.000 |
Cl3 | 0.0241 (5) | 0.0112 (5) | 0.0229 (5) | −0.0006 (4) | −0.0023 (6) | 0.0014 (6) |
Cl4 | 0.0179 (5) | 0.0172 (5) | 0.0237 (5) | −0.0064 (4) | −0.0031 (6) | 0.0034 (6) |
O1 | 0.0255 (18) | 0.0156 (17) | 0.016 (2) | 0.0005 (14) | 0.0061 (14) | −0.0010 (14) |
O2 | 0.027 (2) | 0.016 (2) | 0.0184 (18) | −0.0011 (16) | 0.0046 (15) | −0.0011 (15) |
O3 | 0.0233 (18) | 0.0147 (18) | 0.0146 (16) | 0.0019 (14) | 0.0004 (14) | 0.0031 (14) |
O4 | 0.0220 (18) | 0.0102 (17) | 0.0136 (16) | 0.0005 (13) | −0.0005 (13) | −0.0006 (13) |
O5 | 0.0187 (13) | 0.0102 (13) | 0.017 (3) | 0.0021 (17) | 0.0054 (14) | −0.0013 (16) |
O6 | 0.0195 (17) | 0.0151 (17) | 0.0130 (17) | 0.0023 (13) | 0.0018 (12) | −0.0003 (12) |
O7 | 0.026 (2) | 0.022 (2) | 0.049 (2) | −0.0009 (16) | −0.0164 (17) | 0.0057 (18) |
C1 | 0.039 (3) | 0.027 (3) | 0.020 (3) | 0.004 (2) | 0.013 (2) | 0.000 (2) |
C2 | 0.033 (3) | 0.030 (3) | 0.026 (3) | 0.005 (3) | 0.012 (3) | 0.004 (3) |
C3 | 0.032 (3) | 0.017 (3) | 0.017 (2) | −0.008 (2) | 0.000 (2) | 0.003 (2) |
C4 | 0.029 (2) | 0.014 (2) | 0.015 (2) | −0.0047 (18) | −0.005 (2) | 0.004 (2) |
C5 | 0.024 (2) | 0.010 (2) | 0.024 (3) | 0.0044 (18) | −0.001 (2) | 0.003 (2) |
C6 | 0.026 (3) | 0.011 (2) | 0.021 (3) | 0.000 (2) | 0.003 (2) | 0.000 (2) |
C7 | 0.027 (3) | 0.017 (3) | 0.016 (3) | 0.000 (2) | 0.003 (2) | −0.002 (2) |
C8 | 0.025 (3) | 0.018 (3) | 0.018 (2) | 0.0057 (19) | 0.007 (2) | 0.002 (2) |
C9 | 0.020 (2) | 0.011 (2) | 0.018 (3) | −0.0035 (18) | 0.0008 (18) | 0.0010 (18) |
C10 | 0.019 (2) | 0.010 (2) | 0.018 (3) | −0.0010 (18) | −0.0015 (18) | 0.0013 (18) |
C11 | 0.021 (2) | 0.016 (2) | 0.021 (3) | 0.0044 (18) | 0.001 (2) | −0.0034 (19) |
C12 | 0.023 (3) | 0.015 (3) | 0.019 (3) | 0.000 (2) | 0.001 (2) | −0.006 (2) |
N1 | 0.0226 (19) | 0.0145 (19) | 0.017 (2) | −0.0013 (15) | 0.0002 (19) | 0.0010 (19) |
Pt1—Cl4 | 2.3184 (10) | C3—H3B | 0.9900 |
Pt1—Cl4i | 2.3184 (10) | C4—H4A | 0.9900 |
Pt1—Cl3i | 2.3202 (10) | C4—H4B | 0.9900 |
Pt1—Cl3 | 2.3202 (10) | C5—C6 | 1.499 (7) |
Pt1—Cl2 | 2.327 (3) | C5—H5A | 0.9900 |
Pt1—Cl1 | 2.328 (3) | C5—H5B | 0.9900 |
O1—C1 | 1.428 (6) | C6—H6A | 0.9900 |
O1—C12 | 1.435 (6) | C6—H6B | 0.9900 |
O2—C3 | 1.424 (6) | C7—C8 | 1.496 (7) |
O2—C2 | 1.428 (6) | C7—H7A | 0.9900 |
O3—C5 | 1.427 (5) | C7—H7B | 0.9900 |
O3—C4 | 1.435 (6) | C8—H8A | 0.9900 |
O4—C6 | 1.426 (5) | C8—H8B | 0.9900 |
O4—C7 | 1.429 (5) | C9—C10 | 1.493 (6) |
O5—C9 | 1.427 (6) | C9—H9A | 0.9900 |
O5—C8 | 1.436 (6) | C9—H9B | 0.9900 |
O6—C10 | 1.425 (5) | C10—H10A | 0.9900 |
O6—C11 | 1.432 (5) | C10—H10B | 0.9900 |
O7—N1 | 1.416 (5) | C11—C12 | 1.500 (6) |
O7—H7O | 0.8400 | C11—H11A | 0.9900 |
C1—C2 | 1.497 (7) | C11—H11B | 0.9900 |
C1—H1A | 0.9900 | C12—H12A | 0.9900 |
C1—H1B | 0.9900 | C12—H12B | 0.9900 |
C2—H2A | 0.9900 | N1—H1C | 0.9100 |
C2—H2B | 0.9900 | N1—H1D | 0.9100 |
C3—C4 | 1.489 (6) | N1—H1E | 0.9100 |
C3—H3A | 0.9900 | ||
Cl4—Pt1—Cl4i | 178.46 (7) | C6—C5—H5B | 110.1 |
Cl4—Pt1—Cl3i | 91.73 (4) | H5A—C5—H5B | 108.4 |
Cl4i—Pt1—Cl3i | 88.29 (4) | O4—C6—C5 | 109.2 (4) |
Cl4—Pt1—Cl3 | 88.29 (4) | O4—C6—H6A | 109.8 |
Cl4i—Pt1—Cl3 | 91.73 (4) | C5—C6—H6A | 109.8 |
Cl3i—Pt1—Cl3 | 178.52 (7) | O4—C6—H6B | 109.8 |
Cl4—Pt1—Cl2 | 90.77 (4) | C5—C6—H6B | 109.8 |
Cl4i—Pt1—Cl2 | 90.77 (4) | H6A—C6—H6B | 108.3 |
Cl3i—Pt1—Cl2 | 89.26 (4) | O4—C7—C8 | 109.0 (4) |
Cl3—Pt1—Cl2 | 89.26 (4) | O4—C7—H7A | 109.9 |
Cl4—Pt1—Cl1 | 89.23 (4) | C8—C7—H7A | 109.9 |
Cl4i—Pt1—Cl1 | 89.23 (4) | O4—C7—H7B | 109.9 |
Cl3i—Pt1—Cl1 | 90.74 (4) | C8—C7—H7B | 109.9 |
Cl3—Pt1—Cl1 | 90.74 (4) | H7A—C7—H7B | 108.3 |
Cl2—Pt1—Cl1 | 180.000 (1) | O5—C8—C7 | 109.6 (4) |
C1—O1—C12 | 112.5 (4) | O5—C8—H8A | 109.8 |
C3—O2—C2 | 111.9 (4) | C7—C8—H8A | 109.8 |
C5—O3—C4 | 112.5 (3) | O5—C8—H8B | 109.8 |
C6—O4—C7 | 110.3 (4) | C7—C8—H8B | 109.8 |
C9—O5—C8 | 110.9 (3) | H8A—C8—H8B | 108.2 |
C10—O6—C11 | 110.8 (3) | O5—C9—C10 | 108.7 (4) |
N1—O7—H7O | 109.5 | O5—C9—H9A | 109.9 |
O1—C1—C2 | 108.9 (4) | C10—C9—H9A | 109.9 |
O1—C1—H1A | 109.9 | O5—C9—H9B | 109.9 |
C2—C1—H1A | 109.9 | C10—C9—H9B | 109.9 |
O1—C1—H1B | 109.9 | H9A—C9—H9B | 108.3 |
C2—C1—H1B | 109.9 | O6—C10—C9 | 108.6 (4) |
H1A—C1—H1B | 108.3 | O6—C10—H10A | 110.0 |
O2—C2—C1 | 108.2 (4) | C9—C10—H10A | 110.0 |
O2—C2—H2A | 110.1 | O6—C10—H10B | 110.0 |
C1—C2—H2A | 110.1 | C9—C10—H10B | 110.0 |
O2—C2—H2B | 110.1 | H10A—C10—H10B | 108.3 |
C1—C2—H2B | 110.1 | O6—C11—C12 | 108.8 (4) |
H2A—C2—H2B | 108.4 | O6—C11—H11A | 109.9 |
O2—C3—C4 | 109.5 (4) | C12—C11—H11A | 109.9 |
O2—C3—H3A | 109.8 | O6—C11—H11B | 109.9 |
C4—C3—H3A | 109.8 | C12—C11—H11B | 109.9 |
O2—C3—H3B | 109.8 | H11A—C11—H11B | 108.3 |
C4—C3—H3B | 109.8 | O1—C12—C11 | 108.6 (4) |
H3A—C3—H3B | 108.2 | O1—C12—H12A | 110.0 |
O3—C4—C3 | 108.7 (4) | C11—C12—H12A | 110.0 |
O3—C4—H4A | 109.9 | O1—C12—H12B | 110.0 |
C3—C4—H4A | 109.9 | C11—C12—H12B | 110.0 |
O3—C4—H4B | 109.9 | H12A—C12—H12B | 108.4 |
C3—C4—H4B | 109.9 | O7—N1—H1C | 109.5 |
H4A—C4—H4B | 108.3 | O7—N1—H1D | 109.5 |
O3—C5—C6 | 108.1 (4) | H1C—N1—H1D | 109.5 |
O3—C5—H5A | 110.1 | O7—N1—H1E | 109.5 |
C6—C5—H5A | 110.1 | H1C—N1—H1E | 109.5 |
O3—C5—H5B | 110.1 | H1D—N1—H1E | 109.5 |
Symmetry code: (i) −x+1/2, −y+1/2, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7O···Cl4 | 0.84 | 2.44 | 3.237 (4) | 159 |
O7—H7O···Cl3 | 0.84 | 2.69 | 3.184 (4) | 119 |
N1—H1C···O1 | 0.91 | 1.90 | 2.811 (5) | 177 |
N1—H1D···O3 | 0.91 | 2.02 | 2.849 (5) | 152 |
N1—H1D···O4 | 0.91 | 2.54 | 3.006 (5) | 113 |
N1—H1E···O5 | 0.91 | 1.95 | 2.856 (6) | 172 |
N1—H1E···O6 | 0.91 | 2.58 | 3.039 (5) | 112 |
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7O···Cl4 | 0.84 | 2.44 | 3.237 (4) | 158.6 |
O7—H7O···Cl3 | 0.84 | 2.69 | 3.184 (4) | 119.3 |
N1—H1C···O1 | 0.91 | 1.90 | 2.811 (5) | 177.3 |
N1—H1D···O3 | 0.91 | 2.02 | 2.849 (5) | 151.6 |
N1—H1D···O4 | 0.91 | 2.54 | 3.006 (5) | 112.5 |
N1—H1E···O5 | 0.91 | 1.95 | 2.856 (6) | 172.2 |
N1—H1E···O6 | 0.91 | 2.58 | 3.039 (5) | 111.9 |
Acknowledgements
The authors are grateful to the Russian Fund for Basic Research for grant 11–03-90417, Saint Petersburg State University for a research grant (2011–2013), and the Ministry of Education and Science of the Russian Federation for the Scholarship of the President of the Russian Federation for Students and PhD Students Training Abroad (2013–2014).
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The crystal structure of the title complex contains one Pt atom coordinated by six Cl atoms in an octahedral geometry (Fig. 1). The Pt—Cl1, Pt—Cl3, and Pt—Cl4 distances are 2.328 (3), 2.3202 (10), and 2.3184 (10) Å, respectively. The hydroxyammonium ions act as linkers between the [PtCl6]2- moieties and the crown ether molecules. The O—H···Cl and N—H···O hydrogen bond parameters are given in Table 1. Association with the platinum complexes changes the conformation of the crown ether. Thus, the cavity of the free 18-crown-6 has two inward-turned CH2 groups and two oxygens with the electron pairs facing outward and away from the center. In other words, the free crown ether does not display the true crown shape or cavity. However, in the presence of (NH3OH)2[PtCl6], reorganization of the crown occurs to give the classic crown shape in which all oxygen atoms are located in the inner part of the crown ring and all CH2 groups are turned to the outside.