Download citation
Download citation
link to html
The title PtIV complex, [PtCl4(C16H28N4O6)] or trans-[PtCl4{NH=C(Et)ON=C(Me)C(=O)OEt}2], possesses a crystallographically imposed centre of symmetry. The coordination environment of the metal centre is a slightly distorted octa­hedron. An intra­molecular N—H...N hydrogen bond between the imine H atom and the oxime N atom stabilizes the E configuration of the imine groups.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805025183/cv6558sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805025183/cv6558Isup2.hkl
Contains datablock I

CCDC reference: 283788

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.020
  • wR factor = 0.042
  • Data-to-parameter ratio = 19.0

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O2 .. 2.84 Ang. PLAT432_ALERT_2_B Short Inter X...Y Contact O2 .. C1 .. 2.88 Ang.
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.270 0.387 Tmin(prime) and Tmax expected: 0.328 0.387 RR(prime) = 0.824 Please check that your absorption correction is appropriate. PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.76 PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C4 - C6 ... 1.53 Ang.
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 2000); cell refinement: DENZO/SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO/SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Sheldrick, 2003); software used to prepare material for publication: SHELXL97.

trans-Tetrachlorobis[(E)-ethyl 2-(1-iminopropoxyimino)propanoate]platinum(IV) top
Crystal data top
[PtCl4(C16H28N4O6)]F(000) = 692
Mr = 709.31Dx = 1.960 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 11553 reflections
a = 8.5514 (3) Åθ = 2.5–27.5°
b = 8.3410 (3) ŵ = 6.32 mm1
c = 17.6134 (7) ÅT = 100 K
β = 106.939 (2)°Block, yellow
V = 1201.81 (8) Å30.17 × 0.16 × 0.15 mm
Z = 2
Data collection top
Nonius KappaCCD area-detector
diffractometer
2748 independent reflections
Radiation source: fine-focus sealed tube2274 reflections with I > 2σ(I)
Horizonally mounted graphite crystal monochromatorRint = 0.033
Detector resolution: 9 pixels mm-1θmax = 27.5°, θmin = 2.5°
φ scans, and ω scans with κ offseth = 1110
Absorption correction: multi-scan
(XPREP in SHELXTL; Sheldrick, 2003)
k = 109
Tmin = 0.270, Tmax = 0.388l = 2222
11553 measured reflections
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)] = 0.020Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.042H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0126P)2 + 0.4361P]
where P = (Fo2 + 2Fc2)/3
2748 reflections(Δ/σ)max = 0.001
145 parametersΔρmax = 0.78 e Å3
0 restraintsΔρmin = 1.40 e Å3
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pt10.00000.00000.00000.01196 (5)
Cl10.12400 (8)0.08601 (9)0.12882 (4)0.01751 (14)
Cl20.24660 (7)0.10073 (9)0.01023 (4)0.01822 (15)
O10.1347 (2)0.4454 (2)0.08360 (11)0.0196 (4)
O20.1627 (2)0.7057 (3)0.30654 (11)0.0243 (5)
O30.2872 (2)0.5123 (2)0.25730 (12)0.0215 (5)
N10.0287 (3)0.2138 (3)0.04816 (13)0.0147 (5)
H10.06170.24800.08260.018*
N20.0225 (3)0.4632 (3)0.14134 (14)0.0191 (6)
C10.1477 (3)0.3102 (3)0.03998 (16)0.0178 (6)
C20.3180 (3)0.2946 (4)0.01449 (17)0.0209 (6)
H2A0.32360.20000.04910.025*
H2B0.39420.27620.01750.025*
C30.3727 (4)0.4430 (4)0.06615 (19)0.0263 (7)
H3A0.30690.45360.10310.039*
H3B0.48830.43230.09620.039*
H3C0.35800.53840.03230.039*
C40.0061 (3)0.5635 (4)0.19350 (16)0.0169 (6)
C50.1482 (3)0.6435 (4)0.19566 (16)0.0201 (6)
H5A0.22950.56200.19760.030*
H5B0.12670.71180.24290.030*
H5C0.19000.70930.14790.030*
C60.1626 (3)0.6019 (4)0.25982 (16)0.0176 (6)
C70.4395 (3)0.5500 (4)0.31963 (17)0.0218 (7)
H7A0.41530.56530.37080.026*
H7B0.51640.45890.32570.026*
C80.5190 (3)0.7016 (4)0.29922 (17)0.0239 (7)
H8A0.44410.79240.29470.036*
H8B0.62070.72330.34120.036*
H8C0.54330.68630.24870.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.01299 (8)0.01114 (8)0.01040 (7)0.00026 (6)0.00127 (5)0.00058 (6)
Cl10.0201 (3)0.0177 (4)0.0120 (3)0.0002 (3)0.0004 (2)0.0018 (3)
Cl20.0157 (3)0.0196 (4)0.0188 (3)0.0026 (3)0.0041 (2)0.0001 (3)
O10.0175 (10)0.0185 (11)0.0188 (10)0.0025 (8)0.0012 (8)0.0048 (8)
O20.0235 (11)0.0276 (13)0.0204 (11)0.0006 (9)0.0042 (8)0.0074 (9)
O30.0168 (10)0.0201 (12)0.0236 (11)0.0002 (8)0.0005 (8)0.0045 (9)
N10.0137 (11)0.0144 (13)0.0145 (11)0.0005 (9)0.0014 (8)0.0003 (10)
N20.0173 (12)0.0185 (15)0.0182 (12)0.0008 (9)0.0001 (10)0.0019 (10)
C10.0245 (15)0.0146 (16)0.0143 (13)0.0009 (12)0.0057 (11)0.0004 (12)
C20.0170 (14)0.0223 (17)0.0212 (15)0.0033 (12)0.0023 (11)0.0024 (13)
C30.0209 (15)0.0280 (18)0.0269 (16)0.0018 (13)0.0021 (12)0.0014 (14)
C40.0197 (14)0.0138 (15)0.0168 (14)0.0016 (12)0.0047 (11)0.0019 (12)
C50.0212 (14)0.0198 (17)0.0178 (14)0.0015 (12)0.0034 (11)0.0015 (12)
C60.0244 (15)0.0123 (15)0.0201 (14)0.0014 (12)0.0128 (11)0.0002 (12)
C70.0173 (14)0.0225 (17)0.0201 (15)0.0015 (12)0.0030 (11)0.0013 (12)
C80.0173 (14)0.033 (2)0.0201 (15)0.0024 (13)0.0034 (11)0.0033 (13)
Geometric parameters (Å, º) top
Pt1—N1i2.020 (2)C2—H2A0.9900
Pt1—N12.020 (2)C2—H2B0.9900
Pt1—Cl12.3206 (6)C3—H3A0.9800
Pt1—Cl1i2.3207 (6)C3—H3B0.9800
Pt1—Cl22.3252 (6)C3—H3C0.9800
Pt1—Cl2i2.3252 (6)C4—C51.489 (4)
O1—C11.351 (3)C4—C61.532 (4)
O1—N21.437 (3)C5—H5A0.9800
O2—C61.195 (3)C5—H5B0.9800
O3—C61.312 (3)C5—H5C0.9800
O3—C71.472 (3)C7—C81.527 (4)
N1—C11.272 (3)C7—H7A0.9900
N1—H10.8800C7—H7B0.9900
N2—C41.280 (4)C8—H8A0.9800
C1—C21.498 (4)C8—H8B0.9800
C2—C31.527 (4)C8—H8C0.9800
N1i—Pt1—N1180.0C2—C3—H3A109.5
N1i—Pt1—Cl186.51 (6)C2—C3—H3B109.5
N1—Pt1—Cl193.49 (6)H3A—C3—H3B109.5
N1i—Pt1—Cl1i93.49 (6)C2—C3—H3C109.5
N1—Pt1—Cl1i86.51 (6)H3A—C3—H3C109.5
Cl1—Pt1—Cl1i180.0H3B—C3—H3C109.5
N1i—Pt1—Cl286.40 (6)N2—C4—C5126.4 (2)
N1—Pt1—Cl293.60 (6)N2—C4—C6115.4 (2)
Cl1—Pt1—Cl291.21 (2)C5—C4—C6118.1 (2)
Cl1i—Pt1—Cl288.79 (2)C4—C5—H5A109.5
N1i—Pt1—Cl2i93.60 (6)C4—C5—H5B109.5
N1—Pt1—Cl2i86.40 (6)H5A—C5—H5B109.5
Cl1—Pt1—Cl2i88.79 (2)C4—C5—H5C109.5
Cl1i—Pt1—Cl2i91.21 (2)H5A—C5—H5C109.5
Cl2—Pt1—Cl2i180.0H5B—C5—H5C109.5
C1—O1—N2113.2 (2)O2—C6—O3126.8 (3)
C6—O3—C7113.8 (2)O2—C6—C4120.1 (2)
C1—N1—Pt1134.54 (19)O3—C6—C4113.1 (2)
C1—N1—H1112.7O3—C7—C8111.0 (2)
Pt1—N1—H1112.7O3—C7—H7A109.4
C4—N2—O1107.5 (2)C8—C7—H7A109.4
N1—C1—O1122.2 (2)O3—C7—H7B109.4
N1—C1—C2127.9 (3)C8—C7—H7B109.4
O1—C1—C2109.9 (2)H7A—C7—H7B108.0
C1—C2—C3112.5 (2)C7—C8—H8A109.5
C1—C2—H2A109.1C7—C8—H8B109.5
C3—C2—H2A109.1H8A—C8—H8B109.5
C1—C2—H2B109.1C7—C8—H8C109.5
C3—C2—H2B109.1H8A—C8—H8C109.5
H2A—C2—H2B107.8H8B—C8—H8C109.5
Cl1—Pt1—N1—C148.5 (3)O1—C1—C2—C354.2 (3)
Cl1i—Pt1—N1—C1131.5 (3)O1—N2—C4—C51.8 (4)
Cl2—Pt1—N1—C142.9 (3)O1—N2—C4—C6178.7 (2)
Cl2i—Pt1—N1—C1137.1 (3)C7—O3—C6—O20.4 (4)
C1—O1—N2—C4160.7 (2)C7—O3—C6—C4178.8 (2)
Pt1—N1—C1—O1176.72 (19)N2—C4—C6—O2172.5 (3)
Pt1—N1—C1—C21.7 (5)C5—C4—C6—O27.9 (4)
N2—O1—C1—N12.7 (4)N2—C4—C6—O36.7 (4)
N2—O1—C1—C2176.0 (2)C5—C4—C6—O3172.9 (2)
N1—C1—C2—C3127.2 (3)C6—O3—C7—C877.4 (3)
Symmetry code: (i) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···N20.882.152.607 (3)112
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds