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Acta Crystallogr Sect E Struct Rep Online. Jul 1, 2008; 64(Pt 7): m898–m899.
Published online Jun 7, 2008. doi:  10.1107/S160053680801533X
PMCID: PMC2961811
Bis(1-{bis­[2-(diphenyl­phosphino­yl)eth­yl]phosphan­yl}-2-(diphenyl­phosphan­yl)ethane)dinitratoplatinum(II) methanol tetra­solvate
Timo Paul Rieckborn,a Emine Karakoc,a and Marc Heinrich Prosenca*
aInstitut für Anorganische und Angewandte Chemie, Department Chemie der Universität Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg, Germany
Correspondence e-mail: prosenc/at/chemie.uni-hamburg.de
Received May 2, 2008; Accepted May 21, 2008.
Abstract
In the title compound, [Pt(NO3)2(C42H42O2P4)2]·4CH3OH, the Pt atom positioned on a crystallographic centre of inversion. The two symmetry-equivalent nitrate anions are weakly coordinated to the PtII ion, creating, together with four P ligand atoms, a distorted octa­hedral coordination environment. In addition, several close C—H(...)O contacts between the nitrate O atoms and phenyl H atoms are found. Hydrogen bonds from two methanol solvent mol­ecules to one of the O—P groups complete the crystal structure.
Related literature
For related literature on PtII complexes, see: Brüggeller et al. (1992 [triangle]). For a structure of a related PtII nitrato complex, see: Fernandez et al. (2001 [triangle]).
An external file that holds a picture, illustration, etc.
Object name is e-64-0m898-scheme1.jpg Object name is e-64-0m898-scheme1.jpg
Crystal data
  • [Pt(NO3)2(C42H42O2P4)2]·4CH4O
  • M r = 1852.64
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m898-efi1.jpg
  • a = 9.9905 (9) Å
  • b = 14.3346 (13) Å
  • c = 16.9916 (15) Å
  • α = 66.200 (1)°
  • β = 77.479 (1)°
  • γ = 88.477 (1)°
  • V = 2168.4 (3) Å3
  • Z = 1
  • Mo Kα radiation
  • μ = 1.83 mm−1
  • T = 153 (2) K
  • 0.48 × 0.10 × 0.03 mm
Data collection
  • Bruker SMART APEX CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1995 [triangle]) T min = 0.474, T max = 0.947
  • 25181 measured reflections
  • 9347 independent reflections
  • 8160 reflections with I > 2σ(I)
  • R int = 0.052
Refinement
  • R[F 2 > 2σ(F 2)] = 0.039
  • wR(F 2) = 0.068
  • S = 0.91
  • 9347 reflections
  • 512 parameters
  • H-atom parameters constrained
  • Δρmax = 1.31 e Å−3
  • Δρmin = −1.37 e Å−3
Data collection: SMART (Bruker, 2000 [triangle]); cell refinement: SAINT (Bruker, 2000 [triangle]); data reduction: SAINT; 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.
Table 1
Table 1
Selected geometric parameters (Å, °)
Table 2
Table 2
Hydrogen-bond geometry (Å, °)
Supplementary Material
Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680801533X/si2089sup1.cif
Structure factors: contains datablocks I. DOI: 10.1107/S160053680801533X/si2089Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report
Acknowledgments
Financial support by the Deutsche Forschungsgemeinschaft (DFG) (grant No. PR 654/1–1) is gratefully acknowlegded. TPR thanks the Studienstiftung des deutschen Volkes for a fellowship.
supplementary crystallographic information
Comment
The title compound, [Pt(L)2]2+ (NO3-)2 (L = (P1,P1-bis(2-(diphenylphosphinoxid)ethyl)-P2,P2-diphenylethane -1,2-diphosphine), crystallizes as a packing of a discrete dication and two nitrate anions with the Pt-atom positioned on a centre of inversion. The two symmetry equivalent ligands molecules L are coordinated to the Pt-center by two phosphine donor atoms P1 and P2 with Pt—P distances (d(Pt—P1) = 2.3399 (9) Å, d(Pt—P2) = 2.3236 (9) Å) (Table 1) creating a square planar coordination environment in accord with previously reported PtII tetraphosphine complexes (Brüggeller et al., 1992). The two additional phosphor oxide groups of the ligands are not coordinated to the metal centre in the solid state. A long distance of d(Pt1—O4) = 3.524 (3) Å, angles of P1—Pt—O4 of 104.36 (5) ° and P2—Pt—O4 of 99.77 (5) ° are indicative of a weak Pt—NO3- interaction which is much weaker than a previously reported PtII—NO3- distance of 2.116 Å in a related complex (Fernandez et al., 2001). The nitrate anion is packed within a cavity created by the coordinated phosphine ligand atoms above and due to symmetry below the square plane spanned by the four phosphor ligand atoms creating a distorted octahedral coordination environment around the PtII ion. In addition several close C—H···O contacts between 2.30 and 2.70 Å were found between ortho-phenyl protons and methylene protons with nitrate oxygen atoms. Two methanol molecules with O—H···O hydrogen bonds to one of the O—P groups (Table 2) complete the crystal packing. The second P—O1 fragment exhibits weak hydrogen bond interactions with d(O1—H17A) of 2.997 Å and d(O1—H18A) of 2.991 Å to one of the adjacent phenyl group hydrogen atoms.
Experimental
All reactions were carried out under an atmosphere of dry nitrogen using standard Schlenk techniques. Solvents were dried and stored under nitrogen. Platinum(II)nitrate was purchased from ChemPur and Tris(2-(diphenylphosphino)ethyl)-phosphine was obtained from Acros Organics.
150 mg (0.47 mmol) Platinum(II)nitrate was dissolved in 50 ml water and 50 ml e thanol was added. 315 mg (0.47 mmol) Tris(2-(diphenylphosphino)ethyl)- phosphine (PP3) was dissolved in dichlormethane and added to the reaction mixture. The suspension was stirred at room temperature for 3 days. Afterwards the mixture was concentrated to small volume and a yellow solid precipitated. The precipitate was filtered and dried in vacuo. Single crystals were received by gas phase diffusion of diethyl ether into a solution of the yellow product in methanol.
Refinement
All non-hydrogen atoms were refined anisotropically and H atoms were refined using riding constraints with C—H distances set to 0.95 Å for aromatic, to 0.99 Å for aliphatic, 0.98 Å for methanol C—H bonds and 0.84 Å for O—H bonds. Uiso(H) values were set to 1.2 Ueq of the parent atom.
Figures
Fig. 1.
Fig. 1.
ORTEP representation of the PtII complex with displacement ellipsoids at 50% probability. H atoms and labels for symmetry equivalent C atoms have been omitted for clarity.
Crystal data
[Pt(NO3)2(C42H42O2P4)2]·4CH4OZ = 1
Mr = 1852.64F000 = 952
Triclinic, P1Dx = 1.419 Mg m3
Hall symbol: -P 1Mo Kα radiation λ = 0.71073 Å
a = 9.9905 (9) ÅCell parameters from 5288 reflections
b = 14.3346 (13) Åθ = 4.9–49.4º
c = 16.9916 (15) ŵ = 1.83 mm1
α = 66.200 (1)ºT = 153 (2) K
β = 77.479 (1)ºPlate, colourless
γ = 88.477 (1)º0.48 × 0.10 × 0.03 mm
V = 2168.4 (3) Å3
Data collection
Bruker SMART APEX CCD area-detector diffractometer8160 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.052
T = 153(2) Kθmax = 27.0º
[var phi] and ω scansθmin = 2.4º
Absorption correction: multi-scan(SADABS; Sheldrick, 1995)h = −12→12
Tmin = 0.474, Tmax = 0.947k = −18→18
25181 measured reflectionsl = −21→21
9347 independent reflections
Refinement
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.039H-atom parameters constrained
wR(F2) = 0.068  w = 1/[σ2(Fo2) + (0.0185P)2] where P = (Fo2 + 2Fc2)/3
S = 0.91(Δ/σ)max < 0.001
9347 reflectionsΔρmax = 1.31 e Å3
512 parametersΔρmin = −1.37 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Special details
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)
xyzUiso*/Ueq
Pt10.00000.00000.00000.01742 (6)
P10.18605 (9)0.10153 (7)−0.00768 (6)0.0217 (2)
P20.14224 (9)−0.01106 (7)−0.12330 (6)0.0210 (2)
P30.24812 (10)−0.28401 (7)−0.17502 (6)0.0255 (2)
P40.09161 (11)0.23615 (7)−0.36073 (6)0.0293 (2)
N1−0.3437 (4)0.2080 (3)−0.0989 (3)0.0416 (9)
O10.1078 (2)−0.29710 (18)−0.18776 (16)0.0335 (6)
O20.2424 (3)0.23539 (19)−0.39496 (16)0.0390 (7)
O3−0.3782 (3)0.2601 (3)−0.1679 (2)0.1131 (17)
O4−0.2262 (3)0.1769 (2)−0.10285 (19)0.0493 (8)
O5−0.4257 (3)0.1826 (2)−0.02587 (19)0.0424 (7)
C10.3381 (3)0.0626 (3)−0.0654 (2)0.0253 (8)
H1B0.41760.1115−0.08100.030*
H1C0.3608−0.0060−0.02690.030*
C20.3073 (3)0.0605 (3)−0.1490 (2)0.0266 (9)
H2B0.38170.0281−0.17570.032*
H2C0.30400.1313−0.19240.032*
C30.1821 (3)−0.1423 (2)−0.1047 (2)0.0237 (8)
H3A0.2208−0.1713−0.05150.028*
H3B0.0949−0.1825−0.09160.028*
C40.2830 (4)−0.1576 (2)−0.1808 (2)0.0271 (9)
H4A0.3787−0.1501−0.17600.032*
H4B0.2720−0.1051−0.23820.032*
C50.0837 (4)0.0428 (2)−0.2265 (2)0.0247 (8)
H5A0.15910.0444−0.27570.030*
H5B0.0058−0.0013−0.22270.030*
C60.0380 (4)0.1520 (3)−0.2456 (2)0.0287 (9)
H6A0.07740.1798−0.21020.034*
H6B−0.06340.1493−0.22720.034*
C70.1743 (4)0.2356 (2)−0.0763 (2)0.0220 (8)
C80.2892 (4)0.3042 (3)−0.1090 (2)0.0308 (9)
H8A0.37480.2814−0.09530.037*
C90.2781 (4)0.4063 (3)−0.1616 (3)0.0368 (10)
H9A0.35700.4529−0.18540.044*
C100.1528 (4)0.4404 (3)−0.1796 (2)0.0373 (10)
H10A0.14540.5106−0.21440.045*
C110.0388 (4)0.3729 (3)−0.1472 (2)0.0320 (9)
H11A−0.04710.3966−0.15960.038*
C120.0493 (4)0.2698 (3)−0.0964 (2)0.0240 (8)
H12A−0.02890.2230−0.07540.029*
C130.2253 (3)0.1005 (3)0.0925 (2)0.0233 (8)
C140.2972 (4)0.0223 (3)0.1429 (2)0.0299 (9)
H14A0.3304−0.02940.12360.036*
C150.3197 (4)0.0204 (3)0.2210 (2)0.0347 (10)
H15A0.3700−0.03220.25460.042*
C160.2702 (4)0.0938 (3)0.2509 (3)0.0396 (10)
H16A0.28470.09080.30530.048*
C170.1997 (4)0.1716 (3)0.2014 (3)0.0399 (11)
H17A0.16570.22230.22180.048*
C180.1783 (4)0.1762 (3)0.1220 (2)0.0308 (9)
H18A0.13170.23080.08750.037*
C190.2724 (4)−0.3735 (3)−0.0693 (2)0.0261 (9)
C200.1804 (4)−0.4595 (3)−0.0227 (2)0.0340 (10)
H20A0.1102−0.4700−0.04870.041*
C210.1888 (5)−0.5295 (3)0.0600 (3)0.0436 (11)
H21A0.1251−0.58750.09080.052*
C220.2916 (5)−0.5138 (3)0.0973 (3)0.0495 (12)
H22A0.2984−0.56180.15430.059*
C230.3843 (5)−0.4296 (3)0.0531 (3)0.0486 (12)
H23A0.4542−0.41990.07970.058*
C240.3753 (4)−0.3594 (3)−0.0300 (3)0.0369 (10)
H24A0.4392−0.3015−0.06050.044*
C250.3817 (4)−0.2982 (2)−0.2594 (2)0.0240 (8)
C260.3442 (4)−0.3123 (3)−0.3279 (2)0.0337 (10)
H26A0.2501−0.3134−0.33010.040*
C270.4446 (5)−0.3247 (3)−0.3938 (3)0.0440 (11)
H27A0.4181−0.3358−0.43990.053*
C280.5810 (5)−0.3209 (3)−0.3923 (3)0.0444 (11)
H28A0.6490−0.3287−0.43740.053*
C290.6188 (4)−0.3057 (3)−0.3250 (3)0.0452 (11)
H29A0.7132−0.3029−0.32390.054*
C300.5202 (4)−0.2944 (3)−0.2589 (3)0.0382 (10)
H30A0.5476−0.2840−0.21280.046*
C310.0423 (4)0.3607 (3)−0.3693 (2)0.0321 (9)
C320.1357 (5)0.4441 (3)−0.4216 (3)0.0454 (12)
H32A0.22270.4346−0.45240.054*
C330.1019 (6)0.5415 (3)−0.4287 (3)0.0630 (15)
H33A0.16590.5984−0.46440.076*
C34−0.0245 (7)0.5558 (4)−0.3839 (3)0.0664 (17)
H34A−0.04670.6224−0.38850.080*
C35−0.1177 (5)0.4744 (3)−0.3330 (3)0.0553 (14)
H35A−0.20490.4850−0.30320.066*
C36−0.0856 (4)0.3765 (3)−0.3245 (3)0.0426 (11)
H36A−0.15030.3202−0.28830.051*
C37−0.0041 (4)0.1944 (3)−0.4207 (2)0.0341 (10)
C38−0.1474 (5)0.1935 (3)−0.4052 (3)0.0441 (11)
H38A−0.19690.2136−0.36090.053*
C39−0.2181 (5)0.1636 (3)−0.4537 (3)0.0600 (14)
H39A−0.31550.1630−0.44240.072*
C40−0.1472 (7)0.1346 (4)−0.5184 (4)0.0686 (16)
H40A−0.19560.1146−0.55210.082*
C41−0.0054 (6)0.1346 (3)−0.5342 (3)0.0628 (15)
H41A0.04340.1146−0.57880.075*
C420.0663 (5)0.1637 (3)−0.4850 (3)0.0445 (11)
H42A0.16360.1625−0.49560.053*
C430.5176 (7)0.3611 (8)−0.3513 (5)0.189 (5)
H43A0.42980.3719−0.31810.283*
H43B0.58890.4101−0.35630.283*
H43C0.54310.2914−0.32040.283*
O60.5062 (8)0.3739 (8)−0.4264 (6)0.323 (5)
H6C0.43660.3392−0.42230.484*
O70.4255 (4)0.0828 (3)−0.3559 (2)0.0696 (10)
H7A0.37810.1338−0.36940.104*
C440.4311 (5)0.0373 (4)−0.4169 (3)0.0693 (15)
H44A0.4950−0.0172−0.40540.104*
H44B0.46290.0893−0.47720.104*
H44C0.33930.0086−0.41020.104*
Atomic displacement parameters (Å2)
U11U22U33U12U13U23
Pt10.01772 (11)0.01445 (11)0.02003 (12)0.00337 (8)−0.00161 (8)−0.00841 (9)
P10.0203 (5)0.0187 (5)0.0269 (5)0.0024 (4)−0.0040 (4)−0.0110 (4)
P20.0212 (5)0.0184 (5)0.0226 (5)0.0036 (4)−0.0014 (4)−0.0094 (4)
P30.0274 (6)0.0221 (5)0.0281 (6)0.0050 (4)−0.0037 (5)−0.0127 (5)
P40.0335 (6)0.0252 (6)0.0243 (6)0.0036 (5)−0.0035 (5)−0.0067 (5)
N10.024 (2)0.047 (2)0.050 (3)−0.0001 (18)−0.0083 (19)−0.016 (2)
O10.0253 (15)0.0367 (16)0.0403 (16)0.0043 (12)−0.0074 (13)−0.0177 (14)
O20.0328 (16)0.0393 (17)0.0355 (16)0.0016 (13)0.0025 (13)−0.0107 (14)
O30.044 (2)0.175 (4)0.052 (2)0.013 (2)−0.0171 (19)0.025 (3)
O40.0298 (17)0.055 (2)0.065 (2)0.0065 (15)−0.0073 (16)−0.0283 (17)
O50.0328 (17)0.0443 (18)0.0494 (19)0.0025 (14)−0.0046 (15)−0.0208 (16)
C10.020 (2)0.0203 (19)0.035 (2)0.0030 (16)−0.0052 (17)−0.0121 (18)
C20.022 (2)0.025 (2)0.032 (2)0.0009 (16)0.0017 (17)−0.0147 (18)
C30.028 (2)0.0185 (19)0.025 (2)0.0046 (16)−0.0039 (17)−0.0105 (17)
C40.029 (2)0.0198 (19)0.032 (2)0.0054 (16)−0.0019 (17)−0.0122 (18)
C50.028 (2)0.024 (2)0.021 (2)0.0027 (16)−0.0019 (16)−0.0094 (17)
C60.031 (2)0.029 (2)0.026 (2)0.0117 (18)−0.0061 (18)−0.0121 (18)
C70.025 (2)0.0199 (19)0.023 (2)0.0049 (16)−0.0024 (16)−0.0122 (16)
C80.028 (2)0.026 (2)0.037 (2)0.0015 (18)−0.0084 (19)−0.0120 (19)
C90.039 (3)0.024 (2)0.043 (3)−0.0067 (19)−0.007 (2)−0.010 (2)
C100.056 (3)0.019 (2)0.033 (2)0.007 (2)−0.012 (2)−0.0071 (19)
C110.034 (2)0.031 (2)0.035 (2)0.0125 (19)−0.0123 (19)−0.016 (2)
C120.023 (2)0.023 (2)0.025 (2)0.0022 (16)−0.0035 (16)−0.0107 (17)
C130.019 (2)0.025 (2)0.026 (2)−0.0022 (16)−0.0032 (16)−0.0118 (17)
C140.028 (2)0.027 (2)0.034 (2)0.0050 (17)−0.0048 (18)−0.0131 (19)
C150.029 (2)0.036 (2)0.034 (2)0.0038 (19)−0.0110 (19)−0.007 (2)
C160.046 (3)0.045 (3)0.033 (2)0.000 (2)−0.016 (2)−0.017 (2)
C170.053 (3)0.036 (2)0.042 (3)0.009 (2)−0.018 (2)−0.025 (2)
C180.035 (2)0.028 (2)0.033 (2)0.0032 (18)−0.0108 (19)−0.0142 (19)
C190.031 (2)0.022 (2)0.026 (2)0.0065 (17)−0.0008 (17)−0.0139 (18)
C200.040 (3)0.028 (2)0.033 (2)0.0030 (19)−0.002 (2)−0.015 (2)
C210.060 (3)0.024 (2)0.037 (3)0.005 (2)0.001 (2)−0.010 (2)
C220.068 (3)0.035 (3)0.037 (3)0.024 (2)−0.013 (3)−0.005 (2)
C230.053 (3)0.053 (3)0.046 (3)0.015 (3)−0.023 (2)−0.021 (3)
C240.039 (3)0.034 (2)0.038 (3)0.005 (2)−0.009 (2)−0.014 (2)
C250.030 (2)0.0147 (18)0.024 (2)0.0037 (16)−0.0013 (17)−0.0070 (16)
C260.038 (3)0.032 (2)0.032 (2)0.0015 (19)−0.007 (2)−0.014 (2)
C270.055 (3)0.051 (3)0.030 (2)0.000 (2)−0.004 (2)−0.022 (2)
C280.049 (3)0.045 (3)0.031 (3)0.004 (2)0.010 (2)−0.018 (2)
C290.034 (3)0.057 (3)0.042 (3)0.011 (2)0.000 (2)−0.022 (2)
C300.037 (3)0.047 (3)0.033 (2)0.008 (2)−0.004 (2)−0.021 (2)
C310.045 (3)0.025 (2)0.025 (2)0.0034 (19)−0.012 (2)−0.0065 (18)
C320.066 (3)0.033 (3)0.035 (3)−0.001 (2)−0.020 (2)−0.007 (2)
C330.109 (5)0.027 (3)0.048 (3)−0.006 (3)−0.032 (3)−0.002 (2)
C340.128 (5)0.028 (3)0.057 (4)0.026 (3)−0.049 (4)−0.017 (3)
C350.087 (4)0.042 (3)0.052 (3)0.034 (3)−0.037 (3)−0.025 (3)
C360.058 (3)0.030 (2)0.042 (3)0.014 (2)−0.021 (2)−0.013 (2)
C370.048 (3)0.022 (2)0.027 (2)0.0042 (19)−0.009 (2)−0.0047 (18)
C380.052 (3)0.037 (3)0.040 (3)0.000 (2)−0.014 (2)−0.010 (2)
C390.069 (4)0.046 (3)0.065 (4)−0.001 (3)−0.033 (3)−0.012 (3)
C400.099 (5)0.045 (3)0.066 (4)−0.010 (3)−0.046 (4)−0.012 (3)
C410.109 (5)0.042 (3)0.042 (3)0.002 (3)−0.023 (3)−0.019 (3)
C420.066 (3)0.031 (2)0.038 (3)0.004 (2)−0.016 (2)−0.013 (2)
C430.124 (7)0.398 (14)0.106 (6)−0.101 (8)0.031 (5)−0.185 (8)
O60.201 (7)0.614 (17)0.306 (11)0.094 (10)−0.050 (7)−0.350 (12)
O70.069 (3)0.088 (3)0.056 (2)0.026 (2)−0.0123 (19)−0.036 (2)
C440.095 (4)0.066 (4)0.050 (3)0.001 (3)−0.009 (3)−0.031 (3)
Geometric parameters (Å, °)
Pt1—P2i2.3235 (9)C17—H17A0.9500
Pt1—P22.3236 (9)C18—H18A0.9500
Pt1—P1i2.3399 (9)C19—C201.396 (5)
Pt1—P12.3399 (9)C19—C241.400 (5)
Pt1—O43.524 (3)C20—C211.377 (5)
P1—C71.818 (3)C20—H20A0.9500
P1—C131.823 (3)C21—C221.385 (6)
P1—C11.825 (3)C21—H21A0.9500
P2—C31.826 (3)C22—C231.380 (6)
P2—C51.828 (3)C22—H22A0.9500
P2—C21.838 (3)C23—C241.386 (5)
P3—O11.492 (2)C23—H23A0.9500
P3—C191.801 (4)C24—H24A0.9500
P3—C251.808 (3)C25—C261.384 (5)
P3—C41.814 (3)C25—C301.388 (5)
P4—O21.494 (3)C26—C271.399 (5)
P4—C311.796 (4)C26—H26A0.9500
P4—C61.801 (3)C27—C281.372 (5)
P4—C371.804 (4)C27—H27A0.9500
N1—O31.228 (4)C28—C291.373 (5)
N1—O41.242 (4)C28—H28A0.9500
N1—O51.247 (4)C29—C301.384 (5)
C1—C21.529 (4)C29—H29A0.9500
C1—H1B0.9900C30—H30A0.9500
C1—H1C0.9900C31—C321.390 (5)
C2—H2B0.9900C31—C361.403 (5)
C2—H2C0.9900C32—C331.390 (6)
C3—C41.545 (4)C32—H32A0.9500
C3—H3A0.9900C33—C341.382 (7)
C3—H3B0.9900C33—H33A0.9500
C4—H4A0.9900C34—C351.367 (6)
C4—H4B0.9900C34—H34A0.9500
C5—C61.543 (4)C35—C361.388 (5)
C5—H5A0.9900C35—H35A0.9500
C5—H5B0.9900C36—H36A0.9500
C6—H6A0.9900C37—C421.386 (5)
C6—H6B0.9900C37—C381.398 (5)
C7—C121.391 (4)C38—C391.384 (6)
C7—C81.391 (5)C38—H38A0.9500
C8—C91.390 (5)C39—C401.378 (7)
C8—H8A0.9500C39—H39A0.9500
C9—C101.383 (5)C40—C411.383 (7)
C9—H9A0.9500C40—H40A0.9500
C10—C111.376 (5)C41—C421.394 (6)
C10—H10A0.9500C41—H41A0.9500
C11—C121.393 (5)C42—H42A0.9500
C11—H11A0.9500C43—O61.244 (8)
C12—H12A0.9500C43—H43A0.9800
C13—C141.398 (5)C43—H43B0.9800
C13—C181.399 (5)C43—H43C0.9800
C14—C151.383 (5)O6—H6C0.8400
C14—H14A0.9500O7—C441.422 (5)
C15—C161.380 (5)O7—H7A0.8400
C15—H15A0.9500C44—H44A0.9800
C16—C171.381 (5)C44—H44B0.9800
C16—H16A0.9500C44—H44C0.9800
C17—C181.387 (5)
P2i—Pt1—P2180.0C16—C15—C14121.0 (4)
P2i—Pt1—P1i83.40 (3)C16—C15—H15A119.5
P2—Pt1—P1i96.60 (3)C14—C15—H15A119.5
P2i—Pt1—P196.60 (3)C15—C16—C17119.7 (4)
P2—Pt1—P183.40 (3)C15—C16—H16A120.2
P1i—Pt1—P1180.0C17—C16—H16A120.2
P2i—Pt1—O480.23 (5)C16—C17—C18120.3 (4)
P2—Pt1—O499.77 (5)C16—C17—H17A119.8
P1i—Pt1—O475.64 (5)C18—C17—H17A119.8
P1—Pt1—O4104.36 (5)C17—C18—C13120.2 (3)
C7—P1—C13104.93 (16)C17—C18—H18A119.9
C7—P1—C1105.46 (16)C13—C18—H18A119.9
C13—P1—C1107.00 (16)C20—C19—C24118.4 (3)
C7—P1—Pt1111.66 (12)C20—C19—P3118.1 (3)
C13—P1—Pt1120.67 (11)C24—C19—P3123.5 (3)
C1—P1—Pt1106.12 (11)C21—C20—C19121.7 (4)
C3—P2—C5106.78 (15)C21—C20—H20A119.2
C3—P2—C2106.38 (16)C19—C20—H20A119.2
C5—P2—C2104.19 (16)C20—C21—C22118.9 (4)
C3—P2—Pt1112.39 (11)C20—C21—H21A120.6
C5—P2—Pt1117.14 (11)C22—C21—H21A120.6
C2—P2—Pt1109.17 (11)C23—C22—C21121.0 (4)
O1—P3—C19112.39 (16)C23—C22—H22A119.5
O1—P3—C25112.26 (16)C21—C22—H22A119.5
C19—P3—C25107.85 (16)C22—C23—C24119.9 (4)
O1—P3—C4111.99 (16)C22—C23—H23A120.1
C19—P3—C4106.38 (16)C24—C23—H23A120.1
C25—P3—C4105.54 (16)C23—C24—C19120.2 (4)
O2—P4—C31112.08 (17)C23—C24—H24A119.9
O2—P4—C6111.78 (16)C19—C24—H24A119.9
C31—P4—C6106.10 (17)C26—C25—C30118.7 (3)
O2—P4—C37110.24 (17)C26—C25—P3118.5 (3)
C31—P4—C37108.83 (17)C30—C25—P3122.8 (3)
C6—P4—C37107.61 (17)C25—C26—C27120.2 (4)
O3—N1—O4118.8 (4)C25—C26—H26A119.9
O3—N1—O5121.3 (4)C27—C26—H26A119.9
O4—N1—O5119.8 (4)C28—C27—C26120.4 (4)
N1—O4—Pt1148.3 (3)C28—C27—H27A119.8
C2—C1—P1108.3 (2)C26—C27—H27A119.8
C2—C1—H1B110.0C27—C28—C29119.6 (4)
P1—C1—H1B110.0C27—C28—H28A120.2
C2—C1—H1C110.0C29—C28—H28A120.2
P1—C1—H1C110.0C28—C29—C30120.5 (4)
H1B—C1—H1C108.4C28—C29—H29A119.8
C1—C2—P2110.6 (2)C30—C29—H29A119.8
C1—C2—H2B109.5C29—C30—C25120.7 (4)
P2—C2—H2B109.5C29—C30—H30A119.7
C1—C2—H2C109.5C25—C30—H30A119.7
P2—C2—H2C109.5C32—C31—C36119.1 (4)
H2B—C2—H2C108.1C32—C31—P4118.4 (3)
C4—C3—P2116.6 (2)C36—C31—P4122.5 (3)
C4—C3—H3A108.1C31—C32—C33120.0 (5)
P2—C3—H3A108.1C31—C32—H32A120.0
C4—C3—H3B108.1C33—C32—H32A120.0
P2—C3—H3B108.1C34—C33—C32120.3 (5)
H3A—C3—H3B107.3C34—C33—H33A119.9
C3—C4—P3109.4 (2)C32—C33—H33A119.9
C3—C4—H4A109.8C35—C34—C33120.2 (5)
P3—C4—H4A109.8C35—C34—H34A119.9
C3—C4—H4B109.8C33—C34—H34A119.9
P3—C4—H4B109.8C34—C35—C36120.4 (5)
H4A—C4—H4B108.3C34—C35—H35A119.8
C6—C5—P2111.1 (2)C36—C35—H35A119.8
C6—C5—H5A109.4C35—C36—C31120.0 (4)
P2—C5—H5A109.4C35—C36—H36A120.0
C6—C5—H5B109.4C31—C36—H36A120.0
P2—C5—H5B109.4C42—C37—C38118.8 (4)
H5A—C5—H5B108.0C42—C37—P4119.2 (3)
C5—C6—P4112.2 (2)C38—C37—P4122.0 (3)
C5—C6—H6A109.2C39—C38—C37120.9 (4)
P4—C6—H6A109.2C39—C38—H38A119.6
C5—C6—H6B109.2C37—C38—H38A119.6
P4—C6—H6B109.2C40—C39—C38120.0 (5)
H6A—C6—H6B107.9C40—C39—H39A120.0
C12—C7—C8119.7 (3)C38—C39—H39A120.0
C12—C7—P1119.6 (3)C39—C40—C41119.8 (5)
C8—C7—P1120.7 (3)C39—C40—H40A120.1
C9—C8—C7119.7 (3)C41—C40—H40A120.1
C9—C8—H8A120.1C40—C41—C42120.5 (5)
C7—C8—H8A120.1C40—C41—H41A119.8
C10—C9—C8120.3 (4)C42—C41—H41A119.8
C10—C9—H9A119.8C37—C42—C41120.1 (4)
C8—C9—H9A119.8C37—C42—H42A120.0
C11—C10—C9120.2 (4)C41—C42—H42A120.0
C11—C10—H10A119.9O6—C43—H43A109.5
C9—C10—H10A119.9O6—C43—H43B109.5
C10—C11—C12120.1 (3)H43A—C43—H43B109.5
C10—C11—H11A119.9O6—C43—H43C109.5
C12—C11—H11A119.9H43A—C43—H43C109.5
C7—C12—C11119.9 (3)H43B—C43—H43C109.5
C7—C12—H12A120.0C43—O6—H6C109.5
C11—C12—H12A120.0C44—O7—H7A109.5
C14—C13—C18119.1 (3)O7—C44—H44A109.5
C14—C13—P1120.8 (3)O7—C44—H44B109.5
C18—C13—P1120.0 (3)H44A—C44—H44B109.5
C15—C14—C13119.7 (3)O7—C44—H44C109.5
C15—C14—H14A120.1H44A—C44—H44C109.5
C13—C14—H14A120.1H44B—C44—H44C109.5
Symmetry codes: (i) −x, −y, −z.
Hydrogen-bond geometry (Å, °)
D—H···AD—HH···AD···AD—H···A
O6—H6C···O20.842.323.160 (9)174
O7—H7A···O20.841.952.777 (4)170
C12—H12A···O40.952.293.132 (4)147
C6—H6B···O40.992.533.294 (4)134
C1—H1B···O5ii0.992.423.289 (5)146
C1—H1C···O5iii0.992.443.399 (5)162
C8—H8A···O3ii0.952.583.376 (5)142
C14—H14A···O4iii0.952.563.317 (5)137
C27—H27A···O6iv0.952.503.338 (11)147
C28—H28A···O2iv0.952.603.385 (5)141
Symmetry codes: (ii) x+1, y, z; (iii) −x, −y, −z; (iv) −x+1, −y, −z−1.
Footnotes
Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SI2089).
References
  • Brüggeller, P., Nar, H. & Messerschmidt, A. (1992). Acta Cryst. C48, 817–821.
  • Bruker (2000). SMART and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  • Fernandez, D., Sevillano, P., Garcia-Seijo, M. S., Castineiras, A., Janosi, L., Berente, Z., Kollar, L. & Garcia-Fernandez, M. E. (2001). Inorg. Chim. Acta, 312, 40–52.
  • Sheldrick, G. M. (1995). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
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