metal-organic compounds
Bis(2,2′-bipyridine-κ2N,N′)dichloridoplatinum(IV) dichloride monohydrate
aSchool of Applied Chemical Engineering, The Research Institute of Catalysis, Chonnam National University, Gwangju 500-757, Republic of Korea, and bDepartment of Chemistry, Pohang University of Science and Technology, Pohang 790-784, Republic of Korea
*Correspondence e-mail: hakwang@chonnam.ac.kr
In the title complex, [PtCl2(C10H8N2)2]Cl2·H2O, the Pt4+ ion is six-coordinated in a distorted octahedral environment by four N atoms from the two 2,2′-bipyridine ligands and two Cl atoms. As a result of the different trans influences of the N and Cl atoms, the Pt—N bonds trans to the Cl atom are slightly longer than those trans to the N atom. The compound displays intermolecular hydrogen bonding between the water molecule and the Cl anions. There are intermolecular π–π interactions between adjacent pyridine rings, with a centroid–centroid distance of 3.962 Å.
Experimental
Crystal data
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Data collection: SMART (Bruker, 2000); cell SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
Supporting information
10.1107/S1600536809000725/bt2846sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536809000725/bt2846Isup2.hkl
To a solution of K2PtCl6 (0.3068 g, 0.631 mmol) in H2O (20 ml) was added 2,2'-bipyridine (0.0971 g, 0.622 mmol) in MeOH (10 ml), and stirred for 2 h under heating. The formed precipitate was separated by filtration and washed with water and MeOH and dried under vacuum, to give a yellow powder (0.1185 g). Crystals suitable for X-ray analysis were obtained by slow evaporation from a CH2Cl2 solution.
H atoms were positioned geometrically and allowed to ride on their respective parent atoms [C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C)]. The H atoms of the solvent H2O molecule were located from Fourier difference maps, but not refined.
Data collection: SMART (Bruker, 2000); cell
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); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).Fig. 1. The structure of the title compound, with displacement ellipsoids drawn at the 50% probability level for non-H atoms. |
[PtCl2(C10H8N2)2]Cl2·H2O | F(000) = 1280 |
Mr = 667.27 | Dx = 2.011 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 958 reflections |
a = 11.1345 (12) Å | θ = 2.4–26.4° |
b = 11.5867 (12) Å | µ = 6.87 mm−1 |
c = 17.0873 (19) Å | T = 293 K |
V = 2204.5 (4) Å3 | Stick, colorless |
Z = 4 | 0.35 × 0.20 × 0.15 mm |
Bruker SMART 1000 CCD diffractometer | 4462 independent reflections |
Radiation source: fine-focus sealed tube | 4284 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
ϕ and ω scans | θmax = 26.4°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −12→13 |
Tmin = 0.251, Tmax = 0.357 | k = −14→14 |
12649 measured reflections | l = −21→16 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.016 | H-atom parameters constrained |
wR(F2) = 0.038 | w = 1/[σ2(Fo2)] where P = (Fo2 + 2Fc2)/3 |
S = 0.84 | (Δ/σ)max = 0.003 |
4462 reflections | Δρmax = 0.95 e Å−3 |
271 parameters | Δρmin = −0.53 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 1901 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.006 (4) |
[PtCl2(C10H8N2)2]Cl2·H2O | V = 2204.5 (4) Å3 |
Mr = 667.27 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 11.1345 (12) Å | µ = 6.87 mm−1 |
b = 11.5867 (12) Å | T = 293 K |
c = 17.0873 (19) Å | 0.35 × 0.20 × 0.15 mm |
Bruker SMART 1000 CCD diffractometer | 4462 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 4284 reflections with I > 2σ(I) |
Tmin = 0.251, Tmax = 0.357 | Rint = 0.017 |
12649 measured reflections |
R[F2 > 2σ(F2)] = 0.016 | H-atom parameters constrained |
wR(F2) = 0.038 | Δρmax = 0.95 e Å−3 |
S = 0.84 | Δρmin = −0.53 e Å−3 |
4462 reflections | Absolute structure: Flack (1983), 1901 Friedel pairs |
271 parameters | Absolute structure parameter: −0.006 (4) |
0 restraints |
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 | 0.520023 (9) | 0.241999 (9) | 0.124231 (6) | 0.02622 (4) | |
Cl1 | 0.35373 (7) | 0.12668 (7) | 0.10471 (5) | 0.0410 (2) | |
Cl2 | 0.40172 (7) | 0.40216 (7) | 0.14570 (5) | 0.0394 (2) | |
Cl3 | 0.36627 (9) | 0.07710 (8) | 0.54638 (6) | 0.0517 (2) | |
Cl4 | 0.15636 (8) | 0.59942 (8) | 0.20502 (5) | 0.0421 (2) | |
N1 | 0.6674 (2) | 0.3407 (2) | 0.14792 (15) | 0.0272 (6) | |
N2 | 0.5239 (2) | 0.2274 (2) | 0.24255 (14) | 0.0290 (5) | |
N3 | 0.5272 (2) | 0.2554 (2) | 0.00599 (14) | 0.0288 (5) | |
N4 | 0.6210 (2) | 0.1002 (2) | 0.09926 (15) | 0.0309 (6) | |
C1 | 0.7301 (3) | 0.3999 (3) | 0.0943 (2) | 0.0340 (7) | |
H1 | 0.7110 | 0.3925 | 0.0416 | 0.041* | |
C2 | 0.8225 (3) | 0.4716 (3) | 0.1167 (2) | 0.0389 (8) | |
H2 | 0.8644 | 0.5140 | 0.0794 | 0.047* | |
C3 | 0.8524 (3) | 0.4801 (3) | 0.1945 (2) | 0.0413 (8) | |
H3 | 0.9159 | 0.5270 | 0.2099 | 0.050* | |
C4 | 0.7876 (3) | 0.4185 (3) | 0.2500 (2) | 0.0364 (8) | |
H4 | 0.8078 | 0.4227 | 0.3027 | 0.044* | |
C5 | 0.6933 (3) | 0.3516 (3) | 0.22561 (18) | 0.0284 (7) | |
C6 | 0.6124 (3) | 0.2891 (3) | 0.27847 (18) | 0.0282 (7) | |
C7 | 0.6188 (3) | 0.2940 (3) | 0.35849 (19) | 0.0391 (8) | |
H7 | 0.6792 | 0.3364 | 0.3827 | 0.047* | |
C8 | 0.5347 (3) | 0.2355 (3) | 0.4032 (2) | 0.0415 (8) | |
H8 | 0.5378 | 0.2380 | 0.4575 | 0.050* | |
C9 | 0.4458 (3) | 0.1728 (3) | 0.3651 (2) | 0.0452 (9) | |
H9 | 0.3886 | 0.1327 | 0.3940 | 0.054* | |
C10 | 0.4424 (3) | 0.1702 (3) | 0.2852 (2) | 0.0399 (8) | |
H10 | 0.3827 | 0.1281 | 0.2601 | 0.048* | |
C11 | 0.4779 (3) | 0.3413 (3) | −0.0360 (2) | 0.0386 (8) | |
H11 | 0.4407 | 0.4024 | −0.0103 | 0.046* | |
C12 | 0.4818 (3) | 0.3402 (3) | −0.1165 (2) | 0.0453 (9) | |
H12 | 0.4465 | 0.3996 | −0.1450 | 0.054* | |
C13 | 0.5380 (3) | 0.2508 (3) | −0.15455 (19) | 0.0413 (8) | |
H13 | 0.5409 | 0.2489 | −0.2089 | 0.050* | |
C14 | 0.5907 (3) | 0.1629 (3) | −0.11082 (19) | 0.0371 (8) | |
H14 | 0.6302 | 0.1024 | −0.1356 | 0.045* | |
C15 | 0.5836 (3) | 0.1666 (3) | −0.03080 (19) | 0.0294 (7) | |
C16 | 0.6334 (3) | 0.0775 (3) | 0.02149 (18) | 0.0299 (7) | |
C17 | 0.6884 (3) | −0.0219 (3) | −0.0035 (2) | 0.0404 (8) | |
H17 | 0.6942 | −0.0385 | −0.0566 | 0.048* | |
C18 | 0.7351 (3) | −0.0971 (3) | 0.0517 (2) | 0.0444 (9) | |
H18 | 0.7734 | −0.1644 | 0.0357 | 0.053* | |
C19 | 0.7249 (3) | −0.0725 (3) | 0.1296 (2) | 0.0435 (8) | |
H19 | 0.7567 | −0.1223 | 0.1669 | 0.052* | |
C20 | 0.6665 (3) | 0.0280 (3) | 0.1524 (2) | 0.0366 (8) | |
H20 | 0.6589 | 0.0451 | 0.2054 | 0.044* | |
O1 | 0.0454 (3) | 0.2475 (2) | 0.37482 (18) | 0.0807 (11) | |
H1A | 0.0141 | 0.3103 | 0.4125 | 0.080* | |
H1B | −0.0004 | 0.1831 | 0.3636 | 0.080* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.02736 (6) | 0.02822 (6) | 0.02310 (6) | −0.00141 (5) | −0.00187 (4) | 0.00024 (5) |
Cl1 | 0.0367 (4) | 0.0447 (5) | 0.0416 (5) | −0.0117 (4) | −0.0046 (3) | −0.0014 (4) |
Cl2 | 0.0400 (4) | 0.0375 (4) | 0.0408 (5) | 0.0082 (4) | −0.0011 (3) | −0.0036 (3) |
Cl3 | 0.0656 (6) | 0.0536 (6) | 0.0360 (5) | −0.0087 (5) | 0.0145 (4) | −0.0081 (4) |
Cl4 | 0.0430 (5) | 0.0454 (5) | 0.0379 (5) | 0.0001 (4) | −0.0017 (4) | −0.0040 (4) |
N1 | 0.0243 (13) | 0.0257 (13) | 0.0314 (16) | −0.0014 (10) | −0.0031 (11) | 0.0011 (10) |
N2 | 0.0319 (13) | 0.0301 (13) | 0.0251 (13) | −0.0025 (14) | 0.0013 (10) | 0.0010 (10) |
N3 | 0.0294 (13) | 0.0332 (13) | 0.0238 (12) | 0.0022 (16) | −0.0056 (9) | 0.0013 (10) |
N4 | 0.0294 (14) | 0.0309 (14) | 0.0325 (15) | −0.0022 (11) | −0.0021 (11) | −0.0006 (11) |
C1 | 0.0361 (18) | 0.0362 (18) | 0.0297 (18) | 0.0021 (15) | 0.0030 (14) | 0.0024 (14) |
C2 | 0.0323 (17) | 0.0387 (18) | 0.046 (2) | −0.0046 (13) | 0.0074 (17) | 0.0082 (17) |
C3 | 0.0320 (18) | 0.0377 (19) | 0.054 (2) | −0.0076 (15) | −0.0029 (16) | −0.0009 (16) |
C4 | 0.0338 (18) | 0.042 (2) | 0.033 (2) | −0.0010 (15) | −0.0042 (14) | −0.0032 (15) |
C5 | 0.0288 (16) | 0.0294 (16) | 0.0271 (17) | 0.0042 (13) | −0.0025 (13) | 0.0009 (13) |
C6 | 0.0277 (16) | 0.0301 (15) | 0.0269 (16) | 0.0028 (12) | −0.0013 (12) | −0.0002 (12) |
C7 | 0.0398 (19) | 0.0493 (19) | 0.0281 (19) | −0.0004 (15) | −0.0020 (14) | −0.0022 (15) |
C8 | 0.050 (2) | 0.050 (2) | 0.0240 (16) | 0.003 (2) | 0.0016 (13) | 0.0056 (14) |
C9 | 0.058 (2) | 0.0409 (19) | 0.037 (2) | −0.0088 (16) | 0.0134 (18) | 0.0074 (16) |
C10 | 0.047 (2) | 0.0370 (18) | 0.035 (2) | −0.0099 (16) | 0.0033 (16) | 0.0032 (14) |
C11 | 0.044 (2) | 0.0380 (17) | 0.0336 (19) | 0.0054 (17) | −0.0062 (16) | 0.0047 (14) |
C12 | 0.051 (2) | 0.0494 (19) | 0.035 (2) | 0.0019 (17) | −0.0079 (18) | 0.0104 (16) |
C13 | 0.0481 (19) | 0.052 (2) | 0.0233 (15) | 0.000 (3) | −0.0028 (13) | 0.0036 (15) |
C14 | 0.0406 (19) | 0.0441 (18) | 0.0267 (19) | −0.0010 (15) | 0.0029 (15) | −0.0038 (14) |
C15 | 0.0268 (16) | 0.0338 (17) | 0.0277 (17) | −0.0020 (13) | −0.0035 (13) | 0.0011 (13) |
C16 | 0.0288 (17) | 0.0327 (17) | 0.0283 (18) | −0.0023 (13) | −0.0017 (13) | −0.0008 (13) |
C17 | 0.045 (2) | 0.039 (2) | 0.037 (2) | 0.0053 (17) | 0.0047 (15) | −0.0058 (15) |
C18 | 0.044 (2) | 0.038 (2) | 0.051 (3) | 0.0120 (17) | 0.0043 (17) | −0.0011 (17) |
C19 | 0.0421 (19) | 0.0395 (18) | 0.049 (2) | 0.0079 (15) | −0.0068 (18) | 0.0024 (19) |
C20 | 0.0423 (19) | 0.0386 (18) | 0.0287 (18) | −0.0012 (15) | −0.0087 (15) | 0.0029 (14) |
O1 | 0.0528 (17) | 0.084 (2) | 0.106 (3) | −0.0042 (15) | −0.0045 (15) | −0.043 (2) |
Pt1—N3 | 2.028 (2) | C7—H7 | 0.9300 |
Pt1—N2 | 2.029 (2) | C8—C9 | 1.389 (5) |
Pt1—N4 | 2.037 (3) | C8—H8 | 0.9300 |
Pt1—N1 | 2.040 (2) | C9—C10 | 1.366 (5) |
Pt1—Cl2 | 2.3051 (8) | C9—H9 | 0.9300 |
Pt1—Cl1 | 2.3076 (8) | C10—H10 | 0.9300 |
N1—C1 | 1.341 (4) | C11—C12 | 1.377 (5) |
N1—C5 | 1.364 (4) | C11—H11 | 0.9300 |
N2—C10 | 1.339 (4) | C12—C13 | 1.375 (5) |
N2—C6 | 1.364 (4) | C12—H12 | 0.9300 |
N3—C11 | 1.344 (4) | C13—C14 | 1.393 (5) |
N3—C15 | 1.360 (4) | C13—H13 | 0.9300 |
N4—C20 | 1.335 (4) | C14—C15 | 1.370 (4) |
N4—C16 | 1.361 (4) | C14—H14 | 0.9300 |
C1—C2 | 1.377 (4) | C15—C16 | 1.474 (4) |
C1—H1 | 0.9300 | C16—C17 | 1.373 (4) |
C2—C3 | 1.373 (5) | C17—C18 | 1.385 (5) |
C2—H2 | 0.9300 | C17—H17 | 0.9300 |
C3—C4 | 1.389 (5) | C18—C19 | 1.367 (5) |
C3—H3 | 0.9300 | C18—H18 | 0.9300 |
C4—C5 | 1.370 (4) | C19—C20 | 1.389 (4) |
C4—H4 | 0.9300 | C19—H19 | 0.9300 |
C5—C6 | 1.467 (4) | C20—H20 | 0.9300 |
C6—C7 | 1.370 (4) | O1—H1A | 1.033 |
C7—C8 | 1.385 (5) | O1—H1B | 0.924 |
N3—Pt1—N2 | 176.52 (10) | C7—C6—C5 | 124.2 (3) |
N3—Pt1—N4 | 80.30 (10) | C6—C7—C8 | 119.6 (3) |
N2—Pt1—N4 | 97.47 (10) | C6—C7—H7 | 120.2 |
N3—Pt1—N1 | 97.07 (10) | C8—C7—H7 | 120.2 |
N2—Pt1—N1 | 80.33 (10) | C7—C8—C9 | 118.7 (3) |
N4—Pt1—N1 | 92.84 (9) | C7—C8—H8 | 120.7 |
N3—Pt1—Cl2 | 96.85 (7) | C9—C8—H8 | 120.7 |
N2—Pt1—Cl2 | 85.44 (7) | C10—C9—C8 | 119.9 (3) |
N4—Pt1—Cl2 | 176.91 (7) | C10—C9—H9 | 120.1 |
N1—Pt1—Cl2 | 88.68 (7) | C8—C9—H9 | 120.1 |
N3—Pt1—Cl1 | 86.10 (7) | N2—C10—C9 | 121.0 (3) |
N2—Pt1—Cl1 | 96.47 (7) | N2—C10—H10 | 119.5 |
N4—Pt1—Cl1 | 86.88 (7) | C9—C10—H10 | 119.5 |
N1—Pt1—Cl1 | 176.73 (7) | N3—C11—C12 | 120.9 (3) |
Cl2—Pt1—Cl1 | 91.76 (3) | N3—C11—H11 | 119.5 |
C1—N1—C5 | 120.5 (3) | C12—C11—H11 | 119.5 |
C1—N1—Pt1 | 124.8 (2) | C13—C12—C11 | 119.6 (3) |
C5—N1—Pt1 | 114.53 (19) | C13—C12—H12 | 120.2 |
C10—N2—C6 | 120.3 (3) | C11—C12—H12 | 120.2 |
C10—N2—Pt1 | 124.7 (2) | C12—C13—C14 | 119.3 (3) |
C6—N2—Pt1 | 114.83 (19) | C12—C13—H13 | 120.3 |
C11—N3—C15 | 120.2 (3) | C14—C13—H13 | 120.3 |
C11—N3—Pt1 | 124.9 (2) | C15—C14—C13 | 119.2 (3) |
C15—N3—Pt1 | 114.88 (19) | C15—C14—H14 | 120.4 |
C20—N4—C16 | 120.3 (3) | C13—C14—H14 | 120.4 |
C20—N4—Pt1 | 124.9 (2) | N3—C15—C14 | 120.8 (3) |
C16—N4—Pt1 | 114.6 (2) | N3—C15—C16 | 115.1 (3) |
N1—C1—C2 | 120.6 (3) | C14—C15—C16 | 124.1 (3) |
N1—C1—H1 | 119.7 | N4—C16—C17 | 120.7 (3) |
C2—C1—H1 | 119.7 | N4—C16—C15 | 114.8 (3) |
C3—C2—C1 | 119.5 (3) | C17—C16—C15 | 124.5 (3) |
C3—C2—H2 | 120.2 | C16—C17—C18 | 118.9 (3) |
C1—C2—H2 | 120.2 | C16—C17—H17 | 120.6 |
C2—C3—C4 | 119.9 (3) | C18—C17—H17 | 120.6 |
C2—C3—H3 | 120.0 | C19—C18—C17 | 120.1 (3) |
C4—C3—H3 | 120.0 | C19—C18—H18 | 119.9 |
C5—C4—C3 | 118.7 (3) | C17—C18—H18 | 119.9 |
C5—C4—H4 | 120.6 | C18—C19—C20 | 119.1 (3) |
C3—C4—H4 | 120.6 | C18—C19—H19 | 120.4 |
N1—C5—C4 | 120.7 (3) | C20—C19—H19 | 120.4 |
N1—C5—C6 | 115.0 (3) | N4—C20—C19 | 120.8 (3) |
C4—C5—C6 | 124.2 (3) | N4—C20—H20 | 119.6 |
N2—C6—C7 | 120.6 (3) | C19—C20—H20 | 119.6 |
N2—C6—C5 | 115.2 (3) | H1A—O1—H1B | 120.8 |
N3—Pt1—N1—C1 | 6.2 (3) | C3—C4—C5—C6 | −175.4 (3) |
N2—Pt1—N1—C1 | −176.1 (3) | C10—N2—C6—C7 | −0.4 (4) |
N4—Pt1—N1—C1 | 86.8 (3) | Pt1—N2—C6—C7 | 174.8 (2) |
Cl2—Pt1—N1—C1 | −90.5 (2) | C10—N2—C6—C5 | −177.7 (3) |
N3—Pt1—N1—C5 | −179.5 (2) | Pt1—N2—C6—C5 | −2.6 (3) |
N2—Pt1—N1—C5 | −1.9 (2) | N1—C5—C6—N2 | 1.0 (4) |
N4—Pt1—N1—C5 | −99.0 (2) | C4—C5—C6—N2 | 179.9 (3) |
Cl2—Pt1—N1—C5 | 83.7 (2) | N1—C5—C6—C7 | −176.2 (3) |
N4—Pt1—N2—C10 | −91.0 (3) | C4—C5—C6—C7 | 2.7 (5) |
N1—Pt1—N2—C10 | 177.4 (3) | N2—C6—C7—C8 | 0.2 (5) |
Cl2—Pt1—N2—C10 | 87.9 (2) | C5—C6—C7—C8 | 177.3 (3) |
Cl1—Pt1—N2—C10 | −3.3 (3) | C6—C7—C8—C9 | 0.1 (5) |
N4—Pt1—N2—C6 | 94.0 (2) | C7—C8—C9—C10 | −0.2 (5) |
N1—Pt1—N2—C6 | 2.4 (2) | C6—N2—C10—C9 | 0.3 (5) |
Cl2—Pt1—N2—C6 | −87.0 (2) | Pt1—N2—C10—C9 | −174.4 (3) |
Cl1—Pt1—N2—C6 | −178.28 (19) | C8—C9—C10—N2 | 0.0 (5) |
N4—Pt1—N3—C11 | −178.1 (3) | C15—N3—C11—C12 | 1.1 (5) |
N1—Pt1—N3—C11 | −86.4 (3) | Pt1—N3—C11—C12 | −176.5 (2) |
Cl2—Pt1—N3—C11 | 3.1 (2) | N3—C11—C12—C13 | −0.8 (5) |
Cl1—Pt1—N3—C11 | 94.4 (2) | C11—C12—C13—C14 | −0.3 (5) |
N4—Pt1—N3—C15 | 4.2 (2) | C12—C13—C14—C15 | 1.0 (5) |
N1—Pt1—N3—C15 | 95.9 (2) | C11—N3—C15—C14 | −0.3 (4) |
Cl2—Pt1—N3—C15 | −174.61 (19) | Pt1—N3—C15—C14 | 177.5 (2) |
Cl1—Pt1—N3—C15 | −83.3 (2) | C11—N3—C15—C16 | −179.7 (3) |
N3—Pt1—N4—C20 | 178.5 (3) | Pt1—N3—C15—C16 | −1.8 (3) |
N2—Pt1—N4—C20 | 1.2 (3) | C13—C14—C15—N3 | −0.7 (5) |
N1—Pt1—N4—C20 | 81.8 (3) | C13—C14—C15—C16 | 178.6 (3) |
Cl1—Pt1—N4—C20 | −94.9 (3) | C20—N4—C16—C17 | 2.6 (5) |
N3—Pt1—N4—C16 | −6.0 (2) | Pt1—N4—C16—C17 | −173.2 (2) |
N2—Pt1—N4—C16 | 176.7 (2) | C20—N4—C16—C15 | −177.5 (3) |
N1—Pt1—N4—C16 | −102.7 (2) | Pt1—N4—C16—C15 | 6.8 (3) |
Cl1—Pt1—N4—C16 | 80.5 (2) | N3—C15—C16—N4 | −3.3 (4) |
C5—N1—C1—C2 | 0.8 (5) | C14—C15—C16—N4 | 177.4 (3) |
Pt1—N1—C1—C2 | 174.7 (2) | N3—C15—C16—C17 | 176.6 (3) |
N1—C1—C2—C3 | 1.6 (5) | C14—C15—C16—C17 | −2.7 (5) |
C1—C2—C3—C4 | −1.5 (5) | N4—C16—C17—C18 | −2.3 (5) |
C2—C3—C4—C5 | −1.0 (5) | C15—C16—C17—C18 | 177.8 (3) |
C1—N1—C5—C4 | −3.4 (4) | C16—C17—C18—C19 | 0.7 (5) |
Pt1—N1—C5—C4 | −177.9 (2) | C17—C18—C19—C20 | 0.6 (5) |
C1—N1—C5—C6 | 175.6 (3) | C16—N4—C20—C19 | −1.3 (5) |
Pt1—N1—C5—C6 | 1.1 (3) | Pt1—N4—C20—C19 | 174.0 (2) |
C3—C4—C5—N1 | 3.4 (5) | C18—C19—C20—N4 | −0.3 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···Cl3i | 1.033 | 2.21 | 3.150 (3) | 149.79 (16) |
O1—H1B···Cl4ii | 0.924 | 2.31 | 3.139 (3) | 149.3 (2) |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1; (ii) −x, y−1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [PtCl2(C10H8N2)2]Cl2·H2O |
Mr | 667.27 |
Crystal system, space group | Orthorhombic, P212121 |
Temperature (K) | 293 |
a, b, c (Å) | 11.1345 (12), 11.5867 (12), 17.0873 (19) |
V (Å3) | 2204.5 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 6.87 |
Crystal size (mm) | 0.35 × 0.20 × 0.15 |
Data collection | |
Diffractometer | Bruker SMART 1000 CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2000) |
Tmin, Tmax | 0.251, 0.357 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12649, 4462, 4284 |
Rint | 0.017 |
(sin θ/λ)max (Å−1) | 0.625 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.016, 0.038, 0.84 |
No. of reflections | 4462 |
No. of parameters | 271 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.95, −0.53 |
Absolute structure | Flack (1983), 1901 Friedel pairs |
Absolute structure parameter | −0.006 (4) |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997).
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···Cl3i | 1.033 | 2.21 | 3.150 (3) | 149.79 (16) |
O1—H1B···Cl4ii | 0.924 | 2.31 | 3.139 (3) | 149.3 (2) |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1; (ii) −x, y−1/2, −z+1/2. |
Acknowledgements
This work was supported by the Korea Research Foundation (2006–353-C00028).
References
Bruker (2000). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. CrossRef IUCr Journals Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Hambley, T. W. (1986). Acta Cryst. C42, 49–51. CSD CrossRef CAS Web of Science IUCr Journals Google Scholar
Hojjat Kashani, L., Amani, V., Yousefi, M. & Khavasi, H. R. (2008). Acta Cryst. E64, m905–m906. Web of Science CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
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In the title complex, [PtCl2(C10H8N2)2]Cl2.H2O, the central Pt4+ ion is six-coordinated in a distorted octahedral environment by four N atoms from the two 2,2'-bipyridine ligands and two Cl atoms (Fig. 1). The main contributions to the distortion are the tight N—Pt—N chelate angles (80.33 (10)° and 80.30 (10)°), which result in non-linear trans axes (<Cl1—Pt1—N1 = 176.73 (7)°, <Cl2—Pt1—N4 = 176.91 (7)° and <N2—Pt1—N3 = 176.52 (10)°).
Because of the different trans influences of the N and Cl atoms, the Pt—N bonds trans to the Cl atom (lengths: 2.040 (2) and 2.037 (3) Å) are slightly longer than those trans to the N atom (lengths: 2.029 (2) and 2.028 (2) Å).
The compound displays intermolecular hydrogen bonding between the solvent H2O molecule and the Cl anions (Table 1). There is also an intermolecular π-π interaction between the pyridine ring containing N1 and the one containg N3 at 1/2+x,1/2-y,-z, with a centroid-centroid distance of 3.962 Å and with a dihedral angle between the ring planes of 20.3°.