metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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catena-Poly[[(18-crown-6-κ6O)potassium]-μ-chlorido-[(1H-benzotriazol-1-ol-κN3)chloridoplatinum(II)]-μ-(benzotriazol-1-olato-κ2N3:O)]

aDepartment of Chemistry, Popes College, Sawyerpuram 628 251, India, bDepartment of Physics, Sethupathy Government Arts College, Ramanathapuram 623 502, Tamilnadu, India, cDepartment of Chemistry, Sarah Tucker College, Tirunelveli 627 007, Tamilnadu, India, dDepartment of Chemistry, T.D.M.N.S. College, T. Kallikulam, Tamilnadu, India, and eInstitut für Organische Chemie, Universität Mainz, Duesbergweg 10-14, 55099 Mainz, Germany
*Correspondence e-mail: b_ravidurai@yahoo.com

(Received 25 April 2010; accepted 29 April 2010; online 8 May 2010)

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[Anderson, G. W., Zimmerman, J. E. & Calahan, F. M. (1963). J. Am. Chem. Soc. 85, 3039-3039.]). For related structures, see Bosch et al. (1983[Bosch, R., Jung, G. & Winter, W. (1983). Acta Cryst. C39, 1089-1092.]).

[Scheme 1]

Experimental

Crystal data
  • [KPt(C6H4N3O)Cl2(C6H5N3O)(C12H24O6)]

  • Mr = 838.65

  • Monoclinic, P 21 /c

  • 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[Sheldrick, G. M. (1999). TWINABS. University of Göttingen, Germany.]) Tmin = 0.494, Tmax = 0.746

  • 10775 measured reflections

  • 10775 independent reflections

  • 9006 reflections with I > 2σ(I)

Refinement
  • R[F2 > 2σ(F2)] = 0.063

  • wR(F2) = 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

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O20—H20⋯O10i 0.84 1.76 2.466 (12) 141
Symmetry code: (i) [x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}].

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2008[Bruker (2008). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]).

Supporting information


Comment top

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.

Related literature top

For related literature [on what subject?], see Anderson et al. (1963). For related structures, see Bosch et al. (1983).

Experimental top

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 top

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).

Structure description top

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.

For related literature [on what subject?], see Anderson et al. (1963). For related structures, see Bosch et al. (1983).

Computing details top

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

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound, showing 50% probability displacement ellipsoids and the atom numbering scheme.
catena-Poly[[(18-crown-6-κ6O)potassium]-µ-chlorido- [(1H-benzotriazol-1-ol-κN3)chloridoplatinum(II)]- µ-(benzotriazol-1-olato-κ2N3:O)] top
Crystal data top
[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 top
Bruker SMART CCD
diffractometer
10775 independent reflections
Radiation source: sealed Tube9006 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.000
CCD scanθmax = 28.0°, θmin = 1.5°
Absorption correction: multi-scan
(TWINABS; Sheldrick, 1999)
h = 1818
Tmin = 0.494, Tmax = 0.746k = 014
10775 measured reflectionsl = 026
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)] = 0.063Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.178H-atom parameters constrained
S = 1.07 w = 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
Crystal data top
[KPt(C6H4N3O)Cl2(C6H5N3O)(C12H24O6)]V = 3105.2 (5) Å3
Mr = 838.65Z = 4
Monoclinic, P21/cMo Kα radiation
a = 14.2727 (13) ŵ = 4.88 mm1
b = 10.9821 (10) ÅT = 173 K
c = 20.0716 (18) Å0.17 × 0.10 × 0.08 mm
β = 99.249 (3)°
Data collection top
Bruker SMART CCD
diffractometer
10775 independent reflections
Absorption correction: multi-scan
(TWINABS; Sheldrick, 1999)
9006 reflections with I > 2σ(I)
Tmin = 0.494, Tmax = 0.746Rint = 0.000
10775 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0630 restraints
wR(F2) = 0.178H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0972P)2 + 18.2058P]
where P = (Fo2 + 2Fc2)/3
10775 reflectionsΔρmax = 1.77 e Å3
382 parametersΔρmin = 1.78 e Å3
Special details top

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) top
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)
H40.01000.72930.51560.051*
C50.0348 (10)0.7488 (11)0.6216 (7)0.039 (3)
H50.01130.80790.62840.047*
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)
H31A0.05300.74860.37870.108*
H31B0.01000.79180.31370.108*
C320.0092 (14)0.613 (3)0.3341 (10)0.092 (8)
H32A0.01740.56020.37460.111*
H32B0.05040.58860.30480.111*
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) top
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, º) top
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—K1113.6 (3)C31—O30—K1—O3317.8 (13)
N11—Pt1—Cl2—K163.3 (3)C29—O30—K1—O36161.1 (17)
Cl1—Pt1—N1—N959.4 (9)C31—O30—K1—O3629.7 (14)
Cl2—Pt1—N1—N9118.4 (9)C29—O30—K1—O10ii42.1 (17)
Cl1—Pt1—N1—C2116.4 (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—Cl2115.3 (13)
Pt1—N1—C2—C7178.0 (7)C29—O30—K1—C2530.0 (18)
N9—N1—C2—C3176.5 (13)C31—O30—K1—C25161.4 (13)
Pt1—N1—C2—C30.1 (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—C52.3 (19)C31—O30—K1—C26167.1 (14)
C3—C4—C5—C63 (2)C32—O33—K1—O2720.5 (16)
C4—C5—C6—C72.9 (18)C34—O33—K1—O27152.6 (12)
C3—C2—C7—N8176.0 (10)C32—O33—K1—O3012.3 (15)
N1—C2—C7—N82.4 (12)C34—O33—K1—O30144.5 (13)
C3—C2—C7—C61.2 (17)C32—O33—K1—O21164.0 (15)
N1—C2—C7—C6179.6 (10)C34—O33—K1—O2131.8 (13)
C5—C6—C7—N8174.4 (12)C32—O33—K1—O36155.5 (16)
C5—C6—C7—C22.0 (17)C34—O33—K1—O3623.4 (12)
C2—C7—N8—O10176.8 (10)C32—O33—K1—O10ii97.2 (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—Cl259.1 (12)
C2—N1—N9—N80.0 (12)C32—O33—K1—C2515 (2)
Pt1—N1—N9—N8176.3 (7)C34—O33—K1—C25147.0 (17)
O10—N8—N9—N1177.7 (9)C32—O33—K1—C23159.7 (15)
C7—N8—N9—N11.6 (12)C34—O33—K1—C2327.5 (17)
N9—N8—O10—K1i147.6 (8)C32—O33—K1—C265.1 (18)
C7—N8—O10—K1i33.1 (15)C34—O33—K1—C26137.2 (13)
Cl1—Pt1—N11—N1965.1 (8)C38—O21—K1—O24145.4 (10)
Cl2—Pt1—N11—N19117.1 (8)C22—O21—K1—O2417.7 (9)
Cl1—Pt1—N11—C12121.8 (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—O3324.2 (10)
Pt1—N11—C12—C17171.5 (7)C22—O21—K1—O33151.9 (9)
N19—N11—C12—C13178.6 (11)C38—O21—K1—O3615.6 (10)
Pt1—N11—C12—C137.9 (17)C22—O21—K1—O36143.4 (10)
C17—C12—C13—C140.7 (15)C38—O21—K1—O10ii133.0 (10)
N11—C12—C13—C14178.6 (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—Cl256.1 (9)
C14—C15—C16—C170.8 (18)C38—O21—K1—C25155.4 (10)
N11—C12—C17—C16177.6 (10)C22—O21—K1—C2527.7 (10)
C13—C12—C17—C161.9 (16)C38—O21—K1—C23153.4 (11)
N11—C12—C17—N181.2 (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—N18179.7 (12)C35—O36—K1—O24179.6 (12)
C12—C17—N18—N190.0 (12)C37—O36—K1—O2440.0 (13)
C16—C17—N18—N19178.6 (11)C35—O36—K1—O3022.2 (14)
C12—C17—N18—O20178.1 (10)C37—O36—K1—O30161.8 (11)
C16—C17—N18—O201 (2)C35—O36—K1—O3310.1 (12)
C12—N11—N19—N182.0 (11)C37—O36—K1—O33149.7 (13)
Pt1—N11—N19—N18172.4 (7)C35—O36—K1—O21161.0 (14)
O20—N18—N19—N11177.0 (9)C37—O36—K1—O2121.4 (11)
C17—N18—N19—N111.2 (12)C35—O36—K1—O10ii86.3 (13)
C38—O21—C22—C23179.7 (13)C37—O36—K1—O10ii53.3 (12)
K1—O21—C22—C2349.7 (13)C35—O36—K1—Cl2109.3 (13)
O21—C22—C23—O2466.5 (15)C37—O36—K1—Cl2111.2 (12)
O21—C22—C23—K135.5 (9)C35—O36—K1—C25174.4 (13)
C22—C23—O24—C25175.4 (14)C37—O36—K1—C2534.9 (15)
K1—C23—O24—C25136.9 (14)C35—O36—K1—C23168.3 (13)
C22—C23—O24—K147.7 (14)C37—O36—K1—C2328.8 (12)
C23—O24—C25—C26177.5 (16)C35—O36—K1—C26157.2 (15)
K1—O24—C25—C2645 (2)C37—O36—K1—C2663.3 (18)
C23—O24—C25—K1137.9 (14)Pt1—Cl2—K1—O24172.2 (3)
O24—C25—C26—O2764 (2)Pt1—Cl2—K1—O27126.0 (3)
K1—C25—C26—O2733.7 (13)Pt1—Cl2—K1—O3065.8 (4)
O24—C25—C26—K130.0 (14)Pt1—Cl2—K1—O335.6 (4)
C25—C26—O27—C28179.1 (16)Pt1—Cl2—K1—O21111.6 (3)
K1—C26—O27—C28131.0 (14)Pt1—Cl2—K1—O3653.2 (3)
C25—C26—O27—K148.1 (19)Pt1—Cl2—K1—O10ii162.9 (5)
C26—O27—C28—C29173.2 (17)Pt1—Cl2—K1—C25167.1 (4)
K1—O27—C28—C2943.5 (19)Pt1—Cl2—K1—C23152.7 (4)
O27—C28—C29—O3066 (2)Pt1—Cl2—K1—C26144.5 (5)
C28—C29—O30—C31173.9 (14)C26—C25—K1—O24139 (2)
C28—C29—O30—K155 (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—O3359 (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—O21162.5 (14)
K1—O33—C34—C3554 (2)O24—C25—K1—O2123.9 (12)
O33—C34—C35—O3662 (2)C26—C25—K1—O36150.9 (12)
C34—C35—O36—C37179.2 (17)O24—C25—K1—O3612.4 (17)
C34—C35—O36—K140 (2)C26—C25—K1—O10ii104.6 (13)
C35—O36—C37—C38165.3 (16)O24—C25—K1—O10ii116.8 (13)
K1—O36—C37—C3853.0 (15)C26—C25—K1—Cl273.5 (13)
C22—O21—C38—C37176.1 (12)O24—C25—K1—Cl265.1 (12)
K1—O21—C38—C3749.1 (15)C26—C25—K1—C23160.4 (17)
O36—C37—C38—O2166.6 (17)O24—C25—K1—C2321.8 (9)
C23—O24—K1—O27150.9 (10)O24—C25—K1—C26139 (2)
C25—O24—K1—O2713.0 (13)C22—C23—K1—O24135.1 (14)
C23—O24—K1—O30169.2 (9)O24—C23—K1—O2726.0 (9)
C25—O24—K1—O3031.3 (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—O33154.2 (9)
C25—O24—K1—O36170.9 (13)C22—C23—K1—O3319.0 (15)
C23—O24—K1—O10ii79.1 (9)O24—C23—K1—O21160.0 (11)
C25—O24—K1—O10ii58.7 (13)C22—C23—K1—O2124.9 (8)
C23—O24—K1—Cl2111.1 (9)O24—C23—K1—O36150.5 (9)
C25—O24—K1—Cl2111.0 (13)C22—C23—K1—O3615.4 (9)
C23—O24—K1—C25137.9 (17)O24—C23—K1—O10ii97.5 (9)
C25—O24—K1—C23137.9 (17)C22—C23—K1—O10ii127.4 (9)
C23—O24—K1—C26160.6 (12)O24—C23—K1—Cl265.1 (9)
C25—O24—K1—C2622.7 (13)C22—C23—K1—Cl270.0 (8)
C26—O27—K1—O2417.5 (12)O24—C23—K1—C2523.2 (9)
C28—O27—K1—O24149.2 (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—O2132.2 (13)C25—C26—K1—O27135 (2)
C28—O27—K1—O21164.0 (12)C25—C26—K1—O30165.8 (14)
C26—O27—K1—O10ii109.1 (13)O27—C26—K1—O3031.0 (12)
C28—O27—K1—O10ii119.2 (13)C25—C26—K1—O33172.2 (11)
C26—O27—K1—Cl255.4 (13)O27—C26—K1—O3337.5 (16)
C28—O27—K1—Cl276.3 (13)C25—C26—K1—O2117.8 (14)
C26—O27—K1—C2524.8 (13)O27—C26—K1—O21152.5 (12)
C28—O27—K1—C25156.6 (15)C25—C26—K1—O3653 (2)
C26—O27—K1—C2327.5 (13)O27—C26—K1—O36171.9 (9)
C28—O27—K1—C23159.3 (13)C25—C26—K1—O10ii69.5 (13)
C28—O27—K1—C26131.8 (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—Cl2122.5 (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—O33149.2 (18)O27—C26—K1—C23148.8 (14)
Symmetry codes: (i) x, y+3/2, z+1/2; (ii) x, y+3/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O20—H20···O10iii0.841.762.466 (12)141
Symmetry code: (iii) x, y+1/2, z1/2.

Experimental details

Crystal data
Chemical formula[KPt(C6H4N3O)Cl2(C6H5N3O)(C12H24O6)]
Mr838.65
Crystal system, space groupMonoclinic, P21/c
Temperature (K)173
a, b, c (Å)14.2727 (13), 10.9821 (10), 20.0716 (18)
β (°) 99.249 (3)
V3)3105.2 (5)
Z4
Radiation typeMo Kα
µ (mm1)4.88
Crystal size (mm)0.17 × 0.10 × 0.08
Data collection
DiffractometerBruker SMART CCD
Absorption correctionMulti-scan
(TWINABS; Sheldrick, 1999)
Tmin, Tmax0.494, 0.746
No. of measured, independent and
observed [I > 2σ(I)] reflections
10775, 10775, 9006
Rint0.000
(sin θ/λ)max1)0.661
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.063, 0.178, 1.07
No. of reflections10775
No. of parameters382
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0972P)2 + 18.2058P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.77, 1.78

Computer programs: APEX2 (Bruker, 2008), SAINT-Plus (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O20—H20···O10i0.841.762.466 (12)140.8
Symmetry code: (i) x, y+1/2, z1/2.
 

References

First citationAnderson, G. W., Zimmerman, J. E. & Calahan, F. M. (1963). J. Am. Chem. Soc. 85, 3039–3039.  CrossRef CAS Web of Science Google Scholar
First citationBosch, R., Jung, G. & Winter, W. (1983). Acta Cryst. C39, 1089–1092.  CSD CrossRef CAS Web of Science IUCr Journals Google Scholar
First citationBruker (2008). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationSheldrick, G. M. (1999). TWINABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationSpek, A. L. (2009). Acta Cryst. D65, 148–155.  Web of Science CrossRef CAS IUCr Journals Google Scholar

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