Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536809053100/ng2700sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536809053100/ng2700Isup2.hkl |
CCDC reference: 766679
Key indicators
- Single-crystal X-ray study
- T = 200 K
- Mean (C-C) = 0.012 Å
- R factor = 0.033
- wR factor = 0.084
- Data-to-parameter ratio = 14.8
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.18 PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 12 PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.596 20 PLAT971_ALERT_2_C Large Calcd. Non-Metal Positive Residual Density 1.80 eA-3 PLAT971_ALERT_2_C Large Calcd. Non-Metal Positive Residual Density 1.67 eA-3
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 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 0 ALERT type 5 Informative message, check
To a solution of K2PtCl4 (0.2011 g, 0.484 mmol) in H2O (20 ml) were added KI (1.6010 g, 9.644 mmol) and 1,10-phenanthroline (0.0967 g, 0.537 mmol), and refluxed for 3 h. The precipitate obtained was separated by filtration, washed with water and acetone, and dried at 100 °C, to give a dark yellow powder (0.2732 g). Crystals suitable for X-ray analysis were obtained by slow evaporation from an N,N-dimethylformamide solution at 50 °C.
H atoms were positioned geometrically and allowed to ride on their respective parent atoms [C—H = 0.95 Å and Uiso(H) = 1.2Ueq(C)]. The maximum and minimum residual electron density peaks of 3.05 and -1.40 e Å-3, respectively, were located 0.97 and 0.92 Å from the Pt Atom.
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2009); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).
Fig. 1. The structure of the title complex, with displacement ellipsoids drawn at the 50% probability level for non-H atoms. | |
Fig. 2. Crystal packing of the title complex. |
[PtI2(C12H8N2)] | F(000) = 1112 |
Mr = 629.09 | Dx = 3.221 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 5463 reflections |
a = 10.3284 (9) Å | θ = 2.3–28.2° |
b = 17.9462 (16) Å | µ = 15.55 mm−1 |
c = 7.3833 (7) Å | T = 200 K |
β = 108.569 (2)° | Needle, yellow |
V = 1297.3 (2) Å3 | 0.32 × 0.13 × 0.08 mm |
Z = 4 |
Bruker SMART 1000 CCD diffractometer | 2284 independent reflections |
Radiation source: fine-focus sealed tube | 2110 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
ϕ and ω scans | θmax = 25.1°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −11→12 |
Tmin = 0.422, Tmax = 1.000 | k = −21→21 |
7331 measured reflections | l = −8→8 |
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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.084 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0524P)2 + 0.9657P] where P = (Fo2 + 2Fc2)/3 |
2284 reflections | (Δ/σ)max < 0.001 |
154 parameters | Δρmax = 3.05 e Å−3 |
0 restraints | Δρmin = −1.40 e Å−3 |
[PtI2(C12H8N2)] | V = 1297.3 (2) Å3 |
Mr = 629.09 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.3284 (9) Å | µ = 15.55 mm−1 |
b = 17.9462 (16) Å | T = 200 K |
c = 7.3833 (7) Å | 0.32 × 0.13 × 0.08 mm |
β = 108.569 (2)° |
Bruker SMART 1000 CCD diffractometer | 2284 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 2110 reflections with I > 2σ(I) |
Tmin = 0.422, Tmax = 1.000 | Rint = 0.033 |
7331 measured reflections |
R[F2 > 2σ(F2)] = 0.033 | 0 restraints |
wR(F2) = 0.084 | H-atom parameters constrained |
S = 1.06 | Δρmax = 3.05 e Å−3 |
2284 reflections | Δρmin = −1.40 e Å−3 |
154 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Pt1 | 0.71220 (3) | 0.337678 (16) | 0.39502 (4) | 0.02011 (13) | |
I1 | 0.74244 (6) | 0.48072 (3) | 0.41617 (8) | 0.03146 (17) | |
I2 | 0.45788 (6) | 0.35783 (3) | 0.20604 (9) | 0.03744 (18) | |
N1 | 0.7037 (6) | 0.2230 (4) | 0.3858 (8) | 0.0245 (15) | |
N2 | 0.9082 (6) | 0.3142 (4) | 0.5563 (9) | 0.0219 (13) | |
C1 | 0.6012 (9) | 0.1789 (5) | 0.2965 (12) | 0.034 (2) | |
H1 | 0.5167 | 0.2005 | 0.2237 | 0.041* | |
C2 | 0.6130 (9) | 0.1009 (5) | 0.3056 (13) | 0.035 (2) | |
H2 | 0.5376 | 0.0709 | 0.2367 | 0.042* | |
C3 | 0.7305 (10) | 0.0681 (6) | 0.4114 (11) | 0.036 (2) | |
H3 | 0.7375 | 0.0153 | 0.4195 | 0.044* | |
C4 | 0.8426 (9) | 0.1132 (4) | 0.5097 (12) | 0.0291 (19) | |
C5 | 0.9726 (10) | 0.0861 (5) | 0.6267 (13) | 0.034 (2) | |
H5 | 0.9862 | 0.0338 | 0.6419 | 0.041* | |
C6 | 1.0755 (9) | 0.1317 (5) | 0.7155 (13) | 0.0317 (19) | |
H6 | 1.1602 | 0.1114 | 0.7921 | 0.038* | |
C7 | 1.0598 (8) | 0.2110 (4) | 0.6964 (11) | 0.0248 (17) | |
C8 | 1.1647 (8) | 0.2622 (5) | 0.7825 (11) | 0.0311 (19) | |
H8 | 1.2519 | 0.2453 | 0.8600 | 0.037* | |
C9 | 1.1388 (9) | 0.3359 (4) | 0.7527 (12) | 0.0300 (19) | |
H9 | 1.2091 | 0.3708 | 0.8101 | 0.036* | |
C10 | 1.0137 (8) | 0.3614 (5) | 0.6417 (11) | 0.0261 (17) | |
H10 | 0.9999 | 0.4135 | 0.6236 | 0.031* | |
C11 | 0.9351 (8) | 0.2394 (4) | 0.5838 (10) | 0.0208 (16) | |
C12 | 0.8236 (8) | 0.1915 (4) | 0.4917 (11) | 0.0233 (17) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.0168 (2) | 0.0209 (2) | 0.0209 (2) | −0.00133 (10) | 0.00349 (14) | −0.00034 (10) |
I1 | 0.0309 (3) | 0.0217 (3) | 0.0393 (3) | 0.0010 (2) | 0.0077 (3) | 0.0001 (2) |
I2 | 0.0184 (3) | 0.0439 (4) | 0.0433 (4) | 0.0001 (2) | 0.0004 (2) | 0.0026 (3) |
N1 | 0.024 (4) | 0.028 (4) | 0.023 (3) | −0.004 (3) | 0.010 (3) | −0.002 (3) |
N2 | 0.018 (4) | 0.025 (3) | 0.022 (3) | 0.001 (3) | 0.006 (3) | 0.001 (3) |
C1 | 0.031 (5) | 0.040 (5) | 0.032 (5) | −0.019 (4) | 0.010 (4) | −0.012 (4) |
C2 | 0.030 (5) | 0.034 (5) | 0.041 (5) | −0.015 (4) | 0.011 (4) | −0.007 (4) |
C3 | 0.059 (7) | 0.026 (5) | 0.031 (5) | −0.006 (4) | 0.025 (5) | −0.005 (3) |
C4 | 0.043 (5) | 0.021 (4) | 0.031 (4) | −0.005 (4) | 0.023 (4) | 0.001 (3) |
C5 | 0.048 (6) | 0.024 (5) | 0.038 (5) | 0.009 (4) | 0.023 (5) | 0.002 (4) |
C6 | 0.028 (5) | 0.032 (5) | 0.038 (5) | 0.003 (4) | 0.014 (4) | 0.004 (4) |
C7 | 0.019 (4) | 0.030 (4) | 0.027 (4) | 0.007 (3) | 0.009 (3) | 0.003 (3) |
C8 | 0.020 (4) | 0.046 (5) | 0.025 (4) | 0.010 (4) | 0.005 (3) | 0.006 (4) |
C9 | 0.026 (5) | 0.033 (5) | 0.025 (4) | −0.005 (3) | 0.000 (4) | −0.001 (3) |
C10 | 0.017 (4) | 0.023 (4) | 0.032 (4) | −0.008 (3) | −0.001 (3) | −0.003 (3) |
C11 | 0.024 (4) | 0.019 (4) | 0.021 (4) | −0.003 (3) | 0.010 (3) | 0.000 (3) |
C12 | 0.033 (5) | 0.021 (4) | 0.022 (4) | −0.001 (3) | 0.016 (4) | 0.003 (3) |
Pt1—N2 | 2.039 (6) | C4—C12 | 1.419 (11) |
Pt1—N1 | 2.060 (7) | C4—C5 | 1.431 (13) |
Pt1—I2 | 2.5774 (7) | C5—C6 | 1.337 (12) |
Pt1—I1 | 2.5847 (6) | C5—H5 | 0.9500 |
N1—C1 | 1.319 (10) | C6—C7 | 1.434 (11) |
N1—C12 | 1.360 (10) | C6—H6 | 0.9500 |
N2—C10 | 1.365 (10) | C7—C11 | 1.389 (11) |
N2—C11 | 1.374 (10) | C7—C8 | 1.407 (12) |
C1—C2 | 1.405 (13) | C8—C9 | 1.354 (12) |
C1—H1 | 0.9500 | C8—H8 | 0.9500 |
C2—C3 | 1.351 (13) | C9—C10 | 1.369 (12) |
C2—H2 | 0.9500 | C9—H9 | 0.9500 |
C3—C4 | 1.410 (12) | C10—H10 | 0.9500 |
C3—H3 | 0.9500 | C11—C12 | 1.423 (11) |
N2—Pt1—N1 | 80.6 (2) | C6—C5—C4 | 122.3 (8) |
N2—Pt1—I2 | 175.02 (17) | C6—C5—H5 | 118.9 |
N1—Pt1—I2 | 95.57 (17) | C4—C5—H5 | 118.9 |
N2—Pt1—I1 | 95.23 (18) | C5—C6—C7 | 120.8 (8) |
N1—Pt1—I1 | 175.72 (17) | C5—C6—H6 | 119.6 |
I2—Pt1—I1 | 88.63 (2) | C7—C6—H6 | 119.6 |
C1—N1—C12 | 118.5 (8) | C11—C7—C8 | 117.7 (7) |
C1—N1—Pt1 | 129.5 (6) | C11—C7—C6 | 118.5 (7) |
C12—N1—Pt1 | 112.1 (5) | C8—C7—C6 | 123.8 (7) |
C10—N2—C11 | 116.4 (7) | C9—C8—C7 | 118.7 (8) |
C10—N2—Pt1 | 129.8 (5) | C9—C8—H8 | 120.6 |
C11—N2—Pt1 | 113.8 (5) | C7—C8—H8 | 120.6 |
N1—C1—C2 | 122.1 (9) | C8—C9—C10 | 121.5 (8) |
N1—C1—H1 | 119.0 | C8—C9—H9 | 119.2 |
C2—C1—H1 | 119.0 | C10—C9—H9 | 119.2 |
C3—C2—C1 | 120.6 (8) | N2—C10—C9 | 122.1 (8) |
C3—C2—H2 | 119.7 | N2—C10—H10 | 118.9 |
C1—C2—H2 | 119.7 | C9—C10—H10 | 118.9 |
C2—C3—C4 | 119.2 (9) | N2—C11—C7 | 123.5 (7) |
C2—C3—H3 | 120.4 | N2—C11—C12 | 115.2 (7) |
C4—C3—H3 | 120.4 | C7—C11—C12 | 121.3 (7) |
C3—C4—C12 | 117.0 (8) | N1—C12—C4 | 122.6 (7) |
C3—C4—C5 | 125.0 (8) | N1—C12—C11 | 118.2 (7) |
C12—C4—C5 | 117.9 (7) | C4—C12—C11 | 119.1 (7) |
N2—Pt1—N1—C1 | −178.5 (7) | Pt1—N2—C10—C9 | 177.2 (6) |
I2—Pt1—N1—C1 | 4.8 (7) | C8—C9—C10—N2 | 0.4 (13) |
N2—Pt1—N1—C12 | 2.5 (5) | C10—N2—C11—C7 | 2.1 (10) |
I2—Pt1—N1—C12 | −174.3 (4) | Pt1—N2—C11—C7 | −176.9 (6) |
N1—Pt1—N2—C10 | 179.0 (7) | C10—N2—C11—C12 | −179.5 (6) |
I1—Pt1—N2—C10 | 0.1 (7) | Pt1—N2—C11—C12 | 1.6 (8) |
N1—Pt1—N2—C11 | −2.2 (5) | C8—C7—C11—N2 | −1.6 (11) |
I1—Pt1—N2—C11 | 178.8 (4) | C6—C7—C11—N2 | 179.6 (7) |
C12—N1—C1—C2 | −0.9 (11) | C8—C7—C11—C12 | −179.9 (7) |
Pt1—N1—C1—C2 | −179.9 (6) | C6—C7—C11—C12 | 1.2 (10) |
N1—C1—C2—C3 | 1.6 (12) | C1—N1—C12—C4 | 0.0 (10) |
C1—C2—C3—C4 | −1.4 (12) | Pt1—N1—C12—C4 | 179.2 (5) |
C2—C3—C4—C12 | 0.5 (11) | C1—N1—C12—C11 | 178.4 (7) |
C2—C3—C4—C5 | 179.9 (8) | Pt1—N1—C12—C11 | −2.4 (8) |
C3—C4—C5—C6 | 179.5 (7) | C3—C4—C12—N1 | 0.2 (10) |
C12—C4—C5—C6 | −1.1 (12) | C5—C4—C12—N1 | −179.3 (7) |
C4—C5—C6—C7 | −0.2 (12) | C3—C4—C12—C11 | −178.2 (7) |
C5—C6—C7—C11 | 0.1 (11) | C5—C4—C12—C11 | 2.4 (10) |
C5—C6—C7—C8 | −178.6 (8) | N2—C11—C12—N1 | 0.6 (10) |
C11—C7—C8—C9 | 0.4 (11) | C7—C11—C12—N1 | 179.1 (6) |
C6—C7—C8—C9 | 179.2 (7) | N2—C11—C12—C4 | 179.0 (6) |
C7—C8—C9—C10 | 0.1 (12) | C7—C11—C12—C4 | −2.5 (10) |
C11—N2—C10—C9 | −1.5 (11) |
Experimental details
Crystal data | |
Chemical formula | [PtI2(C12H8N2)] |
Mr | 629.09 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 200 |
a, b, c (Å) | 10.3284 (9), 17.9462 (16), 7.3833 (7) |
β (°) | 108.569 (2) |
V (Å3) | 1297.3 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 15.55 |
Crystal size (mm) | 0.32 × 0.13 × 0.08 |
Data collection | |
Diffractometer | Bruker SMART 1000 CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2000) |
Tmin, Tmax | 0.422, 1.000 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7331, 2284, 2110 |
Rint | 0.033 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.033, 0.084, 1.06 |
No. of reflections | 2284 |
No. of parameters | 154 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 3.05, −1.40 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2009).
Pt1—N2 | 2.039 (6) | Pt1—I2 | 2.5774 (7) |
Pt1—N1 | 2.060 (7) | Pt1—I1 | 2.5847 (6) |
N2—Pt1—N1 | 80.6 (2) |
The title complex, [PtI2(phen)] (where phen is 1,10-phenanthroline, C12H8N2), is isomorphous with the yellow form of [PtCl2(phen)], whereas the orange form of [PtCl2(phen)] crystallized in the orthorhombic space group Pca21 (Grzesiak & Matzger, 2007).
In the title complex, the Pt2+ ion is four-coordinated in a slightly distorted square-planar environment by two N atoms of the chelating 1,10-phenanthroline ligand and two iodide ions (Fig. 1). The main contribution to the distortion is the tight N1—Pt1—N2 chelate angle [80.6 (2)°], which results in non-linear trans arrangement [<N1—Pt1—I1 = 175.72 (17)° and <N2—Pt1—I2 = 175.02 (17)°]. The Pt1—N and Pt1—I bond lengths are almost equal, respectively [Pt1—N: 2.060 (7) and 2.039 (6) Å; Pt1—I 2.5847 (6) and 2.5774 (7) Å] (Table 1). The complex displays numerous intermolecular π-π interactions between adjacent six-membered rings, with a shortest centroid-centroid distance of 3.703 (5) Å and the dihedral angle between the ring planes is 3.4 (4)°. The nearly planar [PtI2(phen)] molecules, with a largest deviation of 0.170 (3) Å from the least-squares plane, stack in columns along the c axis with a Pt···Pt distance of 4.8510 (6) Å (Fig. 2).