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Acta Crystallogr Sect E Struct Rep Online. 2010 June 1; 66(Pt 6): m631.
Published online 2010 May 8. doi:  10.1107/S1600536810015898
PMCID: PMC2979437

catena-Poly[[(18-crown-6-κ6 O)potassium]-μ-chlorido-[(1H-benzotriazol-1-ol-κN 3)chloridoplatinum(II)]-μ-(benzotriazol-1-olato-κ2 N 3:O)]

Abstract

In the structure of the title compound, [KPt(C6H4N3O)Cl2(C6H5N3O)(C12H24O6)], the PtII atom is in a distorted square-planar geometry. The crystal structure is consolidated by O—H(...)O hydrogen bonds. The measured crystal was a non-merohedral twin with four components.

Related literature

For related literature, see Anderson et al. (1963 [triangle]). For related structures, see Bosch et al. (1983 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-0m631-scheme1.jpg

Experimental

Crystal data

  • [KPt(C6H4N3O)Cl2(C6H5N3O)(C12H24O6)]
  • M r = 838.65
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m631-efi1.jpg
  • a = 14.2727 (13) Å
  • b = 10.9821 (10) Å
  • c = 20.0716 (18) Å
  • β = 99.249 (3)°
  • V = 3105.2 (5) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 4.88 mm−1
  • T = 173 K
  • 0.17 × 0.10 × 0.08 mm

Data collection

  • Bruker SMART APEXII CCD diffractometer
  • Absorption correction: multi-scan (TWINABS; Sheldrick, 1999 [triangle]) T min = 0.494, T max = 0.746
  • 10775 measured reflections
  • 10775 independent reflections
  • 9006 reflections with I > 2σ(I)

Refinement

  • R[F 2 > 2σ(F 2)] = 0.063
  • wR(F 2) = 0.178
  • S = 1.07
  • 10775 reflections
  • 382 parameters
  • H-atom parameters constrained
  • Δρmax = 1.77 e Å−3
  • Δρmin = −1.78 e Å−3

Data collection: APEX2 (Bruker, 2008 [triangle]); cell refinement: SAINT-Plus (Bruker, 2008 [triangle]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009 [triangle]).

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810015898/bt5255sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810015898/bt5255Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

supplementary crystallographic information

Comment

For related literature, see Anderson et al. (1963) and for related structures see Bosch et al. (1983).

The metal platinum exhibits the distorted square planar coordination geometry. The geometry is completed by two chorine atoms and two nitrogen atoms from the 1-oxobenzotriazole ligands. Distortion in the square-planar Pt coordination sphere is signaled by angles about Pt ranging from 88.9 (3) Å to 91.2 (3) Å. The K ion is coordinated by six oxygen atoms of the crown ether and also by one terminal Cl atom attached to the metal platinum and one O atom from the 1-oxobenzotriazole ligand forming a hexagonal pyramid. The potassium ion lies in the plane of the 18-crown 6-molecule, with mean K—O distance of 2.8 Å.

The crystal structure is consolidated by O—H···O hydrogen bonds.

Experimental

A mixture of potassium tetrachloroplatinate(II) (0.0208 g, 0.05 mmol) and 1-hydroxybenzotriazole (0.0135 g, 0.1 mmol) 18-crown-6 ether (0.013 g 0.05 mmol) in acetone (15 ml) was heated at 313 K with stirring for 30 min. The yellow colour compound formed was filtered off, and dried. The compound was then dissolved in dichloromethane and kept at 278 K. Pale yellow crystals are formed after one month on slow evaporation.

Refinement

All H atoms were positioned geometrically with C—H=0.95 Å (aromatic) C—H=0.98Å (methylene), O—H= 0.84Å and refined using a riding model with, Uiso(H)=1.2Uequ (C) and 1.5Uequ(O). The measured crystal was a non-merohedral twin with four components 0.536 (1) 0.194 (2), 0.226 (1) and 0.044 (1).

Figures

Fig. 1.
The molecular structure of the title compound, showing 50% probability displacement ellipsoids and the atom numbering scheme.

Crystal data

[KPt(C6H4N3O)Cl2(C6H5N3O)(C12H24O6)]F(000) = 1656
Mr = 838.65Dx = 1.794 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybcCell parameters from 8964 reflections
a = 14.2727 (13) Åθ = 2.3–26.9°
b = 10.9821 (10) ŵ = 4.88 mm1
c = 20.0716 (18) ÅT = 173 K
β = 99.249 (3)°Block, light yellow
V = 3105.2 (5) Å30.17 × 0.10 × 0.08 mm
Z = 4

Data collection

Bruker SMART CCD diffractometer10775 independent reflections
Radiation source: sealed Tube9006 reflections with I > 2σ(I)
graphiteRint = 0.0000
CCD scanθmax = 28.0°, θmin = 1.5°
Absorption correction: multi-scan (TWINABS; Sheldrick, 1999)h = −18→18
Tmin = 0.494, Tmax = 0.746k = 0→14
10775 measured reflectionsl = 0→26

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.063Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.178H-atom parameters constrained
S = 1.07w = 1/[σ2(Fo2) + (0.0972P)2 + 18.2058P] where P = (Fo2 + 2Fc2)/3
10775 reflections(Δ/σ)max = 0.001
382 parametersΔρmax = 1.77 e Å3
0 restraintsΔρmin = −1.78 e Å3

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 h 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. Crystal was split into 4 fragments and refined using HKLF 5/BASF method'

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Pt10.26231 (3)0.37872 (3)0.527664 (17)0.02221 (11)
Cl10.2212 (2)0.2066 (3)0.58061 (15)0.0375 (7)
Cl20.3097 (2)0.5510 (2)0.47650 (14)0.0352 (6)
N10.2340 (6)0.4823 (8)0.6036 (4)0.0229 (17)
C20.1620 (8)0.5710 (9)0.5966 (5)0.025 (2)
C30.0955 (8)0.6111 (11)0.5421 (5)0.033 (2)
H30.09400.57680.49850.040*
C40.0340 (8)0.6989 (12)0.5523 (7)0.042 (3)
H4−0.01000.72930.51560.051*
C50.0348 (10)0.7488 (11)0.6216 (7)0.039 (3)
H5−0.01130.80790.62840.047*
C60.0992 (9)0.7126 (10)0.6750 (6)0.033 (2)
H60.10180.74680.71880.039*
C70.1626 (8)0.6199 (10)0.6609 (5)0.026 (2)
N80.2308 (7)0.5555 (8)0.7023 (4)0.0261 (18)
N90.2737 (7)0.4742 (8)0.6659 (4)0.0281 (19)
O100.2552 (6)0.5648 (7)0.7691 (4)0.0341 (18)
N110.2852 (7)0.2812 (8)0.4469 (4)0.0256 (19)
C120.3658 (7)0.2703 (9)0.4180 (5)0.022 (2)
C130.4600 (9)0.3121 (10)0.4392 (5)0.029 (2)
H130.47810.35490.48040.035*
C140.5228 (9)0.2866 (11)0.3965 (6)0.034 (3)
H140.58700.31190.40810.040*
C150.4941 (9)0.2230 (12)0.3349 (6)0.038 (3)
H150.54030.20780.30670.045*
C160.4049 (9)0.1832 (10)0.3144 (6)0.030 (2)
H160.38640.14160.27280.036*
C170.3423 (8)0.2076 (9)0.3586 (5)0.028 (2)
N180.2459 (7)0.1814 (9)0.3558 (4)0.031 (2)
N190.2129 (6)0.2248 (8)0.4094 (4)0.0274 (19)
O200.1871 (6)0.1243 (9)0.3072 (4)0.0410 (19)
H200.21880.08470.28280.062*
O210.4161 (7)0.6331 (9)0.3022 (5)0.047 (2)
C220.4979 (11)0.6571 (17)0.3516 (7)0.056 (4)
H22A0.49800.60220.39070.067*
H22B0.55610.64070.33200.067*
C230.4981 (11)0.7788 (17)0.3731 (9)0.060 (5)
H23A0.55880.79710.40280.073*
H23B0.49230.83360.33350.073*
O240.4228 (7)0.7993 (8)0.4081 (5)0.041 (2)
C250.4190 (14)0.9189 (16)0.4377 (13)0.084 (7)
H25A0.47960.93500.46800.100*
H25B0.41190.98080.40140.100*
C260.3432 (19)0.9305 (19)0.4746 (11)0.093 (7)
H26A0.34651.01110.49690.111*
H26B0.34900.86720.51010.111*
O270.2539 (9)0.9180 (9)0.4314 (5)0.058 (3)
C280.1692 (19)0.9269 (17)0.4658 (11)0.085 (7)
H28A0.17520.86910.50410.103*
H28B0.16391.01030.48350.103*
C290.084 (2)0.897 (2)0.4162 (15)0.108 (10)
H29A0.02610.91170.43640.129*
H29B0.08130.95040.37600.129*
O300.0883 (8)0.7821 (13)0.3984 (6)0.072 (4)
C310.0019 (12)0.740 (3)0.3545 (10)0.090 (8)
H31A−0.05300.74860.37870.108*
H31B−0.01000.79180.31370.108*
C320.0092 (14)0.613 (3)0.3341 (10)0.092 (8)
H32A0.01740.56020.37460.111*
H32B−0.05040.58860.30480.111*
O330.0817 (8)0.5961 (12)0.3011 (6)0.072 (4)
C340.0933 (18)0.468 (2)0.2871 (12)0.096 (8)
H34A0.03160.43310.26650.115*
H34B0.11580.42420.32970.115*
C350.1637 (17)0.4551 (19)0.2400 (11)0.092 (7)
H35A0.17040.36820.22850.110*
H35B0.14200.50060.19780.110*
O360.2516 (10)0.5015 (11)0.2723 (6)0.074 (4)
C370.3247 (16)0.4920 (14)0.2324 (8)0.072 (6)
H37A0.31630.55390.19600.086*
H37B0.32470.41020.21170.086*
C380.4148 (16)0.5133 (16)0.2799 (8)0.069 (5)
H38A0.41880.45710.31890.083*
H38B0.46990.49800.25680.083*
K10.25264 (18)0.7160 (2)0.34906 (12)0.0318 (5)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Pt10.02707 (18)0.02415 (16)0.01630 (15)0.0034 (2)0.00617 (14)−0.00098 (16)
Cl10.0513 (18)0.0285 (13)0.0382 (15)0.0003 (12)0.0242 (14)0.0044 (12)
Cl20.0531 (17)0.0260 (12)0.0287 (13)−0.0019 (12)0.0135 (12)0.0038 (11)
N10.026 (4)0.025 (4)0.018 (4)0.005 (3)0.004 (3)0.004 (3)
C20.027 (5)0.028 (5)0.023 (5)0.002 (4)0.007 (4)0.000 (4)
C30.043 (6)0.035 (6)0.022 (5)0.014 (5)0.005 (4)0.000 (5)
C40.018 (5)0.051 (8)0.055 (8)0.014 (5)−0.003 (5)0.009 (6)
C50.045 (7)0.033 (6)0.041 (7)0.015 (5)0.016 (6)−0.005 (5)
C60.037 (6)0.026 (5)0.037 (6)−0.001 (5)0.013 (5)0.000 (5)
C70.036 (6)0.025 (4)0.019 (4)−0.002 (5)0.005 (4)−0.001 (4)
N80.036 (5)0.030 (5)0.013 (4)0.004 (4)0.005 (3)−0.002 (3)
N90.037 (5)0.024 (4)0.023 (4)0.007 (4)0.004 (4)0.007 (3)
O100.049 (5)0.031 (4)0.021 (4)0.008 (4)0.002 (3)−0.002 (3)
N110.035 (5)0.029 (4)0.013 (4)0.006 (4)0.004 (3)−0.003 (3)
C120.030 (5)0.019 (4)0.020 (4)0.003 (4)0.011 (4)0.001 (4)
C130.037 (6)0.031 (5)0.018 (5)−0.002 (5)0.002 (5)−0.002 (4)
C140.031 (6)0.037 (6)0.034 (6)0.009 (5)0.007 (5)−0.001 (5)
C150.041 (7)0.048 (7)0.027 (6)0.001 (6)0.016 (5)−0.006 (5)
C160.039 (6)0.031 (5)0.023 (5)0.006 (5)0.013 (5)0.003 (4)
C170.029 (6)0.023 (5)0.033 (5)0.001 (4)0.013 (5)0.001 (4)
N180.040 (6)0.036 (5)0.016 (4)0.003 (4)0.001 (4)−0.013 (4)
N190.028 (5)0.035 (5)0.020 (4)−0.002 (4)0.002 (3)−0.009 (4)
O200.043 (5)0.049 (5)0.028 (4)0.010 (5)−0.003 (3)−0.011 (4)
O210.057 (6)0.047 (5)0.038 (4)0.003 (5)0.010 (4)0.009 (4)
C220.051 (8)0.094 (13)0.028 (6)0.019 (8)0.023 (6)0.009 (7)
C230.033 (7)0.081 (12)0.066 (10)−0.005 (8)0.004 (7)0.035 (9)
O240.045 (5)0.033 (4)0.040 (5)−0.004 (4)−0.014 (4)0.006 (4)
C250.067 (12)0.041 (8)0.127 (19)−0.007 (8)−0.032 (12)−0.025 (10)
C260.13 (2)0.058 (11)0.084 (14)0.005 (13)−0.008 (15)−0.035 (10)
O270.094 (9)0.038 (5)0.047 (6)0.015 (5)0.025 (6)−0.002 (4)
C280.14 (2)0.049 (9)0.084 (14)−0.011 (11)0.081 (15)−0.017 (9)
C290.13 (2)0.090 (17)0.13 (2)0.052 (16)0.086 (19)0.021 (16)
O300.052 (7)0.093 (9)0.079 (8)0.027 (6)0.032 (6)0.037 (7)
C310.031 (9)0.19 (3)0.051 (10)0.021 (12)0.012 (7)0.019 (14)
C320.054 (11)0.16 (3)0.055 (11)−0.038 (15)0.001 (8)0.004 (14)
O330.045 (6)0.095 (10)0.075 (8)−0.024 (6)0.001 (5)0.035 (7)
C340.111 (18)0.077 (14)0.096 (16)−0.060 (13)0.008 (14)0.005 (12)
C350.125 (19)0.064 (12)0.091 (15)−0.052 (13)0.031 (14)−0.018 (11)
O360.098 (10)0.071 (8)0.060 (7)−0.047 (7)0.027 (7)−0.031 (6)
C370.137 (19)0.041 (8)0.039 (8)−0.007 (10)0.021 (10)−0.013 (6)
C380.106 (15)0.058 (10)0.045 (9)0.026 (10)0.016 (9)0.007 (7)
K10.0270 (12)0.0395 (13)0.0281 (11)−0.0044 (10)0.0020 (9)−0.0003 (10)

Geometric parameters (Å, °)

Pt1—N11.996 (8)C23—H23A0.9900
Pt1—N112.013 (8)C23—H23B0.9900
Pt1—Cl12.290 (3)O24—C251.446 (19)
Pt1—Cl22.306 (3)O24—K12.687 (9)
Cl2—K13.133 (4)C25—C261.41 (3)
N1—N91.290 (12)C25—K13.523 (16)
N1—C21.407 (13)C25—H25A0.9900
C2—C71.396 (13)C25—H25B0.9900
C2—C31.399 (15)C26—O271.43 (3)
C3—C41.341 (16)C26—K13.538 (19)
C3—H30.9500C26—H26A0.9900
C4—C51.492 (19)C26—H26B0.9900
C4—H40.9500O27—C281.49 (2)
C5—C61.355 (18)O27—K12.764 (10)
C5—H50.9500C28—C291.48 (4)
C6—C71.421 (15)C28—H28A0.9900
C6—H60.9500C28—H28B0.9900
C7—N81.371 (14)C29—O301.32 (3)
N8—O101.334 (11)C29—H29A0.9900
N8—N91.360 (12)C29—H29B0.9900
O10—K1i2.897 (8)O30—C311.47 (2)
N11—N191.329 (13)O30—K12.785 (11)
N11—C121.374 (13)C31—C321.46 (3)
C12—C171.371 (14)C31—H31A0.9900
C12—C131.420 (16)C31—H31B0.9900
C13—C141.366 (16)C32—O331.33 (2)
C13—H130.9500C32—H32A0.9900
C14—C151.422 (17)C32—H32B0.9900
C14—H140.9500O33—C341.44 (3)
C15—C161.346 (18)O33—K12.804 (11)
C15—H150.9500C34—C351.49 (3)
C16—C171.382 (14)C34—H34A0.9900
C16—H160.9500C34—H34B0.9900
C17—N181.398 (15)C35—O361.41 (2)
N18—N191.331 (12)C35—H35A0.9900
N18—O201.336 (12)C35—H35B0.9900
O20—H200.8400O36—C371.42 (2)
O21—C381.39 (2)O36—K12.814 (11)
O21—C221.430 (18)C37—C381.49 (3)
O21—K12.804 (10)C37—H37A0.9900
C22—C231.41 (2)C37—H37B0.9900
C22—H22A0.9900C38—H38A0.9900
C22—H22B0.9900C38—H38B0.9900
C23—O241.393 (19)K1—O10ii2.897 (8)
C23—K13.527 (15)
N1—Pt1—N11176.3 (3)H28A—C28—H28B108.4
N1—Pt1—Cl191.0 (3)O30—C29—C28109 (2)
N11—Pt1—Cl191.2 (3)O30—C29—H29A109.9
N1—Pt1—Cl289.0 (3)C28—C29—H29A109.9
N11—Pt1—Cl288.9 (3)O30—C29—H29B109.9
Cl1—Pt1—Cl2177.77 (12)C28—C29—H29B109.9
Pt1—Cl2—K1141.43 (13)H29A—C29—H29B108.3
N9—N1—C2110.2 (8)C29—O30—C31113 (2)
N9—N1—Pt1126.1 (7)C29—O30—K1115.1 (13)
C2—N1—Pt1123.6 (7)C31—O30—K1112.2 (10)
C7—C2—C3120.3 (10)C32—C31—O30112.2 (16)
C7—C2—N1106.1 (9)C32—C31—H31A109.2
C3—C2—N1133.5 (9)O30—C31—H31A109.2
C4—C3—C2118.9 (11)C32—C31—H31B109.2
C4—C3—H3120.5O30—C31—H31B109.2
C2—C3—H3120.5H31A—C31—H31B107.9
C3—C4—C5120.0 (11)O33—C32—C31111.7 (18)
C3—C4—H4120.0O33—C32—H32A109.3
C5—C4—H4120.0C31—C32—H32A109.3
C6—C5—C4122.2 (11)O33—C32—H32B109.3
C6—C5—H5118.9C31—C32—H32B109.3
C4—C5—H5118.9H32A—C32—H32B108.0
C5—C6—C7115.1 (11)C32—O33—C34110.8 (17)
C5—C6—H6122.4C32—O33—K1117.9 (13)
C7—C6—H6122.4C34—O33—K1113.7 (12)
N8—C7—C2105.1 (9)O33—C34—C35109.2 (15)
N8—C7—C6131.4 (9)O33—C34—H34A109.9
C2—C7—C6123.4 (10)C35—C34—H34A109.9
O10—N8—N9121.5 (9)O33—C34—H34B109.9
O10—N8—C7128.0 (9)C35—C34—H34B109.9
N9—N8—C7110.5 (8)H34A—C34—H34B108.3
N1—N9—N8108.0 (8)O36—C35—C34108.2 (17)
N8—O10—K1i126.6 (6)O36—C35—H35A110.1
N19—N11—C12110.3 (8)C34—C35—H35A110.1
N19—N11—Pt1119.5 (7)O36—C35—H35B110.1
C12—N11—Pt1129.9 (7)C34—C35—H35B110.1
C17—C12—N11107.9 (9)H35A—C35—H35B108.4
C17—C12—C13120.7 (9)C35—O36—C37113.3 (13)
N11—C12—C13131.4 (9)C35—O36—K1118.7 (12)
C14—C13—C12115.5 (10)C37—O36—K1115.5 (9)
C14—C13—H13122.3O36—C37—C38105.3 (12)
C12—C13—H13122.3O36—C37—H37A110.7
C13—C14—C15121.4 (12)C38—C37—H37A110.7
C13—C14—H14119.3O36—C37—H37B110.7
C15—C14—H14119.3C38—C37—H37B110.7
C16—C15—C14123.5 (11)H37A—C37—H37B108.8
C16—C15—H15118.3O21—C38—C37108.6 (14)
C14—C15—H15118.3O21—C38—H38A110.0
C15—C16—C17114.6 (11)C37—C38—H38A110.0
C15—C16—H16122.7O21—C38—H38B110.0
C17—C16—H16122.7C37—C38—H38B110.0
C12—C17—C16124.3 (11)H38A—C38—H38B108.3
C12—C17—N18103.8 (9)O24—K1—O2762.9 (3)
C16—C17—N18131.9 (11)O24—K1—O30120.5 (4)
N19—N18—O20119.6 (9)O27—K1—O3060.2 (4)
N19—N18—C17111.6 (9)O24—K1—O33170.7 (3)
O20—N18—C17128.7 (9)O27—K1—O33120.3 (4)
N11—N19—N18106.3 (8)O30—K1—O3360.5 (4)
N18—O20—H20109.5O24—K1—O2161.1 (3)
C38—O21—C22111.3 (13)O27—K1—O21122.3 (4)
C38—O21—K1116.5 (11)O30—K1—O21176.1 (4)
C22—O21—K1109.8 (7)O33—K1—O21117.2 (4)
C23—C22—O21110.4 (13)O24—K1—O36116.9 (4)
C23—C22—H22A109.6O27—K1—O36176.5 (4)
O21—C22—H22A109.6O30—K1—O36118.8 (4)
C23—C22—H22B109.6O33—K1—O3659.4 (4)
O21—C22—H22B109.6O21—K1—O3658.4 (3)
H22A—C22—H22B108.1O24—K1—O10ii82.6 (3)
O24—C23—C22110.2 (13)O27—K1—O10ii70.4 (3)
C22—C23—K179.6 (9)O30—K1—O10ii93.8 (3)
O24—C23—H23A109.6O33—K1—O10ii106.7 (3)
C22—C23—H23A109.6O21—K1—O10ii89.9 (3)
K1—C23—H23A151.2O36—K1—O10ii113.1 (3)
O24—C23—H23B109.6O24—K1—Cl274.9 (2)
C22—C23—H23B109.6O27—K1—Cl290.0 (2)
K1—C23—H23B93.2O30—K1—Cl289.1 (2)
H23A—C23—H23B108.1O33—K1—Cl296.1 (2)
C23—O24—C25115.9 (14)O21—K1—Cl288.0 (2)
C23—O24—K1116.0 (9)O36—K1—Cl286.6 (3)
C25—O24—K1113.5 (10)O10ii—K1—Cl2155.23 (19)
C26—C25—O24112.3 (16)O24—K1—C2522.1 (4)
C26—C25—K179.1 (11)O27—K1—C2541.5 (5)
C26—C25—H25A109.1O30—K1—C25101.2 (5)
O24—C25—H25A109.1O33—K1—C25161.7 (5)
K1—C25—H25A151.0O21—K1—C2581.1 (4)
C26—C25—H25B109.1O36—K1—C25138.6 (5)
O24—C25—H25B109.1O10ii—K1—C2571.7 (4)
K1—C25—H25B94.7Cl2—K1—C2583.6 (4)
H25A—C25—H25B107.9O24—K1—C2320.8 (4)
C25—C26—O27111.0 (17)O27—K1—C2381.4 (4)
C25—C26—K177.9 (10)O30—K1—C23140.8 (5)
O27—C26—K146.8 (7)O33—K1—C23158.4 (5)
C25—C26—H26A109.4O21—K1—C2341.2 (4)
O27—C26—H26A109.4O36—K1—C2399.0 (4)
K1—C26—H26A154.5O10ii—K1—C2379.2 (3)
C25—C26—H26B109.4Cl2—K1—C2383.1 (3)
O27—C26—H26B109.4C25—K1—C2339.9 (5)
K1—C26—H26B91.4O24—K1—C2642.1 (5)
H26A—C26—H26B108.0O27—K1—C2622.1 (5)
C26—O27—C28115.1 (16)O30—K1—C2678.8 (5)
C26—O27—K1111.1 (9)O33—K1—C26139.1 (5)
C28—O27—K1113.7 (10)O21—K1—C26103.1 (5)
C29—C28—O27108.3 (15)O36—K1—C26156.4 (5)
C29—C28—H28A110.0O10ii—K1—C2678.8 (4)
O27—C28—H28A110.0Cl2—K1—C2677.7 (4)
C29—C28—H28B110.0C25—K1—C2623.1 (5)
O27—C28—H28B110.0C23—K1—C2662.0 (5)
N1—Pt1—Cl2—K1−113.6 (3)C31—O30—K1—O33−17.8 (13)
N11—Pt1—Cl2—K163.3 (3)C29—O30—K1—O36−161.1 (17)
Cl1—Pt1—N1—N959.4 (9)C31—O30—K1—O36−29.7 (14)
Cl2—Pt1—N1—N9−118.4 (9)C29—O30—K1—O10ii−42.1 (17)
Cl1—Pt1—N1—C2−116.4 (8)C31—O30—K1—O10ii89.3 (13)
Cl2—Pt1—N1—C265.8 (8)C29—O30—K1—Cl2113.3 (17)
N9—N1—C2—C71.6 (12)C31—O30—K1—Cl2−115.3 (13)
Pt1—N1—C2—C7178.0 (7)C29—O30—K1—C2530.0 (18)
N9—N1—C2—C3−176.5 (13)C31—O30—K1—C25161.4 (13)
Pt1—N1—C2—C3−0.1 (17)C29—O30—K1—C2335.5 (19)
C7—C2—C3—C41.4 (18)C31—O30—K1—C23166.9 (13)
N1—C2—C3—C4179.2 (12)C29—O30—K1—C2635.7 (17)
C2—C3—C4—C5−2.3 (19)C31—O30—K1—C26167.1 (14)
C3—C4—C5—C63(2)C32—O33—K1—O27−20.5 (16)
C4—C5—C6—C7−2.9 (18)C34—O33—K1—O27−152.6 (12)
C3—C2—C7—N8176.0 (10)C32—O33—K1—O30−12.3 (15)
N1—C2—C7—N8−2.4 (12)C34—O33—K1—O30−144.5 (13)
C3—C2—C7—C6−1.2 (17)C32—O33—K1—O21164.0 (15)
N1—C2—C7—C6−179.6 (10)C34—O33—K1—O2131.8 (13)
C5—C6—C7—N8−174.4 (12)C32—O33—K1—O36155.5 (16)
C5—C6—C7—C22.0 (17)C34—O33—K1—O3623.4 (12)
C2—C7—N8—O10−176.8 (10)C32—O33—K1—O10ii−97.2 (15)
C6—C7—N8—O100.1 (19)C34—O33—K1—O10ii130.7 (12)
C2—C7—N8—N92.5 (12)C32—O33—K1—Cl273.1 (16)
C6—C7—N8—N9179.4 (11)C34—O33—K1—Cl2−59.1 (12)
C2—N1—N9—N80.0 (12)C32—O33—K1—C25−15 (2)
Pt1—N1—N9—N8−176.3 (7)C34—O33—K1—C25−147.0 (17)
O10—N8—N9—N1177.7 (9)C32—O33—K1—C23159.7 (15)
C7—N8—N9—N1−1.6 (12)C34—O33—K1—C2327.5 (17)
N9—N8—O10—K1i147.6 (8)C32—O33—K1—C26−5.1 (18)
C7—N8—O10—K1i−33.1 (15)C34—O33—K1—C26−137.2 (13)
Cl1—Pt1—N11—N1965.1 (8)C38—O21—K1—O24145.4 (10)
Cl2—Pt1—N11—N19−117.1 (8)C22—O21—K1—O2417.7 (9)
Cl1—Pt1—N11—C12−121.8 (9)C38—O21—K1—O27160.4 (9)
Cl2—Pt1—N11—C1255.9 (9)C22—O21—K1—O2732.6 (10)
N19—N11—C12—C172.0 (12)C38—O21—K1—O33−24.2 (10)
Pt1—N11—C12—C17−171.5 (7)C22—O21—K1—O33−151.9 (9)
N19—N11—C12—C13−178.6 (11)C38—O21—K1—O36−15.6 (10)
Pt1—N11—C12—C137.9 (17)C22—O21—K1—O36−143.4 (10)
C17—C12—C13—C140.7 (15)C38—O21—K1—O10ii−133.0 (10)
N11—C12—C13—C14−178.6 (11)C22—O21—K1—O10ii99.2 (9)
C12—C13—C14—C150.3 (17)C38—O21—K1—Cl271.6 (9)
C13—C14—C15—C160(2)C22—O21—K1—Cl2−56.1 (9)
C14—C15—C16—C17−0.8 (18)C38—O21—K1—C25155.4 (10)
N11—C12—C17—C16177.6 (10)C22—O21—K1—C2527.7 (10)
C13—C12—C17—C16−1.9 (16)C38—O21—K1—C23153.4 (11)
N11—C12—C17—N18−1.2 (11)C22—O21—K1—C2325.6 (9)
C13—C12—C17—N18179.3 (9)C38—O21—K1—C26148.5 (10)
C15—C16—C17—C121.9 (17)C22—O21—K1—C2620.7 (10)
C15—C16—C17—N18−179.7 (12)C35—O36—K1—O24−179.6 (12)
C12—C17—N18—N190.0 (12)C37—O36—K1—O24−40.0 (13)
C16—C17—N18—N19−178.6 (11)C35—O36—K1—O3022.2 (14)
C12—C17—N18—O20178.1 (10)C37—O36—K1—O30161.8 (11)
C16—C17—N18—O20−1(2)C35—O36—K1—O3310.1 (12)
C12—N11—N19—N18−2.0 (11)C37—O36—K1—O33149.7 (13)
Pt1—N11—N19—N18172.4 (7)C35—O36—K1—O21−161.0 (14)
O20—N18—N19—N11−177.0 (9)C37—O36—K1—O21−21.4 (11)
C17—N18—N19—N111.2 (12)C35—O36—K1—O10ii−86.3 (13)
C38—O21—C22—C23179.7 (13)C37—O36—K1—O10ii53.3 (12)
K1—O21—C22—C23−49.7 (13)C35—O36—K1—Cl2109.3 (13)
O21—C22—C23—O2466.5 (15)C37—O36—K1—Cl2−111.2 (12)
O21—C22—C23—K135.5 (9)C35—O36—K1—C25−174.4 (13)
C22—C23—O24—C25175.4 (14)C37—O36—K1—C25−34.9 (15)
K1—C23—O24—C25−136.9 (14)C35—O36—K1—C23−168.3 (13)
C22—C23—O24—K1−47.7 (14)C37—O36—K1—C23−28.8 (12)
C23—O24—C25—C26−177.5 (16)C35—O36—K1—C26157.2 (15)
K1—O24—C25—C2645 (2)C37—O36—K1—C26−63.3 (18)
C23—O24—C25—K1137.9 (14)Pt1—Cl2—K1—O24−172.2 (3)
O24—C25—C26—O27−64 (2)Pt1—Cl2—K1—O27126.0 (3)
K1—C25—C26—O27−33.7 (13)Pt1—Cl2—K1—O3065.8 (4)
O24—C25—C26—K1−30.0 (14)Pt1—Cl2—K1—O335.6 (4)
C25—C26—O27—C28179.1 (16)Pt1—Cl2—K1—O21−111.6 (3)
K1—C26—O27—C28131.0 (14)Pt1—Cl2—K1—O36−53.2 (3)
C25—C26—O27—K148.1 (19)Pt1—Cl2—K1—O10ii162.9 (5)
C26—O27—C28—C29−173.2 (17)Pt1—Cl2—K1—C25167.1 (4)
K1—O27—C28—C29−43.5 (19)Pt1—Cl2—K1—C23−152.7 (4)
O27—C28—C29—O3066 (2)Pt1—Cl2—K1—C26144.5 (5)
C28—C29—O30—C31173.9 (14)C26—C25—K1—O24−139 (2)
C28—C29—O30—K1−55 (2)C26—C25—K1—O2723.8 (11)
C29—O30—C31—C32178.5 (17)O24—C25—K1—O27162.4 (17)
K1—O30—C31—C3246.2 (18)C26—C25—K1—O3014.2 (14)
O30—C31—C32—O33−59 (2)O24—C25—K1—O30152.8 (12)
C31—C32—O33—C34174.4 (17)C26—C25—K1—O3316 (2)
C31—C32—O33—K141 (2)O24—C25—K1—O33155.1 (10)
C32—O33—C34—C35170.2 (18)C26—C25—K1—O21−162.5 (14)
K1—O33—C34—C35−54 (2)O24—C25—K1—O21−23.9 (12)
O33—C34—C35—O3662 (2)C26—C25—K1—O36−150.9 (12)
C34—C35—O36—C37179.2 (17)O24—C25—K1—O36−12.4 (17)
C34—C35—O36—K1−40 (2)C26—C25—K1—O10ii104.6 (13)
C35—O36—C37—C38−165.3 (16)O24—C25—K1—O10ii−116.8 (13)
K1—O36—C37—C3853.0 (15)C26—C25—K1—Cl2−73.5 (13)
C22—O21—C38—C37176.1 (12)O24—C25—K1—Cl265.1 (12)
K1—O21—C38—C3749.1 (15)C26—C25—K1—C23−160.4 (17)
O36—C37—C38—O21−66.6 (17)O24—C25—K1—C23−21.8 (9)
C23—O24—K1—O27−150.9 (10)O24—C25—K1—C26139 (2)
C25—O24—K1—O27−13.0 (13)C22—C23—K1—O24135.1 (14)
C23—O24—K1—O30−169.2 (9)O24—C23—K1—O2726.0 (9)
C25—O24—K1—O30−31.3 (13)C22—C23—K1—O27161.1 (9)
C23—O24—K1—O2114.9 (9)O24—C23—K1—O3014.8 (12)
C25—O24—K1—O21152.8 (13)C22—C23—K1—O30149.9 (8)
C23—O24—K1—O3633.0 (10)O24—C23—K1—O33−154.2 (9)
C25—O24—K1—O36170.9 (13)C22—C23—K1—O33−19.0 (15)
C23—O24—K1—O10ii−79.1 (9)O24—C23—K1—O21−160.0 (11)
C25—O24—K1—O10ii58.7 (13)C22—C23—K1—O21−24.9 (8)
C23—O24—K1—Cl2111.1 (9)O24—C23—K1—O36−150.5 (9)
C25—O24—K1—Cl2−111.0 (13)C22—C23—K1—O36−15.4 (9)
C23—O24—K1—C25−137.9 (17)O24—C23—K1—O10ii97.5 (9)
C25—O24—K1—C23137.9 (17)C22—C23—K1—O10ii−127.4 (9)
C23—O24—K1—C26−160.6 (12)O24—C23—K1—Cl2−65.1 (9)
C25—O24—K1—C26−22.7 (13)C22—C23—K1—Cl270.0 (8)
C26—O27—K1—O24−17.5 (12)O24—C23—K1—C2523.2 (9)
C28—O27—K1—O24−149.2 (13)C22—C23—K1—C25158.3 (12)
C26—O27—K1—O30144.4 (13)O24—C23—K1—C2614.6 (9)
C28—O27—K1—O3012.6 (12)C22—C23—K1—C26149.7 (10)
C26—O27—K1—O33152.5 (12)C25—C26—K1—O2421.8 (11)
C28—O27—K1—O3320.8 (14)O27—C26—K1—O24156.5 (16)
C26—O27—K1—O21−32.2 (13)C25—C26—K1—O27−135 (2)
C28—O27—K1—O21−164.0 (12)C25—C26—K1—O30−165.8 (14)
C26—O27—K1—O10ii−109.1 (13)O27—C26—K1—O30−31.0 (12)
C28—O27—K1—O10ii119.2 (13)C25—C26—K1—O33−172.2 (11)
C26—O27—K1—Cl255.4 (13)O27—C26—K1—O33−37.5 (16)
C28—O27—K1—Cl2−76.3 (13)C25—C26—K1—O2117.8 (14)
C26—O27—K1—C25−24.8 (13)O27—C26—K1—O21152.5 (12)
C28—O27—K1—C25−156.6 (15)C25—C26—K1—O3653 (2)
C26—O27—K1—C23−27.5 (13)O27—C26—K1—O36−171.9 (9)
C28—O27—K1—C23−159.3 (13)C25—C26—K1—O10ii−69.5 (13)
C28—O27—K1—C26−131.8 (18)O27—C26—K1—O10ii65.2 (12)
C29—O30—K1—O2441.5 (18)C25—C26—K1—Cl2102.8 (13)
C31—O30—K1—O24172.9 (13)O27—C26—K1—Cl2−122.5 (13)
C29—O30—K1—O2722.7 (17)O27—C26—K1—C25135 (2)
C31—O30—K1—O27154.1 (14)C25—C26—K1—C2314.1 (12)
C29—O30—K1—O33−149.2 (18)O27—C26—K1—C23148.8 (14)

Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) x, −y+3/2, z−1/2.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O20—H20···O10iii0.841.762.466 (12)141

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

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT5255).

References

  • Anderson, G. W., Zimmerman, J. E. & Calahan, F. M. (1963). J. Am. Chem. Soc.85, 3039–3039.
  • Bosch, R., Jung, G. & Winter, W. (1983). Acta Cryst. C39, 1089–1092.
  • Bruker (2008). APEX2 andSAINT-Plus Bruker AXS Inc., Madison, Wisconsin, USA.
  • Sheldrick, G. M. (1999). TWINABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Spek, A. L. (2009). Acta Cryst. D65, 148–155. [PMC free article] [PubMed]

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