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In the title compound, [PtCl2(C25H30N2OP2)]·CHCl3, the urea ligand is P,P′-coordinated, leading to square-planar geometry at the Pt atom [bond lengths Pt—P 2.2102 (19) Å to the Ph2P moiety and 2.2275 (18) Å to tBu(Ph)P; Pt—Cl 2.3658 (16) and 2.3658 (18) Å]. The ligand bite angle is 89.41 (7)°. The chloro­form mol­ecule is associated with the metal complex via a hydrogen-bond system of the form C—H(...Cl)2.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802014083/bt6178sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802014083/bt6178Isup2.hkl
Contains datablock I

CCDC reference: 197446

Key indicators

  • Single-crystal X-ray study
  • T = 178 K
  • Mean [sigma](C-C) = 0.010 Å
  • R factor = 0.034
  • wR factor = 0.087
  • Data-to-parameter ratio = 16.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
ABSTM_02 Alert B The ratio of expected to reported Tmax/Tmin(RR) is > 1.50 Tmin and Tmax reported: 0.506 0.999 Tmin and Tmax expected: 0.150 0.465 RR = 1.569 Please check that your absorption correction is appropriate. General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.465 Tmax scaled 0.465 Tmin scaled 0.235
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
0 Alert Level C = Please check

Comment top

The title compound, (I), formed part of a study of phosphorus-substituted N,N'-diorganylureas (Vogt, 1992). It crystallizes as a chloroform monosolvate.

The formula unit is shown in Fig. 1. The structure determination confirms the expected P,P'-bonding mode of the ligand; related derivatives of pentacarbonylchromium and -molybdenum unexpectedly proved to be P,O-bonded (Vogt et al., 1991). The geometry at platinum is square planar; the Pt—Cl bond lengths are exactly equal, but the Pt—P bond to the Ph2P moiety is slightly shorter than that to tBu(Ph)P (Table 1). The P—N bond lengths display a similar qualitative difference, perhaps because of steric effects from the bulky tert-butyl group. The ligand bite angle is 89.41 (7)°. The chelate ring is not planar; torsion angles are given in Table 1.

The preparation and structures of several closely related compounds have recently been reported by Slawin et al. (2001). The dichloroplatinum complexes of [Ph2PN(R)C(O)N(R)PPh2] (R = Me, Et) display bond lengths and angles similar to those of the title compound.

The solvent molecule is associated with the metal complex by a three-centre hydrogen bond of the form C—H(···Cl)2 (Table 2). The role of metal-bonded chlorine as a hydrogen-bond acceptor is well established for both `classical' (Aullón et al., 1998) and `weak' (Freytag & Jones, 2000) hydrogen bonds.

Experimental top

The title compound was prepared by treating (cyclooctadiene)PtCl2 with the phosphinourea ligand in dichloromethane (Vogt, 1992). Single crystals were obtained by evaporation from chloroform.

Refinement top

Methyl H atoms were identified in difference syntheses, idealized and then refined allowing rigid methyl groups to rotate but not tip. The maxima at C1 and C3 were indistinct, which may indicate disorder or appreciable rotation of these methyl groups. Other H atoms were included using a riding model with fixed C—H bond lengths (aromatic 0.95, methyl 0.98 and methine 1.00 Å); Uiso(H) values were fixed at 1.2 times the Ueq of the parent atom. Three significant difference peaks (the largest 2.4 e Å−3) do not lie near the Pt atom. They may be caused by a minor but unidentified twinning or disorder component.

Computing details top

Data collection: P3 (Nicolet, 1987); cell refinement: P3; data reduction: XDISK (Nicolet, 1987); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1994); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The formula unit of the title compound in the crystal. Ellipsoids represent 30% probability levels. H-atom radii are arbitrary.
{N-[tert-Butyl(phenyl)phosphino]-N'-diphenylphosphino-N,N'-dimethylurea- P,P'}dichloroplatinum(II) chloroform solvate top
Crystal data top
[PtCl2(C25H30N2OP2)]·CHCl3Dx = 1.769 Mg m3
Mr = 821.81Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PbcaCell parameters from 50 reflections
a = 16.380 (4) Åθ = 10–11.5°
b = 15.653 (3) ŵ = 5.11 mm1
c = 24.074 (4) ÅT = 178 K
V = 6172 (2) Å3Tablet, colourless
Z = 80.40 × 0.40 × 0.15 mm
F(000) = 3216
Data collection top
Nicolet R3
diffractometer
3612 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.043
Graphite monochromatorθmax = 25.0°, θmin = 3.0°
ω scansh = 019
Absorption correction: ψ scan
(XEMP; Nicolet, 1987)
k = 1818
Tmin = 0.506, Tmax = 0.999l = 280
10607 measured reflections3 standard reflections every 147 reflections
5419 independent reflections intensity decay: 2%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.087H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0367P)2 + 1.8493P]
where P = (Fo2 + 2Fc2)/3
5419 reflections(Δ/σ)max = 0.006
339 parametersΔρmax = 2.40 e Å3
66 restraintsΔρmin = 0.85 e Å3
Crystal data top
[PtCl2(C25H30N2OP2)]·CHCl3V = 6172 (2) Å3
Mr = 821.81Z = 8
Orthorhombic, PbcaMo Kα radiation
a = 16.380 (4) ŵ = 5.11 mm1
b = 15.653 (3) ÅT = 178 K
c = 24.074 (4) Å0.40 × 0.40 × 0.15 mm
Data collection top
Nicolet R3
diffractometer
3612 reflections with I > 2σ(I)
Absorption correction: ψ scan
(XEMP; Nicolet, 1987)
Rint = 0.043
Tmin = 0.506, Tmax = 0.9993 standard reflections every 147 reflections
10607 measured reflections intensity decay: 2%
5419 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03466 restraints
wR(F2) = 0.087H-atom parameters constrained
S = 1.05Δρmax = 2.40 e Å3
5419 reflectionsΔρmin = 0.85 e Å3
339 parameters
Special details top

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.

Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

8.9801 (0.0074) x + 13.0701 (0.0055) y − 1.1370 (0.0129) z = 14.0493 (0.0084)

* 0.0582 (0.0007) Pt * −0.0059 (0.0009) P1 * −0.0241 (0.0009) P2 * −0.0223 (0.0009) Cl1 * −0.0058 (0.0008) Cl2 − 0.4900 (0.0056) N1 0.7146 (0.0056) N2 0.2307 (0.0072) C2

Rms deviation of fitted atoms = 0.0301

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pt0.669917 (14)0.666824 (15)0.548759 (10)0.01825 (9)
Cl10.62226 (10)0.68541 (11)0.45678 (7)0.0290 (4)
Cl20.77862 (10)0.58411 (10)0.51279 (7)0.0256 (4)
P10.56220 (10)0.73869 (11)0.58049 (8)0.0212 (4)
P20.70803 (11)0.64188 (11)0.63532 (8)0.0230 (4)
N10.5441 (3)0.7202 (3)0.6507 (2)0.0237 (13)
N20.6817 (3)0.7205 (3)0.6814 (2)0.0221 (13)
O0.5785 (3)0.7715 (4)0.7358 (2)0.0464 (15)
C10.4587 (4)0.7166 (5)0.6719 (3)0.0352 (19)
H1A0.45830.69050.70890.053*
H1B0.42510.68240.64660.053*
H1C0.43640.77470.67420.053*
C20.6007 (4)0.7401 (4)0.6923 (3)0.0297 (17)
C30.7404 (5)0.7576 (5)0.7215 (3)0.044 (2)
H3A0.72350.81580.73100.066*
H3B0.79500.75900.70480.066*
H3C0.74160.72250.75520.066*
C40.5692 (4)0.8575 (4)0.5721 (3)0.0273 (16)
C50.6539 (4)0.8832 (4)0.5935 (3)0.0309 (17)
H5A0.69550.84680.57630.037*
H5B0.65580.87620.63400.037*
H5C0.66460.94310.58400.037*
C60.5630 (5)0.8818 (5)0.5099 (3)0.0369 (18)
H6A0.56570.94410.50610.044*
H6B0.51110.86100.49480.044*
H6C0.60840.85570.48950.044*
C70.5040 (5)0.9046 (4)0.6061 (3)0.040 (2)
H7A0.51190.96640.60230.048*
H7B0.50880.88850.64530.048*
H7C0.44970.88910.59230.048*
C80.4704 (4)0.6931 (4)0.5506 (3)0.0219 (14)
C90.4007 (4)0.7401 (4)0.5366 (3)0.0302 (17)
H90.40070.80070.53870.036*
C100.3315 (4)0.6961 (4)0.5197 (3)0.0329 (17)
H100.28380.72720.51010.039*
C110.3304 (4)0.6074 (4)0.5166 (3)0.0310 (16)
H110.28230.57840.50510.037*
C120.3999 (4)0.5615 (4)0.5305 (3)0.0297 (17)
H120.39980.50090.52820.036*
C130.4692 (4)0.6042 (4)0.5475 (3)0.0260 (15)
H130.51660.57270.55730.031*
C140.6586 (4)0.5461 (4)0.6610 (3)0.0246 (15)
C150.6352 (4)0.4837 (4)0.6236 (3)0.0294 (16)
H150.64850.49010.58540.035*
C160.5927 (4)0.4117 (4)0.6410 (4)0.0411 (19)
H160.57710.36920.61490.049*
C170.5733 (5)0.4025 (5)0.6963 (3)0.042 (2)
H170.54290.35430.70840.051*
C180.5980 (4)0.4633 (5)0.7343 (3)0.0376 (18)
H180.58640.45540.77260.045*
C190.6392 (4)0.5353 (5)0.7171 (3)0.0337 (17)
H190.65450.57760.74350.040*
C200.8164 (4)0.6314 (4)0.6475 (3)0.0251 (15)
C210.8704 (4)0.6822 (4)0.6173 (3)0.0292 (16)
H210.85070.71880.58890.035*
C220.9532 (4)0.6787 (5)0.6292 (3)0.0347 (18)
H220.99060.71190.60810.042*
C230.9817 (5)0.6274 (5)0.6716 (3)0.0403 (19)
H231.03800.62830.68090.048*
C240.9295 (4)0.5750 (5)0.7003 (3)0.0349 (18)
H240.95010.53700.72770.042*
C250.8461 (4)0.5779 (4)0.6892 (3)0.0307 (17)
H250.80940.54340.71000.037*
C260.7291 (5)0.5467 (5)0.3700 (4)0.048 (2)
H260.71120.55500.40940.058*
Cl30.78431 (14)0.63807 (16)0.34978 (10)0.0597 (7)
Cl40.64232 (18)0.5366 (2)0.32931 (12)0.0945 (10)
Cl50.7915 (2)0.45719 (19)0.36777 (13)0.0998 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt0.01974 (13)0.01757 (13)0.01745 (14)0.00010 (11)0.00050 (12)0.00012 (12)
Cl10.0311 (9)0.0368 (10)0.0192 (9)0.0052 (8)0.0034 (8)0.0003 (8)
Cl20.0255 (9)0.0239 (8)0.0273 (10)0.0040 (7)0.0016 (8)0.0016 (7)
P10.0235 (9)0.0176 (9)0.0226 (10)0.0011 (7)0.0012 (8)0.0005 (8)
P20.0229 (9)0.0253 (9)0.0209 (10)0.0012 (7)0.0020 (8)0.0018 (8)
N10.026 (3)0.029 (3)0.016 (3)0.001 (2)0.006 (3)0.001 (3)
N20.022 (3)0.029 (3)0.015 (3)0.002 (2)0.004 (2)0.005 (2)
O0.041 (3)0.069 (4)0.029 (3)0.011 (3)0.001 (3)0.022 (3)
C10.030 (4)0.047 (5)0.028 (5)0.004 (4)0.008 (4)0.001 (4)
C20.031 (4)0.026 (4)0.033 (5)0.003 (3)0.002 (4)0.001 (4)
C30.036 (4)0.052 (5)0.044 (5)0.006 (4)0.005 (4)0.022 (4)
C40.033 (4)0.015 (3)0.034 (4)0.003 (3)0.001 (3)0.002 (3)
C50.039 (4)0.020 (4)0.033 (4)0.010 (3)0.005 (3)0.002 (3)
C60.045 (5)0.026 (4)0.040 (4)0.006 (4)0.000 (4)0.003 (4)
C70.040 (4)0.026 (4)0.054 (5)0.002 (4)0.009 (4)0.010 (4)
C80.024 (3)0.023 (3)0.019 (4)0.005 (3)0.003 (3)0.001 (3)
C90.028 (4)0.022 (3)0.041 (5)0.004 (3)0.004 (3)0.004 (3)
C100.024 (4)0.031 (3)0.043 (5)0.005 (3)0.016 (4)0.003 (3)
C110.029 (4)0.038 (4)0.027 (4)0.008 (3)0.003 (4)0.000 (3)
C120.032 (4)0.021 (3)0.037 (5)0.003 (3)0.004 (3)0.003 (3)
C130.025 (3)0.019 (3)0.034 (4)0.000 (3)0.001 (3)0.001 (3)
C140.021 (4)0.023 (3)0.030 (4)0.001 (3)0.003 (3)0.005 (3)
C150.034 (4)0.027 (4)0.027 (4)0.003 (3)0.003 (3)0.005 (3)
C160.048 (5)0.023 (4)0.052 (5)0.002 (3)0.001 (4)0.007 (4)
C170.038 (5)0.030 (4)0.059 (5)0.004 (4)0.008 (4)0.020 (4)
C180.030 (4)0.044 (4)0.038 (5)0.009 (3)0.005 (4)0.021 (3)
C190.035 (4)0.035 (4)0.031 (4)0.005 (3)0.005 (4)0.003 (3)
C200.026 (4)0.028 (3)0.021 (4)0.002 (3)0.000 (3)0.007 (3)
C210.027 (3)0.035 (4)0.026 (4)0.003 (3)0.003 (3)0.001 (3)
C220.025 (3)0.046 (5)0.033 (4)0.009 (3)0.004 (3)0.013 (3)
C230.027 (4)0.050 (5)0.045 (5)0.008 (3)0.004 (4)0.011 (4)
C240.029 (4)0.044 (5)0.032 (5)0.014 (3)0.008 (3)0.000 (4)
C250.035 (4)0.031 (4)0.026 (4)0.005 (3)0.004 (3)0.001 (3)
C260.048 (5)0.059 (5)0.039 (5)0.003 (4)0.007 (4)0.002 (5)
Cl30.0477 (13)0.0792 (16)0.0522 (15)0.0073 (12)0.0036 (12)0.0142 (13)
Cl40.0788 (19)0.149 (3)0.0555 (18)0.039 (2)0.0225 (15)0.0187 (19)
Cl50.141 (3)0.0783 (19)0.080 (2)0.048 (2)0.063 (2)0.0207 (17)
Geometric parameters (Å, º) top
Pt—P22.2102 (19)C9—C101.388 (8)
Pt—P12.2275 (18)C9—H90.9500
Pt—Cl22.3658 (16)C10—C111.390 (9)
Pt—Cl12.3658 (18)C10—H100.9500
P1—N11.739 (6)C11—C121.387 (8)
P1—C81.814 (7)C11—H110.9500
P1—C41.874 (6)C12—C131.380 (8)
P2—N21.711 (6)C12—H120.9500
P2—C201.806 (7)C13—H130.9500
P2—C141.812 (7)C14—C151.382 (8)
N1—C21.400 (9)C14—C191.400 (8)
N1—C11.491 (8)C15—C161.390 (8)
N2—C21.387 (8)C15—H150.9500
N2—C31.482 (9)C16—C171.378 (9)
O—C21.212 (8)C16—H160.9500
C1—H1A0.9800C17—C181.380 (9)
C1—H1B0.9800C17—H170.9500
C1—H1C0.9800C18—C191.377 (9)
C3—H3A0.9800C18—H180.9500
C3—H3B0.9800C19—H190.9500
C3—H3C0.9800C20—C211.393 (8)
C4—C71.534 (9)C20—C251.396 (8)
C4—C51.535 (9)C21—C221.388 (9)
C4—C61.547 (10)C21—H210.9500
C5—H5A0.9800C22—C231.380 (9)
C5—H5B0.9800C22—H220.9500
C5—H5C0.9800C23—C241.372 (9)
C6—H6A0.9800C23—H230.9500
C6—H6B0.9800C24—C251.393 (9)
C6—H6C0.9800C24—H240.9500
C7—H7A0.9800C25—H250.9500
C7—H7B0.9800C26—Cl41.734 (9)
C7—H7C0.9800C26—Cl51.735 (8)
C8—C131.394 (8)C26—Cl31.760 (9)
C8—C91.398 (8)C26—H261.0000
P2—Pt—P189.41 (7)H7B—C7—H7C109.5
P2—Pt—Cl292.05 (6)C13—C8—C9120.0 (6)
P1—Pt—Cl2176.43 (6)C13—C8—P1115.2 (5)
P2—Pt—Cl1175.87 (6)C9—C8—P1124.5 (5)
P1—Pt—Cl189.86 (6)C10—C9—C8118.4 (6)
Cl2—Pt—Cl188.46 (6)C10—C9—H9120.8
N1—P1—C8100.3 (3)C8—C9—H9120.8
N1—P1—C4106.3 (3)C9—C10—C11121.5 (6)
C8—P1—C4113.5 (3)C9—C10—H10119.3
N1—P1—Pt112.6 (2)C11—C10—H10119.3
C8—P1—Pt108.8 (2)C12—C11—C10119.6 (7)
C4—P1—Pt114.5 (2)C12—C11—H11120.2
N2—P2—C20102.0 (3)C10—C11—H11120.2
N2—P2—C14105.2 (3)C13—C12—C11119.7 (6)
C20—P2—C14108.0 (3)C13—C12—H12120.2
N2—P2—Pt114.4 (2)C11—C12—H12120.2
C20—P2—Pt116.5 (2)C12—C13—C8120.8 (6)
C14—P2—Pt109.9 (2)C12—C13—H13119.6
C2—N1—C1112.6 (6)C8—C13—H13119.6
C2—N1—P1123.0 (5)C15—C14—C19118.7 (6)
C1—N1—P1120.0 (5)C15—C14—P2119.1 (5)
C2—N2—C3114.2 (6)C19—C14—P2122.1 (5)
C2—N2—P2121.5 (5)C14—C15—C16121.1 (7)
C3—N2—P2122.7 (4)C14—C15—H15119.5
N1—C1—H1A109.5C16—C15—H15119.5
N1—C1—H1B109.5C17—C16—C15119.5 (7)
H1A—C1—H1B109.5C17—C16—H16120.3
N1—C1—H1C109.5C15—C16—H16120.3
H1A—C1—H1C109.5C16—C17—C18120.1 (7)
H1B—C1—H1C109.5C16—C17—H17120.0
O—C2—N2122.7 (7)C18—C17—H17120.0
O—C2—N1120.6 (6)C19—C18—C17120.6 (7)
N2—C2—N1116.7 (6)C19—C18—H18119.7
N2—C3—H3A109.5C17—C18—H18119.7
N2—C3—H3B109.5C18—C19—C14120.1 (7)
H3A—C3—H3B109.5C18—C19—H19120.0
N2—C3—H3C109.5C14—C19—H19120.0
H3A—C3—H3C109.5C21—C20—C25119.7 (6)
H3B—C3—H3C109.5C21—C20—P2119.2 (5)
C7—C4—C5108.9 (6)C25—C20—P2120.9 (5)
C7—C4—C6110.6 (6)C22—C21—C20119.5 (7)
C5—C4—C6108.7 (6)C22—C21—H21120.3
C7—C4—P1112.1 (5)C20—C21—H21120.3
C5—C4—P1106.2 (5)C23—C22—C21120.3 (7)
C6—C4—P1110.2 (5)C23—C22—H22119.8
C4—C5—H5A109.5C21—C22—H22119.8
C4—C5—H5B109.5C24—C23—C22120.7 (7)
H5A—C5—H5B109.5C24—C23—H23119.6
C4—C5—H5C109.5C22—C23—H23119.6
H5A—C5—H5C109.5C23—C24—C25119.7 (7)
H5B—C5—H5C109.5C23—C24—H24120.2
C4—C6—H6A109.5C25—C24—H24120.2
C4—C6—H6B109.5C24—C25—C20120.0 (7)
H6A—C6—H6B109.5C24—C25—H25120.0
C4—C6—H6C109.5C20—C25—H25120.0
H6A—C6—H6C109.5Cl4—C26—Cl5113.0 (5)
H6B—C6—H6C109.5Cl4—C26—Cl3109.8 (5)
C4—C7—H7A109.5Cl5—C26—Cl3110.2 (5)
C4—C7—H7B109.5Cl4—C26—H26107.9
H7A—C7—H7B109.5Cl5—C26—H26107.9
C4—C7—H7C109.5Cl3—C26—H26107.9
H7A—C7—H7C109.5
P2—Pt—P1—N114.7 (2)C4—P1—C8—C13169.6 (5)
P2—Pt—P1—C8125.0 (2)Pt—P1—C8—C1340.9 (6)
P2—Pt—P1—C4106.9 (3)N1—P1—C8—C995.6 (6)
Cl1—Pt—P1—N1161.2 (2)C4—P1—C8—C917.3 (7)
Cl1—Pt—P1—C851.0 (2)Pt—P1—C8—C9146.0 (5)
Cl1—Pt—P1—C477.2 (3)C13—C8—C9—C100.2 (9)
P1—Pt—P2—N231.0 (2)P1—C8—C9—C10173.0 (5)
Cl2—Pt—P2—N2152.2 (2)C8—C9—C10—C110.1 (10)
P1—Pt—P2—C20149.8 (2)C9—C10—C11—C120.2 (11)
Cl2—Pt—P2—C2033.5 (2)C10—C11—C12—C130.4 (11)
P1—Pt—P2—C1487.0 (2)C11—C12—C13—C80.5 (11)
Cl2—Pt—P2—C1489.8 (2)C9—C8—C13—C120.4 (10)
C8—P1—N1—C2176.4 (5)P1—C8—C13—C12173.9 (6)
C4—P1—N1—C265.3 (6)N2—P2—C14—C15150.4 (5)
Pt—P1—N1—C260.9 (5)C20—P2—C14—C15101.3 (5)
C8—P1—N1—C128.9 (6)Pt—P2—C14—C1526.8 (5)
C4—P1—N1—C189.4 (5)N2—P2—C14—C1926.1 (6)
Pt—P1—N1—C1144.4 (5)C20—P2—C14—C1982.3 (6)
C20—P2—N2—C2169.8 (5)Pt—P2—C14—C19149.7 (5)
C14—P2—N2—C257.2 (6)C19—C14—C15—C160.6 (9)
Pt—P2—N2—C263.5 (6)P2—C14—C15—C16176.0 (5)
C20—P2—N2—C34.7 (6)C14—C15—C16—C170.1 (9)
C14—P2—N2—C3108.0 (6)C15—C16—C17—C181.7 (11)
Pt—P2—N2—C3131.3 (5)C16—C17—C18—C192.6 (11)
C3—N2—C2—O12.5 (10)C17—C18—C19—C141.9 (11)
P2—N2—C2—O153.9 (6)C15—C14—C19—C180.3 (10)
C3—N2—C2—N1168.8 (6)P2—C14—C19—C18176.7 (5)
P2—N2—C2—N124.9 (8)N2—P2—C20—C2189.0 (5)
C1—N1—C2—O17.4 (9)C14—P2—C20—C21160.5 (5)
P1—N1—C2—O139.0 (6)Pt—P2—C20—C2136.2 (6)
C1—N1—C2—N2161.4 (6)N2—P2—C20—C2586.3 (6)
P1—N1—C2—N242.2 (8)C14—P2—C20—C2524.2 (6)
N1—P1—C4—C741.9 (6)Pt—P2—C20—C25148.4 (5)
C8—P1—C4—C767.4 (6)C25—C20—C21—C220.1 (9)
Pt—P1—C4—C7166.8 (5)P2—C20—C21—C22175.5 (5)
N1—P1—C4—C577.0 (5)C20—C21—C22—C231.8 (9)
C8—P1—C4—C5173.7 (5)C21—C22—C23—C244.0 (11)
Pt—P1—C4—C548.0 (5)C22—C23—C24—C254.3 (12)
N1—P1—C4—C6165.5 (5)C23—C24—C25—C202.5 (11)
C8—P1—C4—C656.2 (6)C21—C20—C25—C240.4 (10)
Pt—P1—C4—C669.5 (5)P2—C20—C25—C24175.7 (6)
N1—P1—C8—C1377.5 (6)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C26—H26···Cl11.002.763.484 (9)130
C26—H26···Cl21.002.763.579 (9)139
C11—H11···Cl2i0.952.773.560 (7)142
Symmetry code: (i) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formula[PtCl2(C25H30N2OP2)]·CHCl3
Mr821.81
Crystal system, space groupOrthorhombic, Pbca
Temperature (K)178
a, b, c (Å)16.380 (4), 15.653 (3), 24.074 (4)
V3)6172 (2)
Z8
Radiation typeMo Kα
µ (mm1)5.11
Crystal size (mm)0.40 × 0.40 × 0.15
Data collection
DiffractometerNicolet R3
diffractometer
Absorption correctionψ scan
(XEMP; Nicolet, 1987)
Tmin, Tmax0.506, 0.999
No. of measured, independent and
observed [I > 2σ(I)] reflections
10607, 5419, 3612
Rint0.043
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.087, 1.05
No. of reflections5419
No. of parameters339
No. of restraints66
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)2.40, 0.85

Computer programs: P3 (Nicolet, 1987), P3, XDISK (Nicolet, 1987), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP (Siemens, 1994), SHELXL97.

Selected geometric parameters (Å, º) top
Pt—P22.2102 (19)P2—C201.806 (7)
Pt—P12.2275 (18)P2—C141.812 (7)
Pt—Cl22.3658 (16)N1—C21.400 (9)
Pt—Cl12.3658 (18)N1—C11.491 (8)
P1—N11.739 (6)N2—C21.387 (8)
P1—C81.814 (7)N2—C31.482 (9)
P1—C41.874 (6)O—C21.212 (8)
P2—N21.711 (6)
P2—Pt—P189.41 (7)C20—P2—C14108.0 (3)
P2—Pt—Cl292.05 (6)N2—P2—Pt114.4 (2)
P1—Pt—Cl2176.43 (6)C20—P2—Pt116.5 (2)
P2—Pt—Cl1175.87 (6)C14—P2—Pt109.9 (2)
P1—Pt—Cl189.86 (6)C2—N1—C1112.6 (6)
Cl2—Pt—Cl188.46 (6)C2—N1—P1123.0 (5)
N1—P1—C8100.3 (3)C1—N1—P1120.0 (5)
N1—P1—C4106.3 (3)C2—N2—C3114.2 (6)
C8—P1—C4113.5 (3)C2—N2—P2121.5 (5)
N1—P1—Pt112.6 (2)C3—N2—P2122.7 (4)
C8—P1—Pt108.8 (2)O—C2—N2122.7 (7)
C4—P1—Pt114.5 (2)O—C2—N1120.6 (6)
N2—P2—C20102.0 (3)N2—C2—N1116.7 (6)
N2—P2—C14105.2 (3)
P2—Pt—P1—N114.7 (2)Pt—P2—N2—C263.5 (6)
P1—Pt—P2—N231.0 (2)P2—N2—C2—N124.9 (8)
Pt—P1—N1—C260.9 (5)P1—N1—C2—N242.2 (8)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C26—H26···Cl11.002.763.484 (9)130
C26—H26···Cl21.002.763.579 (9)139
C11—H11···Cl2i0.952.773.560 (7)142
Symmetry code: (i) x+1, y+1, z+1.
 

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