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The title complex, [Pt(C7F7S)2(C8H12)], has twofold rotation symmetry, with the PtII ion in an approximately square-planar coordination geometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806044436/cf2063sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806044436/cf2063Isup2.hkl
Contains datablock I

CCDC reference: 629465

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.009 Å
  • Disorder in main residue
  • R factor = 0.032
  • wR factor = 0.071
  • Data-to-parameter ratio = 17.1

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C7
Author Response: ... A constant feature found in perfluorinated molecules is that F atoms have significantly higher displacement parameters than their carrier C atoms. In the present case differences in parameters are magnified due to the disorder on CF~3~ groups.

Alert level B PLAT213_ALERT_2_B Atom F712 has ADP max/min Ratio ............. 4.60 prola PLAT213_ALERT_2_B Atom F732 has ADP max/min Ratio ............. 4.40 prola PLAT220_ALERT_2_B Large Non-Solvent F Ueq(max)/Ueq(min) ... 3.85 Ratio PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C10
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.180 0.290 Tmin and Tmax expected: 0.140 0.292 RR = 1.292 Please check that your absorption correction is appropriate. PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.31 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT213_ALERT_2_C Atom F711 has ADP max/min Ratio ............. 3.10 prola PLAT213_ALERT_2_C Atom F721 has ADP max/min Ratio ............. 3.20 prola PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.82 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Pt1
Author Response: ... A constant feature found in perfluorinated molecules is that F atoms have significantly higher displacement parameters than their carrier C atoms. In the present case differences in parameters are magnified due to the disorder on CF~3~ groups.
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.35
PLAT301_ALERT_3_C Main Residue  Disorder .........................      13.00 Perc.
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          9
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond  C8     -   C11_a  ...       1.38 Ang.

1 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 11 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 11 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 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

Computing details top

Data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXTL-Plus (Sheldrick, 1998); program(s) used to refine structure: SHELXTL-Plus; molecular graphics: SHELXTL-Plus; software used to prepare material for publication: SHELXTL-Plus.

[(1,2:5,6-η)-Cycloocta-1,5-diene]bis[2,3,5,6-tetrafluoro-4- (trifluoromethyl)benzenethiolato]platinum(II) top
Crystal data top
[Pt(C7F7S)2(C8H12)]F(000) = 1520
Mr = 801.53Dx = 2.221 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 61 reflections
a = 18.4374 (15) Åθ = 4.7–12.5°
b = 12.9716 (10) ŵ = 6.15 mm1
c = 13.3604 (11) ÅT = 298 K
β = 131.392 (3)°Irregular fragment, yellow
V = 2397.1 (3) Å30.38 × 0.28 × 0.20 mm
Z = 4
Data collection top
Bruker P4
diffractometer
2908 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube, FN4Rint = 0.021
Graphite monochromatorθmax = 30.0°, θmin = 2.2°
2θ/ω scansh = 254
Absorption correction: ψ scan
(XSCANS; Siemens, 1996)
k = 118
Tmin = 0.180, Tmax = 0.290l = 1418
4611 measured reflections3 standard reflections every 97 reflections
3499 independent reflections intensity decay: 1%
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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.071H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0237P)2 + 4.9564P]
where P = (Fo2 + 2Fc2)/3
3499 reflections(Δ/σ)max = 0.002
205 parametersΔρmax = 0.78 e Å3
48 restraintsΔρmin = 0.83 e Å3
Special details top

Experimental. Analysis calculated for C22H12F14S2Pt (%): C 32.97, H 1.51, S 8.0; found (%): C 33.10, H=1.55; S=7.94. IR (cm-1) 1639m, 1474 s, 1323 s, 978m, 855w, 714m. 1H NMR, (d6-acetone): δ 2.84 (m, CH2), δ 2.87 (m, CH2), δ 4.69 (s, CH). 19F NMR, (d6-acetone): δ -57.76 (s, CF3), δ -130.79 (m, F-2,6), δ -144.76 (m, F-3,5).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pt10.50000.516046 (16)0.75000.04292 (8)
S10.59287 (9)0.39631 (8)0.92142 (10)0.0572 (3)
C10.6158 (3)0.2910 (3)0.8632 (4)0.0443 (8)
C20.6424 (3)0.3002 (3)0.7878 (5)0.0535 (10)
F20.6521 (3)0.3941 (2)0.7557 (4)0.0850 (10)
C30.6592 (3)0.2163 (4)0.7439 (5)0.0583 (11)
F30.6821 (3)0.2338 (3)0.6684 (4)0.0948 (11)
C40.6510 (3)0.1171 (4)0.7719 (4)0.0571 (11)
C50.6286 (3)0.1071 (3)0.8518 (4)0.0553 (10)
F50.6201 (3)0.0131 (2)0.8848 (4)0.0868 (11)
C60.6117 (3)0.1920 (3)0.8953 (4)0.0480 (9)
F60.5886 (2)0.1756 (2)0.9705 (3)0.0743 (8)
C70.6629 (4)0.0237 (4)0.7174 (5)0.090 (2)
C80.3890 (4)0.6344 (4)0.6222 (5)0.0706 (14)
H8A0.32410.60730.55000.085*
C90.3934 (6)0.7149 (6)0.7047 (8)0.110 (3)
H9A0.40160.78100.67920.132*
H9B0.33120.71650.68140.132*
C100.4679 (7)0.7061 (6)0.8491 (8)0.125 (3)
H10A0.43700.68550.88300.150*
H10B0.49550.77400.88500.150*
C110.5496 (4)0.6318 (4)0.9027 (5)0.0715 (14)
H11A0.57880.60250.98980.086*
F7110.7088 (13)0.0414 (8)0.6767 (18)0.192 (8)0.671 (16)
F7210.5801 (6)0.0183 (9)0.6238 (10)0.211 (11)0.671 (16)
F7310.7128 (6)0.0501 (5)0.8053 (7)0.089 (3)0.671 (16)
F7120.7534 (7)0.008 (3)0.785 (2)0.29 (3)0.329 (16)
F7220.6260 (16)0.0472 (12)0.5967 (12)0.118 (7)0.329 (16)
F7320.615 (2)0.0560 (12)0.700 (3)0.212 (19)0.329 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.05113 (13)0.03173 (10)0.04706 (12)0.0000.03295 (10)0.000
S10.0691 (7)0.0427 (5)0.0444 (5)0.0077 (5)0.0309 (5)0.0001 (4)
C10.040 (2)0.0393 (19)0.045 (2)0.0002 (15)0.0244 (17)0.0005 (15)
C20.053 (2)0.047 (2)0.065 (3)0.0009 (18)0.041 (2)0.0108 (19)
F20.107 (3)0.0570 (17)0.134 (3)0.0018 (16)0.098 (2)0.0203 (18)
C30.057 (3)0.071 (3)0.059 (2)0.017 (2)0.043 (2)0.016 (2)
F30.124 (3)0.104 (3)0.117 (3)0.032 (2)0.105 (3)0.030 (2)
C40.059 (3)0.057 (3)0.052 (2)0.015 (2)0.035 (2)0.0044 (19)
C50.064 (3)0.040 (2)0.057 (2)0.0076 (19)0.038 (2)0.0100 (18)
F50.136 (3)0.0408 (14)0.112 (3)0.0127 (16)0.094 (3)0.0170 (15)
C60.051 (2)0.047 (2)0.046 (2)0.0053 (17)0.0323 (19)0.0080 (17)
F60.115 (2)0.0602 (16)0.088 (2)0.0165 (16)0.084 (2)0.0212 (15)
C70.094 (5)0.098 (5)0.059 (3)0.041 (4)0.043 (3)0.000 (3)
C80.073 (3)0.048 (3)0.069 (3)0.016 (2)0.037 (3)0.009 (2)
C90.113 (6)0.094 (5)0.115 (5)0.043 (4)0.072 (5)0.002 (4)
C100.181 (9)0.096 (5)0.116 (6)0.057 (5)0.106 (6)0.003 (4)
C110.099 (4)0.043 (2)0.066 (3)0.000 (2)0.052 (3)0.015 (2)
F7110.36 (2)0.121 (7)0.306 (19)0.101 (11)0.31 (2)0.067 (10)
F7210.116 (8)0.205 (15)0.110 (7)0.070 (9)0.011 (6)0.097 (8)
F7310.109 (6)0.047 (3)0.100 (5)0.025 (3)0.064 (5)0.001 (3)
F7120.097 (14)0.42 (5)0.16 (2)0.11 (2)0.007 (13)0.18 (3)
F7220.20 (2)0.097 (11)0.113 (11)0.038 (12)0.128 (14)0.049 (9)
F7320.47 (6)0.045 (8)0.34 (4)0.09 (2)0.37 (4)0.069 (16)
Geometric parameters (Å, º) top
Pt1—S12.3245 (11)C7—F7321.277 (9)
Pt1—C82.200 (5)C7—F7121.283 (9)
Pt1—C112.188 (4)C7—F7211.291 (8)
Pt1—C11i2.188 (4)C7—F7111.293 (8)
Pt1—C8i2.200 (5)C7—F7221.306 (8)
Pt1—S1i2.3245 (11)C7—F7311.310 (7)
S1—C11.756 (4)C8—C11i1.376 (8)
C1—C61.372 (6)C8—C91.481 (8)
C1—C21.387 (6)C8—H8A0.980
C2—F21.342 (5)C9—C101.455 (10)
C2—C31.365 (7)C9—H9A0.970
C3—F31.346 (5)C9—H9B0.970
C3—C41.376 (7)C10—C111.511 (8)
C4—C51.384 (6)C10—H10A0.970
C4—C71.502 (7)C10—H10B0.970
C5—F51.340 (5)C11—C8i1.376 (8)
C5—C61.374 (6)C11—H11A0.980
C6—F61.343 (5)
C11—Pt1—C881.1 (2)F721—C7—F731103.8 (7)
C11—Pt1—C11i93.3 (3)F711—C7—F731103.9 (7)
C8i—Pt1—C891.4 (3)F732—C7—F712114.8 (14)
C8—Pt1—S1158.78 (16)F732—C7—F722103.3 (11)
C8i—Pt1—S190.04 (15)F712—C7—F722106.4 (12)
C11—Pt1—S187.63 (15)F732—C7—C4115.9 (10)
C11—Pt1—S1i163.48 (17)F712—C7—C4108.8 (10)
S1i—Pt1—S196.15 (5)F721—C7—C4110.6 (6)
C1—S1—Pt1108.63 (13)F711—C7—C4114.0 (7)
C11—Pt1—C8i36.5 (2)F722—C7—C4106.6 (8)
C11i—Pt1—C8i81.1 (2)F731—C7—C4113.4 (5)
C11i—Pt1—C836.5 (2)C11i—C8—C9123.3 (6)
C8—Pt1—S1i90.04 (15)C11i—C8—Pt171.3 (3)
C11i—Pt1—S1i87.63 (15)C9—C8—Pt1110.5 (4)
C8i—Pt1—S1i158.78 (16)C11i—C8—H8A114.6
C11i—Pt1—S1163.48 (17)C9—C8—H8A114.6
C6—C1—C2115.3 (4)Pt1—C8—H8A114.6
C6—C1—S1120.7 (3)C10—C9—C8118.1 (5)
C2—C1—S1124.0 (3)C10—C9—H9A107.8
F2—C2—C3118.1 (4)C8—C9—H9A107.8
F2—C2—C1119.8 (4)C10—C9—H9B107.8
C3—C2—C1122.2 (4)C8—C9—H9B107.8
F3—C3—C2117.4 (4)H9A—C9—H9B107.1
F3—C3—C4120.4 (4)C9—C10—C11116.7 (5)
C2—C3—C4122.2 (4)C9—C10—H10A108.1
C3—C4—C5116.1 (4)C11—C10—H10A108.1
C3—C4—C7123.1 (4)C9—C10—H10B108.1
C5—C4—C7120.8 (5)C11—C10—H10B108.1
F5—C5—C6118.8 (4)H10A—C10—H10B107.3
F5—C5—C4119.9 (4)C8i—C11—C10126.3 (6)
C6—C5—C4121.2 (4)C8i—C11—Pt172.2 (3)
F6—C6—C1119.5 (4)C10—C11—Pt1109.0 (4)
F6—C6—C5117.6 (4)C8i—C11—H11A113.8
C1—C6—C5122.9 (4)C10—C11—H11A113.8
F721—C7—F711110.5 (9)Pt1—C11—H11A113.8
C11—Pt1—S1—C1159.3 (2)C3—C4—C7—F71278 (2)
C11i—Pt1—S1—C165.7 (5)C5—C4—C7—F712103.3 (19)
C8i—Pt1—S1—C1122.8 (2)C3—C4—C7—F721105.6 (10)
C8—Pt1—S1—C1143.1 (4)C5—C4—C7—F72172.8 (10)
S1i—Pt1—S1—C136.84 (14)C3—C4—C7—F71119.6 (11)
Pt1—S1—C1—C6138.8 (3)C5—C4—C7—F711162.0 (10)
Pt1—S1—C1—C243.7 (4)C3—C4—C7—F72236.1 (12)
C6—C1—C2—F2177.5 (4)C5—C4—C7—F722142.3 (11)
S1—C1—C2—F20.1 (6)C3—C4—C7—F731138.2 (6)
C6—C1—C2—C32.7 (7)C5—C4—C7—F73143.3 (8)
S1—C1—C2—C3179.7 (4)C11—Pt1—C8—C11i108.0 (4)
F2—C2—C3—F31.5 (7)C8i—Pt1—C8—C11i72.9 (3)
C1—C2—C3—F3178.3 (4)S1i—Pt1—C8—C11i86.0 (3)
F2—C2—C3—C4180.0 (5)S1—Pt1—C8—C11i166.7 (3)
C1—C2—C3—C40.2 (8)C11—Pt1—C8—C911.4 (5)
F3—C3—C4—C5179.1 (4)C11i—Pt1—C8—C9119.5 (7)
C2—C3—C4—C52.5 (7)C8i—Pt1—C8—C946.6 (5)
F3—C3—C4—C72.4 (8)S1i—Pt1—C8—C9154.6 (5)
C2—C3—C4—C7176.0 (5)S1—Pt1—C8—C947.3 (8)
C3—C4—C5—F5179.4 (5)C11i—C8—C9—C1078.7 (10)
C7—C4—C5—F52.0 (7)Pt1—C8—C9—C101.8 (10)
C3—C4—C5—C62.6 (7)C8—C9—C10—C1115.0 (12)
C7—C4—C5—C6175.9 (4)C9—C10—C11—C8i57.9 (11)
C2—C1—C6—F6178.6 (4)C9—C10—C11—Pt123.5 (10)
S1—C1—C6—F60.9 (6)C11i—Pt1—C11—C8i70.2 (3)
C2—C1—C6—C52.6 (6)C8—Pt1—C11—C8i104.8 (4)
S1—C1—C6—C5179.7 (4)S1i—Pt1—C11—C8i163.0 (4)
F5—C5—C6—F60.8 (7)S1—Pt1—C11—C8i93.3 (3)
C4—C5—C6—F6178.8 (4)C11i—Pt1—C11—C1052.9 (5)
F5—C5—C6—C1178.0 (4)C8i—Pt1—C11—C10123.1 (6)
C4—C5—C6—C10.0 (7)C8—Pt1—C11—C1018.4 (5)
C3—C4—C7—F732150.5 (17)S1i—Pt1—C11—C1039.9 (9)
C5—C4—C7—F73228.0 (17)S1—Pt1—C11—C10143.6 (5)
Symmetry code: (i) x+1, y, z+3/2.
 

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