The title complex, [PtCl
4(C
12H
24N
4O
2)] or
trans-[PtCl
4{NH= C(Et)ON=CMe
2}
2], possesses a crystallographically imposed centre of symmetry. The coordination polyhedron of the complex is a slightly distorted octahedron. The two imino ligands are mutually
trans. This configuration is stabilized by intramolecular N—H
N hydrogen bonding between the imine H atom and the oxime N atom.
Supporting information
CCDC reference: 629459
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean (C-C) = 0.008 Å
- R factor = 0.031
- wR factor = 0.092
- Data-to-parameter ratio = 19.7
checkCIF/PLATON results
No syntax errors found
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
Tmin and Tmax reported: 0.213 0.461
Tmin and Tmax expected: 0.171 0.463
RR = 1.252
Please check that your absorption correction is appropriate.
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.25
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
2 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
0 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
0 ALERT type 5 Informative message, check
Data collection: COLLECT (Bruker, 2004); cell refinement: DENZO and SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97.
trans-Bis[(E)-acetone
O-propanimidoyloxime-
κN']tetrachloroplatinum(IV)
top
Crystal data top
[PtCl4(C12H24N4O2)] | F(000) = 1144 |
Mr = 593.24 | Dx = 2.006 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 13900 reflections |
a = 18.0119 (9) Å | θ = 3.0–27.4° |
b = 6.8727 (4) Å | µ = 7.70 mm−1 |
c = 16.4295 (6) Å | T = 120 K |
β = 105.059 (3)° | Block, yellow |
V = 1963.97 (17) Å3 | 0.27 × 0.20 × 0.10 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD area-detector diffractometer | 2223 independent reflections |
Radiation source: fine-focus sealed tube | 1852 reflections with I > 2σ(I) |
Horizontally mounted graphite crystal monochromator | Rint = 0.061 |
Detector resolution: 9 pixels mm-1 | θmax = 27.4°, θmin = 3.0° |
φ scans, and ω scans with κ offset | h = −23→23 |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | k = −8→8 |
Tmin = 0.214, Tmax = 0.461 | l = −20→21 |
13900 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.092 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | w = 1/[σ2(Fo2) + (0.0546P)2 + 4.3124P] where P = (Fo2 + 2Fc2)/3 |
2223 reflections | (Δ/σ)max < 0.001 |
113 parameters | Δρmax = 2.19 e Å−3 |
0 restraints | Δρmin = −1.81 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Pt1 | 0.7500 | 0.2500 | 0.5000 | 0.02485 (12) | |
Cl1 | 0.82730 (7) | 0.51297 (19) | 0.48819 (8) | 0.0323 (3) | |
Cl2 | 0.83276 (7) | 0.04814 (18) | 0.45238 (7) | 0.0325 (3) | |
O2 | 0.6055 (2) | 0.3608 (6) | 0.2539 (2) | 0.0324 (8) | |
N1 | 0.6845 (3) | 0.2620 (6) | 0.3795 (3) | 0.0285 (10) | |
H1 | 0.669 (4) | 0.148 (12) | 0.360 (5) | 0.05 (2)* | |
N2 | 0.5921 (2) | 0.1514 (7) | 0.2396 (3) | 0.0316 (9) | |
C1 | 0.6533 (3) | 0.3988 (8) | 0.3299 (3) | 0.0293 (10) | |
C2 | 0.6645 (3) | 0.6120 (7) | 0.3436 (3) | 0.0319 (10) | |
H2A | 0.6892 | 0.6375 | 0.4038 | 0.038* | |
H2B | 0.6139 | 0.6780 | 0.3287 | 0.038* | |
C3 | 0.7147 (4) | 0.6941 (9) | 0.2898 (4) | 0.0388 (12) | |
H3A | 0.7653 | 0.6310 | 0.3055 | 0.058* | |
H3B | 0.7210 | 0.8346 | 0.2993 | 0.058* | |
H3C | 0.6902 | 0.6693 | 0.2301 | 0.058* | |
C4 | 0.5506 (3) | 0.1220 (8) | 0.1647 (3) | 0.0321 (11) | |
C5 | 0.5204 (4) | 0.2739 (8) | 0.0985 (4) | 0.0380 (14) | |
H5A | 0.5233 | 0.4022 | 0.1251 | 0.057* | |
H5B | 0.4667 | 0.2446 | 0.0696 | 0.057* | |
H5C | 0.5513 | 0.2739 | 0.0574 | 0.057* | |
C6 | 0.5324 (3) | −0.0844 (8) | 0.1420 (3) | 0.0377 (12) | |
H6A | 0.5599 | −0.1256 | 0.1006 | 0.057* | |
H6B | 0.4769 | −0.0986 | 0.1176 | 0.057* | |
H6C | 0.5484 | −0.1655 | 0.1925 | 0.057* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pt1 | 0.02603 (17) | 0.02780 (19) | 0.02122 (18) | 0.00026 (8) | 0.00705 (11) | −0.00101 (8) |
Cl1 | 0.0321 (6) | 0.0338 (7) | 0.0310 (6) | −0.0037 (5) | 0.0082 (4) | 0.0008 (5) |
Cl2 | 0.0338 (6) | 0.0368 (7) | 0.0280 (6) | 0.0049 (5) | 0.0101 (5) | −0.0037 (5) |
O2 | 0.0362 (19) | 0.033 (2) | 0.0264 (18) | −0.0010 (15) | 0.0053 (15) | −0.0004 (15) |
N1 | 0.031 (2) | 0.031 (3) | 0.023 (2) | −0.0011 (16) | 0.0072 (19) | −0.0019 (16) |
N2 | 0.033 (2) | 0.032 (3) | 0.031 (2) | −0.0033 (18) | 0.0102 (18) | −0.0009 (19) |
C1 | 0.026 (2) | 0.040 (3) | 0.022 (2) | 0.0019 (19) | 0.0074 (19) | −0.004 (2) |
C2 | 0.032 (2) | 0.034 (3) | 0.029 (2) | 0.0040 (19) | 0.007 (2) | −0.0053 (19) |
C3 | 0.047 (3) | 0.036 (3) | 0.034 (3) | −0.002 (3) | 0.011 (2) | 0.002 (3) |
C4 | 0.025 (2) | 0.047 (3) | 0.027 (2) | −0.002 (2) | 0.010 (2) | 0.000 (2) |
C5 | 0.038 (3) | 0.049 (4) | 0.023 (3) | −0.003 (2) | 0.003 (2) | 0.000 (2) |
C6 | 0.038 (3) | 0.042 (3) | 0.031 (3) | −0.006 (2) | 0.007 (2) | −0.002 (2) |
Geometric parameters (Å, º) top
Pt1—N1i | 2.026 (5) | C2—H2A | 0.9900 |
Pt1—N1 | 2.026 (5) | C2—H2B | 0.9900 |
Pt1—Cl2i | 2.3161 (11) | C3—H3A | 0.9800 |
Pt1—Cl2 | 2.3162 (11) | C3—H3B | 0.9800 |
Pt1—Cl1 | 2.3201 (12) | C3—H3C | 0.9800 |
Pt1—Cl1i | 2.3201 (12) | C4—C6 | 1.482 (7) |
O2—C1 | 1.345 (6) | C4—C5 | 1.505 (7) |
O2—N2 | 1.468 (7) | C5—H5A | 0.9800 |
N1—C1 | 1.275 (7) | C5—H5B | 0.9800 |
N1—H1 | 0.86 (8) | C5—H5C | 0.9800 |
N2—C4 | 1.279 (7) | C6—H6A | 0.9800 |
C1—C2 | 1.488 (7) | C6—H6B | 0.9800 |
C2—C3 | 1.527 (8) | C6—H6C | 0.9800 |
| | | |
N1i—Pt1—N1 | 179.998 (1) | C3—C2—H2A | 109.5 |
N1i—Pt1—Cl2i | 87.52 (14) | C1—C2—H2B | 109.5 |
N1—Pt1—Cl2i | 92.48 (14) | C3—C2—H2B | 109.5 |
N1i—Pt1—Cl2 | 92.47 (14) | H2A—C2—H2B | 108.1 |
N1—Pt1—Cl2 | 87.52 (14) | C2—C3—H3A | 109.5 |
Cl2i—Pt1—Cl2 | 179.999 (2) | C2—C3—H3B | 109.5 |
N1i—Pt1—Cl1 | 84.47 (13) | H3A—C3—H3B | 109.5 |
N1—Pt1—Cl1 | 95.53 (13) | C2—C3—H3C | 109.5 |
Cl2i—Pt1—Cl1 | 90.83 (4) | H3A—C3—H3C | 109.5 |
Cl2—Pt1—Cl1 | 89.17 (4) | H3B—C3—H3C | 109.5 |
N1i—Pt1—Cl1i | 95.53 (13) | N2—C4—C6 | 115.5 (5) |
N1—Pt1—Cl1i | 84.47 (13) | N2—C4—C5 | 126.7 (5) |
Cl2i—Pt1—Cl1i | 89.17 (4) | C6—C4—C5 | 117.8 (4) |
Cl2—Pt1—Cl1i | 90.83 (4) | C4—C5—H5A | 109.5 |
Cl1—Pt1—Cl1i | 180.0 | C4—C5—H5B | 109.5 |
C1—O2—N2 | 112.2 (4) | H5A—C5—H5B | 109.5 |
C1—N1—Pt1 | 134.6 (4) | C4—C5—H5C | 109.5 |
C1—N1—H1 | 113 (5) | H5A—C5—H5C | 109.5 |
Pt1—N1—H1 | 112 (5) | H5B—C5—H5C | 109.5 |
C4—N2—O2 | 109.9 (4) | C4—C6—H6A | 109.5 |
N1—C1—O2 | 121.3 (5) | C4—C6—H6B | 109.5 |
N1—C1—C2 | 127.5 (5) | H6A—C6—H6B | 109.5 |
O2—C1—C2 | 111.1 (4) | C4—C6—H6C | 109.5 |
C1—C2—C3 | 110.7 (4) | H6A—C6—H6C | 109.5 |
C1—C2—H2A | 109.5 | H6B—C6—H6C | 109.5 |
Symmetry code: (i) −x+3/2, −y+1/2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···N2 | 0.86 (8) | 2.10 (7) | 2.577 (7) | 114 (6) |