Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801006997/ci6023sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801006997/ci6023Isup2.hkl |
CCDC reference: 165635
The title complex was obtained from the reaction of Ru(PPh3)3Cl2 and 3,5-Me2pz (molar ratio 1:2) in tetrahydrofuran (THF) (Stephenson & Wilkinson, 1966). To a solution of Ru(PPh3)3Cl2 (0.104 mmol) in THF (15 ml) was added 3,5-Me2pz (0.21 mmol). The mixture was stirred for 2 h and then the solvent was pumped off and the residue washed with hexane. Red crystals suitable for X-ray data collection were obtained by recrystallization from dichloromethane/hexane at room temperature.
After checking their presence in the difference map, all H atoms were geometrically fixed and allowed to ride on their attached atoms with Uiso = 1.2Ueq for the attached atoms and Uiso = 1.5Ueq for methyl H atoms. The highest peak in the difference Fourier map lies close to the Ru atom (0.97 Å)
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and PLATON (Spek, 1990).
Fig. 1. The structure of the title complex showing 50% probability displacement ellipsoids and the atom-numbering scheme. |
[RuCl2(C5H7N2)2(C18H15P)2] | F(000) = 912 |
Mr = 886.76 | Dx = 1.407 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 11.6466 (2) Å | Cell parameters from 8192 reflections |
b = 17.1438 (3) Å | θ = 3.0–28.4° |
c = 10.5361 (2) Å | µ = 0.62 mm−1 |
β = 95.603 (1)° | T = 293 K |
V = 2093.66 (6) Å3 | Slab, red |
Z = 2 | 0.28 × 0.26 × 0.20 mm |
Siemens SMART CCD area-detector diffractometer | 5169 independent reflections |
Radiation source: fine-focus sealed tube | 3919 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.052 |
Detector resolution: 8.33 pixels mm-1 | θmax = 28.3°, θmin = 3.0° |
ω scans | h = −15→15 |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | k = 0→22 |
Tmin = 0.846, Tmax = 0.887 | l = 0→14 |
14880 measured reflections |
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)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.109 | H-atom parameters constrained |
S = 0.99 | w = 1/[σ2(Fo2) + (0.0562P)2] where P = (Fo2 + 2Fc2)/3 |
5169 reflections | (Δ/σ)max = 0.023 |
252 parameters | Δρmax = 1.06 e Å−3 |
0 restraints | Δρmin = −0.91 e Å−3 |
[RuCl2(C5H7N2)2(C18H15P)2] | V = 2093.66 (6) Å3 |
Mr = 886.76 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.6466 (2) Å | µ = 0.62 mm−1 |
b = 17.1438 (3) Å | T = 293 K |
c = 10.5361 (2) Å | 0.28 × 0.26 × 0.20 mm |
β = 95.603 (1)° |
Siemens SMART CCD area-detector diffractometer | 5169 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 3919 reflections with I > 2σ(I) |
Tmin = 0.846, Tmax = 0.887 | Rint = 0.052 |
14880 measured reflections |
R[F2 > 2σ(F2)] = 0.039 | 0 restraints |
wR(F2) = 0.109 | H-atom parameters constrained |
S = 0.99 | Δρmax = 1.06 e Å−3 |
5169 reflections | Δρmin = −0.91 e Å−3 |
252 parameters |
Experimental. The data collection covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different ϕ angle (0,88 and 180°) for the crystal and each exposure of 30 s covered 0.3° in ω. The crystal-to-detector distance was 4.023 cm and the detector swing angle was -35°. Coverage of the unit set is 99.3% complete. Crystal decay was monitored by SAINT (Siemens, 1996) and was found to be negligible. |
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 | ||
Ru | 0.0000 | 0.0000 | 0.0000 | 0.02737 (9) | |
P1 | −0.20732 (5) | −0.00331 (3) | −0.00383 (6) | 0.03104 (14) | |
Cl1 | −0.01654 (5) | 0.09999 (3) | 0.16324 (6) | 0.03953 (15) | |
N1 | −0.07666 (19) | 0.05116 (12) | −0.2650 (2) | 0.0427 (5) | |
C19 | −0.0920 (3) | 0.10581 (17) | −0.3573 (3) | 0.0519 (7) | |
C1 | −0.2941 (2) | −0.03471 (15) | −0.1511 (2) | 0.0350 (5) | |
C2 | −0.2664 (2) | −0.10480 (15) | −0.2081 (3) | 0.0435 (6) | |
H2A | −0.2059 | −0.1350 | −0.1707 | 0.052* | |
C3 | −0.3278 (3) | −0.12985 (17) | −0.3195 (3) | 0.0519 (7) | |
H3A | −0.3076 | −0.1763 | −0.3571 | 0.062* | |
C4 | −0.4187 (3) | −0.0865 (2) | −0.3752 (3) | 0.0592 (8) | |
H4A | −0.4601 | −0.1034 | −0.4501 | 0.071* | |
C5 | −0.4477 (3) | −0.0178 (2) | −0.3187 (3) | 0.0605 (8) | |
H5A | −0.5096 | 0.0113 | −0.3553 | 0.073* | |
C6 | −0.3859 (3) | 0.00859 (16) | −0.2082 (3) | 0.0484 (7) | |
H6A | −0.4060 | 0.0555 | −0.1719 | 0.058* | |
C7 | −0.2743 (2) | 0.09162 (13) | 0.0258 (2) | 0.0364 (5) | |
C8 | −0.3396 (2) | 0.10426 (17) | 0.1270 (3) | 0.0493 (7) | |
H8A | −0.3532 | 0.0634 | 0.1817 | 0.059* | |
C9 | −0.3851 (3) | 0.17792 (19) | 0.1472 (3) | 0.0646 (9) | |
H9A | −0.4298 | 0.1855 | 0.2147 | 0.077* | |
C10 | −0.3652 (3) | 0.23867 (19) | 0.0702 (4) | 0.0657 (9) | |
H10A | −0.3943 | 0.2879 | 0.0862 | 0.079* | |
C11 | −0.3017 (3) | 0.22717 (17) | −0.0322 (4) | 0.0620 (9) | |
H11A | −0.2887 | 0.2686 | −0.0859 | 0.074* | |
C12 | −0.2572 (2) | 0.15387 (16) | −0.0551 (3) | 0.0505 (7) | |
H12A | −0.2156 | 0.1463 | −0.1251 | 0.061* | |
C13 | −0.2652 (2) | −0.06559 (14) | 0.1170 (2) | 0.0350 (5) | |
C14 | −0.2154 (2) | −0.06151 (16) | 0.2422 (2) | 0.0434 (6) | |
H14A | −0.1564 | −0.0260 | 0.2638 | 0.052* | |
C15 | −0.2528 (3) | −0.10993 (18) | 0.3349 (3) | 0.0533 (7) | |
H15A | −0.2180 | −0.1070 | 0.4181 | 0.064* | |
C16 | −0.3409 (3) | −0.16228 (17) | 0.3055 (3) | 0.0550 (7) | |
H16A | −0.3646 | −0.1954 | 0.3678 | 0.066* | |
C17 | −0.3936 (3) | −0.16511 (16) | 0.1834 (3) | 0.0523 (7) | |
H17A | −0.4549 | −0.1992 | 0.1638 | 0.063* | |
C18 | −0.3564 (2) | −0.11769 (15) | 0.0887 (3) | 0.0424 (6) | |
H18A | −0.3923 | −0.1206 | 0.0061 | 0.051* | |
N2 | −0.02174 (17) | 0.08097 (11) | −0.15353 (19) | 0.0342 (4) | |
C20 | −0.0485 (3) | 0.17434 (16) | −0.3037 (3) | 0.0527 (7) | |
H20A | −0.0486 | 0.2229 | −0.3430 | 0.063* | |
C21 | −0.0041 (2) | 0.15665 (15) | −0.1792 (3) | 0.0415 (6) | |
C22 | −0.1463 (4) | 0.0838 (2) | −0.4866 (3) | 0.0850 (12) | |
H22A | −0.1217 | 0.0323 | −0.5076 | 0.128* | |
H22B | −0.1232 | 0.1203 | −0.5484 | 0.128* | |
H22C | −0.2287 | 0.0846 | −0.4869 | 0.128* | |
C23 | 0.0550 (3) | 0.21223 (15) | −0.0869 (3) | 0.0556 (7) | |
H23A | 0.0562 | 0.2630 | −0.1251 | 0.083* | |
H23B | 0.1326 | 0.1950 | −0.0640 | 0.083* | |
H23C | 0.0144 | 0.2147 | −0.0120 | 0.083* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru | 0.03205 (14) | 0.02362 (13) | 0.02699 (14) | −0.00015 (9) | 0.00571 (10) | 0.00024 (10) |
P1 | 0.0312 (3) | 0.0303 (3) | 0.0325 (3) | −0.0004 (2) | 0.0072 (2) | −0.0012 (2) |
Cl1 | 0.0444 (3) | 0.0341 (3) | 0.0405 (3) | 0.0003 (2) | 0.0062 (3) | −0.0073 (3) |
N1 | 0.0489 (12) | 0.0446 (12) | 0.0347 (11) | 0.0023 (10) | 0.0044 (9) | 0.0032 (10) |
C19 | 0.0633 (18) | 0.0562 (17) | 0.0363 (14) | 0.0080 (14) | 0.0057 (13) | 0.0101 (13) |
C1 | 0.0346 (12) | 0.0400 (13) | 0.0308 (12) | −0.0036 (10) | 0.0056 (10) | −0.0002 (10) |
C2 | 0.0410 (13) | 0.0419 (14) | 0.0478 (15) | −0.0028 (11) | 0.0049 (11) | −0.0048 (12) |
C3 | 0.0582 (17) | 0.0512 (16) | 0.0473 (16) | −0.0100 (13) | 0.0103 (13) | −0.0116 (13) |
C4 | 0.0655 (19) | 0.074 (2) | 0.0363 (15) | −0.0109 (16) | −0.0020 (14) | −0.0064 (15) |
C5 | 0.0553 (18) | 0.075 (2) | 0.0481 (18) | 0.0062 (15) | −0.0106 (15) | 0.0037 (16) |
C6 | 0.0470 (15) | 0.0536 (16) | 0.0443 (16) | 0.0073 (12) | 0.0027 (12) | −0.0022 (12) |
C7 | 0.0312 (11) | 0.0342 (12) | 0.0438 (14) | 0.0018 (9) | 0.0035 (10) | −0.0043 (10) |
C8 | 0.0521 (15) | 0.0472 (15) | 0.0502 (16) | 0.0106 (13) | 0.0130 (13) | −0.0040 (13) |
C9 | 0.069 (2) | 0.062 (2) | 0.064 (2) | 0.0194 (16) | 0.0131 (17) | −0.0180 (17) |
C10 | 0.0615 (19) | 0.0456 (17) | 0.088 (3) | 0.0159 (14) | −0.0015 (19) | −0.0187 (17) |
C11 | 0.0543 (17) | 0.0385 (15) | 0.092 (3) | 0.0055 (13) | −0.0013 (17) | 0.0080 (16) |
C12 | 0.0433 (15) | 0.0441 (15) | 0.0656 (19) | 0.0078 (12) | 0.0133 (13) | 0.0062 (14) |
C13 | 0.0348 (12) | 0.0358 (12) | 0.0359 (13) | 0.0013 (10) | 0.0110 (10) | −0.0001 (10) |
C14 | 0.0427 (14) | 0.0519 (15) | 0.0374 (14) | −0.0066 (11) | 0.0124 (11) | −0.0034 (12) |
C15 | 0.0569 (17) | 0.0660 (19) | 0.0394 (15) | 0.0017 (14) | 0.0162 (13) | 0.0061 (14) |
C16 | 0.0643 (18) | 0.0496 (16) | 0.0552 (18) | −0.0031 (14) | 0.0267 (15) | 0.0128 (14) |
C17 | 0.0493 (16) | 0.0431 (15) | 0.067 (2) | −0.0100 (12) | 0.0198 (14) | 0.0028 (14) |
C18 | 0.0383 (13) | 0.0419 (14) | 0.0479 (15) | −0.0062 (11) | 0.0086 (11) | −0.0016 (12) |
N2 | 0.0380 (10) | 0.0309 (10) | 0.0351 (11) | −0.0006 (8) | 0.0110 (8) | 0.0039 (8) |
C20 | 0.0702 (19) | 0.0417 (15) | 0.0486 (17) | 0.0096 (13) | 0.0185 (14) | 0.0167 (13) |
C21 | 0.0486 (14) | 0.0355 (13) | 0.0432 (14) | 0.0020 (11) | 0.0179 (12) | 0.0047 (11) |
C22 | 0.124 (3) | 0.080 (2) | 0.0457 (19) | 0.014 (2) | −0.016 (2) | 0.0072 (18) |
C23 | 0.072 (2) | 0.0359 (14) | 0.0613 (19) | −0.0064 (13) | 0.0197 (16) | −0.0018 (13) |
Ru—N2 | 2.1278 (19) | C9—C10 | 1.354 (5) |
Ru—N2i | 2.1278 (19) | C9—H9A | 0.9300 |
Ru—P1 | 2.4116 (6) | C10—C11 | 1.380 (5) |
Ru—P1i | 2.4116 (6) | C10—H10A | 0.9300 |
Ru—Cl1i | 2.4491 (6) | C11—C12 | 1.390 (4) |
Ru—Cl1 | 2.4491 (6) | C11—H11A | 0.9300 |
P1—C13 | 1.839 (2) | C12—H12A | 0.9300 |
P1—C7 | 1.845 (2) | C13—C14 | 1.390 (3) |
P1—C1 | 1.847 (2) | C13—C18 | 1.397 (3) |
N1—C19 | 1.349 (3) | C14—C15 | 1.385 (4) |
N1—N2 | 1.380 (3) | C14—H14A | 0.9300 |
C19—C20 | 1.379 (4) | C15—C16 | 1.376 (4) |
C19—C22 | 1.493 (4) | C15—H15A | 0.9300 |
C1—C6 | 1.389 (4) | C16—C17 | 1.370 (4) |
C1—C2 | 1.395 (3) | C16—H16A | 0.9300 |
C2—C3 | 1.382 (4) | C17—C18 | 1.389 (4) |
C2—H2A | 0.9300 | C17—H17A | 0.9300 |
C3—C4 | 1.378 (4) | C18—H18A | 0.9300 |
C3—H3A | 0.9300 | N2—C21 | 1.345 (3) |
C4—C5 | 1.376 (4) | C20—C21 | 1.395 (4) |
C4—H4A | 0.9300 | C20—H20A | 0.9300 |
C5—C6 | 1.383 (4) | C21—C23 | 1.482 (4) |
C5—H5A | 0.9300 | C22—H22A | 0.9600 |
C6—H6A | 0.9300 | C22—H22B | 0.9600 |
C7—C8 | 1.386 (4) | C22—H22C | 0.9600 |
C7—C12 | 1.393 (4) | C23—H23A | 0.9600 |
C8—C9 | 1.394 (4) | C23—H23B | 0.9600 |
C8—H8A | 0.9300 | C23—H23C | 0.9600 |
N2—Ru—N2i | 180.00 (10) | C10—C9—H9A | 119.5 |
N2—Ru—P1 | 87.59 (6) | C8—C9—H9A | 119.5 |
N2i—Ru—P1 | 92.41 (6) | C9—C10—C11 | 119.6 (3) |
N2—Ru—P1i | 92.41 (6) | C9—C10—H10A | 120.2 |
N2i—Ru—P1i | 87.59 (6) | C11—C10—H10A | 120.2 |
P1—Ru—P1i | 180.0 | C10—C11—C12 | 120.2 (3) |
N2—Ru—Cl1i | 86.24 (6) | C10—C11—H11A | 119.9 |
N2i—Ru—Cl1i | 93.76 (6) | C12—C11—H11A | 119.9 |
P1—Ru—Cl1i | 96.84 (2) | C11—C12—C7 | 120.5 (3) |
P1i—Ru—Cl1i | 83.16 (2) | C11—C12—H12A | 119.7 |
N2—Ru—Cl1 | 93.76 (6) | C7—C12—H12A | 119.7 |
N2i—Ru—Cl1 | 86.24 (6) | C14—C13—C18 | 118.2 (2) |
P1—Ru—Cl1 | 83.16 (2) | C14—C13—P1 | 118.70 (19) |
P1i—Ru—Cl1 | 96.84 (2) | C18—C13—P1 | 123.1 (2) |
Cl1i—Ru—Cl1 | 180.00 (4) | C15—C14—C13 | 120.6 (2) |
C13—P1—C7 | 101.84 (11) | C15—C14—H14A | 119.7 |
C13—P1—C1 | 101.81 (11) | C13—C14—H14A | 119.7 |
C7—P1—C1 | 101.17 (11) | C16—C15—C14 | 120.7 (3) |
C13—P1—Ru | 115.87 (8) | C16—C15—H15A | 119.6 |
C7—P1—Ru | 114.56 (8) | C14—C15—H15A | 119.6 |
C1—P1—Ru | 119.06 (8) | C17—C16—C15 | 119.4 (3) |
C19—N1—N2 | 112.0 (2) | C17—C16—H16A | 120.3 |
N1—C19—C20 | 106.2 (2) | C15—C16—H16A | 120.3 |
N1—C19—C22 | 119.8 (3) | C16—C17—C18 | 120.7 (3) |
C20—C19—C22 | 134.0 (3) | C16—C17—H17A | 119.6 |
C6—C1—C2 | 118.3 (2) | C18—C17—H17A | 119.6 |
C6—C1—P1 | 122.9 (2) | C17—C18—C13 | 120.4 (3) |
C2—C1—P1 | 118.79 (19) | C17—C18—H18A | 119.8 |
C3—C2—C1 | 120.7 (3) | C13—C18—H18A | 119.8 |
C3—C2—H2A | 119.6 | C21—N2—N1 | 104.65 (19) |
C1—C2—H2A | 119.6 | C21—N2—Ru | 140.62 (18) |
C4—C3—C2 | 120.5 (3) | N1—N2—Ru | 114.62 (14) |
C4—C3—H3A | 119.8 | C19—C20—C21 | 106.7 (2) |
C2—C3—H3A | 119.8 | C19—C20—H20A | 126.6 |
C5—C4—C3 | 119.2 (3) | C21—C20—H20A | 126.6 |
C5—C4—H4A | 120.4 | N2—C21—C20 | 110.4 (2) |
C3—C4—H4A | 120.4 | N2—C21—C23 | 123.9 (2) |
C4—C5—C6 | 121.0 (3) | C20—C21—C23 | 125.6 (2) |
C4—C5—H5A | 119.5 | C19—C22—H22A | 109.5 |
C6—C5—H5A | 119.5 | C19—C22—H22B | 109.5 |
C5—C6—C1 | 120.3 (3) | H22A—C22—H22B | 109.5 |
C5—C6—H6A | 119.9 | C19—C22—H22C | 109.5 |
C1—C6—H6A | 119.9 | H22A—C22—H22C | 109.5 |
C8—C7—C12 | 118.3 (2) | H22B—C22—H22C | 109.5 |
C8—C7—P1 | 122.8 (2) | C21—C23—H23A | 109.5 |
C12—C7—P1 | 119.0 (2) | C21—C23—H23B | 109.5 |
C7—C8—C9 | 120.3 (3) | H23A—C23—H23B | 109.5 |
C7—C8—H8A | 119.8 | C21—C23—H23C | 109.5 |
C9—C8—H8A | 119.8 | H23A—C23—H23C | 109.5 |
C10—C9—C8 | 121.0 (3) | H23B—C23—H23C | 109.5 |
N2—Ru—P1—C13 | −178.48 (10) | C8—C9—C10—C11 | 1.8 (5) |
N2i—Ru—P1—C13 | 1.52 (10) | C9—C10—C11—C12 | −0.8 (5) |
Cl1i—Ru—P1—C13 | 95.60 (9) | C10—C11—C12—C7 | −1.1 (5) |
Cl1—Ru—P1—C13 | −84.40 (9) | C8—C7—C12—C11 | 1.9 (4) |
N2—Ru—P1—C7 | −60.30 (11) | P1—C7—C12—C11 | −176.9 (2) |
N2i—Ru—P1—C7 | 119.70 (11) | C7—P1—C13—C14 | −79.3 (2) |
Cl1i—Ru—P1—C7 | −146.22 (9) | C1—P1—C13—C14 | 176.5 (2) |
Cl1—Ru—P1—C7 | 33.78 (9) | Ru—P1—C13—C14 | 45.7 (2) |
N2—Ru—P1—C1 | 59.53 (11) | C7—P1—C13—C18 | 101.5 (2) |
N2i—Ru—P1—C1 | −120.47 (11) | C1—P1—C13—C18 | −2.8 (2) |
Cl1i—Ru—P1—C1 | −26.39 (9) | Ru—P1—C13—C18 | −133.52 (19) |
Cl1—Ru—P1—C1 | 153.61 (9) | C18—C13—C14—C15 | 2.2 (4) |
N2—N1—C19—C20 | −1.6 (3) | P1—C13—C14—C15 | −177.0 (2) |
N2—N1—C19—C22 | 177.8 (3) | C13—C14—C15—C16 | −0.9 (4) |
C13—P1—C1—C6 | 102.6 (2) | C14—C15—C16—C17 | −1.4 (5) |
C7—P1—C1—C6 | −2.1 (3) | C15—C16—C17—C18 | 2.2 (5) |
Ru—P1—C1—C6 | −128.6 (2) | C16—C17—C18—C13 | −0.7 (4) |
C13—P1—C1—C2 | −77.6 (2) | C14—C13—C18—C17 | −1.5 (4) |
C7—P1—C1—C2 | 177.7 (2) | P1—C13—C18—C17 | 177.8 (2) |
Ru—P1—C1—C2 | 51.2 (2) | C19—N1—N2—C21 | 0.5 (3) |
C6—C1—C2—C3 | 0.9 (4) | C19—N1—N2—Ru | 177.57 (18) |
P1—C1—C2—C3 | −178.9 (2) | P1—Ru—N2—C21 | 110.7 (3) |
C1—C2—C3—C4 | −1.0 (4) | P1i—Ru—N2—C21 | −69.3 (3) |
C2—C3—C4—C5 | 0.0 (5) | Cl1i—Ru—N2—C21 | −152.3 (3) |
C3—C4—C5—C6 | 0.9 (5) | Cl1—Ru—N2—C21 | 27.7 (3) |
C4—C5—C6—C1 | −0.9 (5) | P1—Ru—N2—N1 | −64.88 (16) |
C2—C1—C6—C5 | 0.0 (4) | P1i—Ru—N2—N1 | 115.12 (16) |
P1—C1—C6—C5 | 179.8 (2) | Cl1i—Ru—N2—N1 | 32.14 (16) |
C13—P1—C7—C8 | 5.9 (2) | Cl1—Ru—N2—N1 | −147.86 (16) |
C1—P1—C7—C8 | 110.6 (2) | N1—C19—C20—C21 | 1.9 (3) |
Ru—P1—C7—C8 | −120.0 (2) | C22—C19—C20—C21 | −177.2 (4) |
C13—P1—C7—C12 | −175.3 (2) | N1—N2—C21—C20 | 0.8 (3) |
C1—P1—C7—C12 | −70.6 (2) | Ru—N2—C21—C20 | −175.0 (2) |
Ru—P1—C7—C12 | 58.8 (2) | N1—N2—C21—C23 | −178.8 (3) |
C12—C7—C8—C9 | −0.9 (4) | Ru—N2—C21—C23 | 5.3 (4) |
P1—C7—C8—C9 | 177.9 (2) | C19—C20—C21—N2 | −1.7 (3) |
C7—C8—C9—C10 | −1.0 (5) | C19—C20—C21—C23 | 177.9 (3) |
Symmetry code: (i) −x, −y, −z. |
Experimental details
Crystal data | |
Chemical formula | [RuCl2(C5H7N2)2(C18H15P)2] |
Mr | 886.76 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 11.6466 (2), 17.1438 (3), 10.5361 (2) |
β (°) | 95.603 (1) |
V (Å3) | 2093.66 (6) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.62 |
Crystal size (mm) | 0.28 × 0.26 × 0.20 |
Data collection | |
Diffractometer | Siemens SMART CCD area-detector diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.846, 0.887 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14880, 5169, 3919 |
Rint | 0.052 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.109, 0.99 |
No. of reflections | 5169 |
No. of parameters | 252 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.06, −0.91 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXTL (Sheldrick, 1997), SHELXTL and PLATON (Spek, 1990).
Ru—N2 | 2.1278 (19) | Ru—Cl1 | 2.4491 (6) |
Ru—P1 | 2.4116 (6) | P1—C13 | 1.839 (2) |
N2—Ru—N2i | 180.00 (10) | P1—Ru—Cl1i | 96.84 (2) |
N2—Ru—P1 | 87.59 (6) | N2—Ru—Cl1 | 93.76 (6) |
N2—Ru—P1i | 92.41 (6) | P1—Ru—Cl1 | 83.16 (2) |
P1—Ru—P1i | 180.0 | Cl1i—Ru—Cl1 | 180.00 (4) |
N2—Ru—Cl1i | 86.24 (6) |
Symmetry code: (i) −x, −y, −z. |
The chemistry of ruthenium complexes containing pyrazolate ligands (pz) has attracted much attention during the last decade (Monica & Ardizzoia, 1997). Much of this interest arises from their role in important catalytic reactions; in particular, attention has focused on the complexes containing electronic-rich metal centers (Okoroafor et al., 1988). Also, these studies have revealed that pyrazolates is of rich coordination modes (Monica & Ardizzoia, 1997). Although reports on the RuII complexes with phosphine ligands are common, however, the number of RuII complexes with phosphine and pz mixed ligands are limited (Sherlock et al., 1989). Several hetero-binuclear complexes formed by pz bridges have recently appeared (Garcia et al., 1990a,b). In this context, we present the crystal structure of the title complex, (I).
The asymmetric unit of (I) contains one-half of the title complex, with the other half generated by inversion through the Ru atom; the Ru atom lies at the origin. A displacement ellipsoid plot with the numbering scheme is shown in Fig. 1. The structure of (I) consists of mononuclear [Ru(PPh3)2(3,5-Me2pz)2Cl2] units. The Ru atom is in a slightly distorted octahedral environment. This coordination is formed by two P atoms from trans-triphenylphosphine ligands, two N atoms from trans-pz ligands and two Cl atoms. The Ru—P bond length in (I) (Table 1) is obviously longer than that in RuCl(PPh3)2{HB(pz)3}] [2.340 (3) Å; Alcock et al., 1992] with two cis-PPh3 ligands. The Ru—N bond distance in (I) with terminal coordination pz ligand is significantly shorter than those in the related complexes with bridging pz ligands, such as [(PPh3)2(OC)HRu(m-pz)2Rh(cod)] (cod = cycloocta-1,5-diene) [2.283 (5) Å; Garcia et al., 1990a] and [(PPh3)2(OC)HRu(m-Cl)(m-pz)Ir(tfb)] (tfb = tetrafulorabenzo-barrelene) [2.302 (4) Å; Garcia et al., 1990b]. The Ru—Cl bond length is normal. There are two intramolecular C—H···Cl weak interactions, C2—H2A···Cl1i [symmetry code: (i) -x, -y, -z] and C23—H23C···Cl1, with H···Cl distances of 2.65 and 2.74 Å, respectively.