Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807037282/bt2455sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807037282/bt2455Isup2.hkl |
CCDC reference: 635750
All chemicals used were of analytical reagent grade and were used directly without further purification. A solution of PPh3 (0.15 mg, 0.6 mmol) in acetonitrile (4 ml) was reacted with CuCl (0.03 mg, 0.3 mmol) in acetonitrile (5 ml). 1,2-Diaminopropane (0.02 mg, 0.3 mmol) in acetonitrile (3 ml) was added to the mixture, which was stirred for 1 h. Slow evaporation at room temperature of the solvent gave blue crystals.
The 1,2-diaminopropane ligand is twofold disordered, with refined occupancy factors of 0.599:0.401 (10); restraints were applied to the displacement parameters of this ligand. All H atoms were positioned geometrically, with N—H = 0.92 and C—H = 0.95–1.00 Å and Uiso(H) = 1.2Ueq(N,C) or 1.5Ueq(C) for methyl groups.
Trinuclear metal complexes can be classified as linear and non-linear. Trinuclear copper complexes with two, three or four bridges (Prins et al., 1996; Feng et al., 2007; Onan et al., 1984; Choi et al., 2006) have been reported. There are also some reported singly-bridged copper complexes (Arrizabalaga et al., 1983; Bailey et al., 1995). We report here the crystal structure of a new linear trinuclear mixed-valence copper compound, (I) (Fig. 1). It contains two CuI atoms with distorted tetrahedral coordination, the four vertices being occupied by two P atoms of PPh3 ligands and two Cl atoms. The largest deviation from ideal tetrahedral geometry is the wide P—Cu—P angle of 121.92 (4)°. The central CuII atom lies on an inversion centre and has octahedral coordination, with two chelating bidentate diamines and two trans-chloro bridges to the CuI atoms. The diamine ligands are disordered over two orientations, with refined occupancy factors of 0.599:0.401 (10). Each of them forms one N—H···Cl hydrogen bond to a terminal Cl atom. The Cu—Cl bonds for the central CuII atom are elongated as a result of a typical Jahn-Teller distortion, and the bridging Cl atoms make longer bonds to the CuI atoms than do the terminal Cl atoms, as expected. There are no significant intermolecular interactions, and acetonitrile solvent molecules simply occupy what would otherwise be voids in the structure.
For related structures, see: Arrizabalaga et al. (1983); Bailey et al. (1995); Choi et al. (2006); Feng et al. (2007); Onan et al. (1984); Prins et al. (1996).
Data collection: COLLECT (Nonius, 1998); cell refinement: EVALCCD (Duisenberg et al., 2003); data reduction: EVALCCD; program(s) used to solve structure: SHELXTL (Sheldrick, 2005); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.
[Cu3Cl4(C3H10N2)2(C18H15P)4]·2C2H3N | F(000) = 1670 |
Mr = 1611.87 | Dx = 1.353 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 15.896 (3) Å | Cell parameters from 32758 reflections |
b = 9.4181 (15) Å | θ = 4.1–25.0° |
c = 26.533 (4) Å | µ = 1.06 mm−1 |
β = 94.957 (12)° | T = 150 K |
V = 3957.4 (11) Å3 | Block, blue |
Z = 2 | 0.25 × 0.20 × 0.20 mm |
Nonius KappaCCD diffractometer | 6923 independent reflections |
Radiation source: sealed tube | 5038 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.074 |
φ and ω scans | θmax = 25.0°, θmin = 4.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2007) | h = −18→18 |
Tmin = 0.780, Tmax = 0.820 | k = −11→11 |
32758 measured reflections | l = −31→31 |
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)] = 0.054 | H-atom parameters constrained |
wR(F2) = 0.158 | w = 1/[σ2(Fo2) + (0.0745P)2 + 8.3144P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max < 0.001 |
6923 reflections | Δρmax = 0.78 e Å−3 |
496 parameters | Δρmin = −0.81 e Å−3 |
136 restraints | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0032 (5) |
[Cu3Cl4(C3H10N2)2(C18H15P)4]·2C2H3N | V = 3957.4 (11) Å3 |
Mr = 1611.87 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 15.896 (3) Å | µ = 1.06 mm−1 |
b = 9.4181 (15) Å | T = 150 K |
c = 26.533 (4) Å | 0.25 × 0.20 × 0.20 mm |
β = 94.957 (12)° |
Nonius KappaCCD diffractometer | 6923 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2007) | 5038 reflections with I > 2σ(I) |
Tmin = 0.780, Tmax = 0.820 | Rint = 0.074 |
32758 measured reflections |
R[F2 > 2σ(F2)] = 0.054 | 136 restraints |
wR(F2) = 0.158 | H-atom parameters constrained |
S = 1.03 | Δρmax = 0.78 e Å−3 |
6923 reflections | Δρmin = −0.81 e Å−3 |
496 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 | Occ. (<1) | |
Cu1 | 0.28031 (3) | 0.32452 (6) | 0.389429 (19) | 0.02994 (19) | |
Cl1 | 0.34277 (7) | 0.11509 (13) | 0.42371 (4) | 0.0381 (3) | |
Cl2 | 0.39546 (7) | 0.49353 (13) | 0.40612 (5) | 0.0395 (3) | |
P1 | 0.16988 (7) | 0.39615 (12) | 0.43263 (4) | 0.0267 (3) | |
P2 | 0.26663 (7) | 0.29168 (13) | 0.30384 (4) | 0.0273 (3) | |
C1 | 0.1891 (3) | 0.3852 (5) | 0.50241 (15) | 0.0291 (10) | |
C2 | 0.1611 (3) | 0.4882 (5) | 0.53478 (17) | 0.0365 (11) | |
H2 | 0.1327 | 0.5705 | 0.5213 | 0.044* | |
C3 | 0.1750 (3) | 0.4699 (7) | 0.58722 (19) | 0.0505 (14) | |
H3 | 0.1574 | 0.5410 | 0.6094 | 0.061* | |
C4 | 0.2143 (3) | 0.3488 (7) | 0.60679 (18) | 0.0531 (15) | |
H4 | 0.2225 | 0.3356 | 0.6424 | 0.064* | |
C5 | 0.2418 (4) | 0.2472 (7) | 0.5747 (2) | 0.0585 (16) | |
H5 | 0.2693 | 0.1645 | 0.5884 | 0.070* | |
C6 | 0.2298 (3) | 0.2639 (6) | 0.52255 (17) | 0.0421 (12) | |
H6 | 0.2491 | 0.1933 | 0.5007 | 0.050* | |
C7 | 0.1373 (3) | 0.5817 (5) | 0.42317 (15) | 0.0308 (10) | |
C8 | 0.2008 (3) | 0.6845 (5) | 0.42215 (18) | 0.0387 (12) | |
H8 | 0.2583 | 0.6557 | 0.4240 | 0.046* | |
C9 | 0.1808 (4) | 0.8288 (5) | 0.41839 (19) | 0.0436 (12) | |
H9 | 0.2247 | 0.8974 | 0.4187 | 0.052* | |
C10 | 0.0973 (3) | 0.8719 (5) | 0.41417 (17) | 0.0407 (12) | |
H10 | 0.0839 | 0.9701 | 0.4116 | 0.049* | |
C11 | 0.0332 (3) | 0.7719 (5) | 0.41377 (17) | 0.0394 (12) | |
H11 | −0.0241 | 0.8015 | 0.4100 | 0.047* | |
C12 | 0.0529 (3) | 0.6268 (5) | 0.41891 (16) | 0.0351 (11) | |
H12 | 0.0088 | 0.5589 | 0.4195 | 0.042* | |
C13 | 0.0702 (3) | 0.2987 (5) | 0.42097 (16) | 0.0285 (10) | |
C14 | 0.0274 (3) | 0.2347 (5) | 0.45891 (17) | 0.0344 (11) | |
H14 | 0.0496 | 0.2428 | 0.4932 | 0.041* | |
C15 | −0.0471 (3) | 0.1590 (6) | 0.4472 (2) | 0.0447 (13) | |
H15 | −0.0749 | 0.1154 | 0.4734 | 0.054* | |
C16 | −0.0808 (3) | 0.1471 (6) | 0.3976 (2) | 0.0455 (13) | |
H16 | −0.1314 | 0.0951 | 0.3898 | 0.055* | |
C17 | −0.0399 (3) | 0.2120 (6) | 0.35907 (19) | 0.0439 (13) | |
H17 | −0.0633 | 0.2059 | 0.3250 | 0.053* | |
C18 | 0.0353 (3) | 0.2857 (5) | 0.37077 (17) | 0.0363 (11) | |
H18 | 0.0633 | 0.3278 | 0.3443 | 0.044* | |
C19 | 0.3537 (3) | 0.1937 (5) | 0.27892 (17) | 0.0332 (11) | |
C20 | 0.4345 (3) | 0.2202 (6) | 0.3011 (2) | 0.0438 (12) | |
H20 | 0.4421 | 0.2812 | 0.3297 | 0.053* | |
C21 | 0.5043 (4) | 0.1580 (7) | 0.2818 (3) | 0.0645 (18) | |
H21 | 0.5594 | 0.1769 | 0.2972 | 0.077* | |
C22 | 0.4941 (4) | 0.0694 (7) | 0.2405 (3) | 0.0646 (18) | |
H22 | 0.5422 | 0.0287 | 0.2272 | 0.078* | |
C23 | 0.4144 (4) | 0.0390 (6) | 0.2182 (2) | 0.0527 (15) | |
H23 | 0.4074 | −0.0221 | 0.1897 | 0.063* | |
C24 | 0.3441 (3) | 0.0994 (5) | 0.23824 (17) | 0.0407 (12) | |
H24 | 0.2890 | 0.0759 | 0.2239 | 0.049* | |
C25 | 0.2624 (3) | 0.4519 (5) | 0.26432 (17) | 0.0317 (10) | |
C26 | 0.2333 (3) | 0.5768 (6) | 0.2848 (2) | 0.0460 (13) | |
H26 | 0.2168 | 0.5776 | 0.3184 | 0.055* | |
C27 | 0.2282 (4) | 0.7010 (6) | 0.2559 (3) | 0.0637 (17) | |
H27 | 0.2093 | 0.7864 | 0.2703 | 0.076* | |
C28 | 0.2503 (4) | 0.7013 (6) | 0.2066 (2) | 0.0577 (16) | |
H28 | 0.2451 | 0.7855 | 0.1869 | 0.069* | |
C29 | 0.2798 (3) | 0.5784 (6) | 0.1865 (2) | 0.0467 (13) | |
H29 | 0.2954 | 0.5781 | 0.1528 | 0.056* | |
C30 | 0.2870 (3) | 0.4546 (6) | 0.21499 (17) | 0.0399 (12) | |
H30 | 0.3089 | 0.3711 | 0.2008 | 0.048* | |
C31 | 0.1742 (3) | 0.1909 (5) | 0.27813 (15) | 0.0278 (10) | |
C32 | 0.1217 (3) | 0.2291 (5) | 0.23523 (16) | 0.0349 (11) | |
H32 | 0.1331 | 0.3129 | 0.2171 | 0.042* | |
C33 | 0.0521 (3) | 0.1441 (6) | 0.21885 (19) | 0.0479 (14) | |
H33 | 0.0172 | 0.1700 | 0.1894 | 0.057* | |
C34 | 0.0340 (3) | 0.0232 (6) | 0.24513 (19) | 0.0453 (13) | |
H34 | −0.0135 | −0.0334 | 0.2340 | 0.054* | |
C35 | 0.0852 (3) | −0.0154 (6) | 0.28761 (19) | 0.0445 (13) | |
H35 | 0.0730 | −0.0991 | 0.3056 | 0.053* | |
C36 | 0.1539 (3) | 0.0669 (5) | 0.30402 (18) | 0.0384 (11) | |
H36 | 0.1883 | 0.0393 | 0.3334 | 0.046* | |
Cu2 | 0.5000 | 0.5000 | 0.5000 | 0.0436 (3) | |
N1 | 0.5266 (6) | 0.7108 (10) | 0.4930 (4) | 0.044 (2) | 0.599 (10) |
H1A | 0.5707 | 0.7364 | 0.5160 | 0.053* | 0.599 (10) |
H1B | 0.5416 | 0.7300 | 0.4610 | 0.053* | 0.599 (10) |
N2 | 0.3990 (6) | 0.5691 (12) | 0.5324 (4) | 0.051 (2) | 0.599 (10) |
H2A | 0.3511 | 0.5558 | 0.5109 | 0.061* | 0.599 (10) |
H2B | 0.3931 | 0.5189 | 0.5616 | 0.061* | 0.599 (10) |
C37 | 0.4493 (8) | 0.7906 (14) | 0.5028 (5) | 0.063 (3) | 0.599 (10) |
H37A | 0.4639 | 0.8903 | 0.5115 | 0.076* | 0.599 (10) |
H37B | 0.4093 | 0.7906 | 0.4721 | 0.076* | 0.599 (10) |
C38 | 0.4101 (14) | 0.724 (2) | 0.5445 (6) | 0.061 (4) | 0.599 (10) |
H38 | 0.4493 | 0.7336 | 0.5758 | 0.073* | 0.599 (10) |
C39 | 0.3253 (7) | 0.7951 (13) | 0.5539 (5) | 0.081 (4) | 0.599 (10) |
H39A | 0.3009 | 0.7473 | 0.5820 | 0.121* | 0.599 (10) |
H39B | 0.2863 | 0.7876 | 0.5233 | 0.121* | 0.599 (10) |
H39C | 0.3349 | 0.8954 | 0.5623 | 0.121* | 0.599 (10) |
N1X | 0.3985 (9) | 0.4925 (18) | 0.5435 (6) | 0.053 (4) | 0.401 (10) |
H1X1 | 0.3505 | 0.4650 | 0.5241 | 0.064* | 0.401 (10) |
H1X2 | 0.4086 | 0.4281 | 0.5694 | 0.064* | 0.401 (10) |
N2X | 0.4906 (10) | 0.7100 (19) | 0.5076 (6) | 0.049 (3) | 0.401 (10) |
H2X1 | 0.5319 | 0.7425 | 0.5312 | 0.059* | 0.401 (10) |
H2X2 | 0.4973 | 0.7540 | 0.4773 | 0.059* | 0.401 (10) |
C37X | 0.3874 (12) | 0.634 (2) | 0.5640 (9) | 0.078 (5) | 0.401 (10) |
H37C | 0.4273 | 0.6486 | 0.5943 | 0.094* | 0.401 (10) |
H37D | 0.3292 | 0.6444 | 0.5742 | 0.094* | 0.401 (10) |
C38X | 0.403 (2) | 0.743 (3) | 0.5247 (10) | 0.064 (5) | 0.401 (10) |
H38X | 0.3595 | 0.7334 | 0.4953 | 0.077* | 0.401 (10) |
C39X | 0.3998 (12) | 0.8929 (17) | 0.5458 (6) | 0.072 (5) | 0.401 (10) |
H39D | 0.4107 | 0.9613 | 0.5193 | 0.108* | 0.401 (10) |
H39E | 0.4428 | 0.9031 | 0.5743 | 0.108* | 0.401 (10) |
H39F | 0.3438 | 0.9106 | 0.5573 | 0.108* | 0.401 (10) |
N3 | 0.4423 (5) | 0.3375 (13) | 0.1140 (3) | 0.156 (4) | |
C40 | 0.5077 (5) | 0.3358 (9) | 0.1341 (3) | 0.078 (2) | |
C41 | 0.5903 (4) | 0.3360 (6) | 0.1589 (2) | 0.0524 (14) | |
H41A | 0.6241 | 0.4097 | 0.1442 | 0.079* | |
H41B | 0.6166 | 0.2431 | 0.1547 | 0.079* | |
H41C | 0.5873 | 0.3552 | 0.1950 | 0.079* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0258 (3) | 0.0369 (4) | 0.0267 (3) | 0.0007 (2) | −0.0002 (2) | −0.0018 (2) |
Cl1 | 0.0391 (6) | 0.0331 (7) | 0.0417 (6) | 0.0027 (5) | 0.0009 (5) | 0.0013 (5) |
Cl2 | 0.0340 (6) | 0.0369 (7) | 0.0455 (7) | −0.0061 (5) | −0.0079 (5) | 0.0000 (5) |
P1 | 0.0257 (6) | 0.0294 (7) | 0.0248 (6) | 0.0016 (5) | 0.0008 (4) | −0.0004 (5) |
P2 | 0.0255 (6) | 0.0317 (7) | 0.0244 (6) | 0.0028 (5) | 0.0000 (4) | −0.0001 (5) |
C1 | 0.025 (2) | 0.039 (3) | 0.023 (2) | −0.001 (2) | 0.0002 (17) | 0.0017 (19) |
C2 | 0.031 (2) | 0.043 (3) | 0.035 (3) | 0.005 (2) | 0.000 (2) | −0.006 (2) |
C3 | 0.046 (3) | 0.071 (4) | 0.035 (3) | 0.002 (3) | 0.003 (2) | −0.017 (3) |
C4 | 0.048 (3) | 0.086 (5) | 0.024 (2) | 0.007 (3) | −0.006 (2) | −0.001 (3) |
C5 | 0.062 (4) | 0.073 (4) | 0.039 (3) | 0.026 (3) | 0.002 (3) | 0.014 (3) |
C6 | 0.046 (3) | 0.051 (3) | 0.029 (2) | 0.014 (3) | −0.001 (2) | −0.002 (2) |
C7 | 0.031 (2) | 0.037 (3) | 0.025 (2) | 0.001 (2) | 0.0013 (18) | −0.0037 (19) |
C8 | 0.036 (3) | 0.037 (3) | 0.043 (3) | −0.003 (2) | −0.001 (2) | 0.000 (2) |
C9 | 0.056 (3) | 0.028 (3) | 0.048 (3) | −0.003 (2) | 0.009 (2) | 0.003 (2) |
C10 | 0.059 (3) | 0.028 (3) | 0.035 (3) | 0.009 (2) | 0.008 (2) | 0.001 (2) |
C11 | 0.044 (3) | 0.040 (3) | 0.035 (3) | 0.013 (2) | 0.006 (2) | 0.002 (2) |
C12 | 0.035 (3) | 0.037 (3) | 0.034 (2) | 0.002 (2) | 0.0015 (19) | −0.001 (2) |
C13 | 0.026 (2) | 0.025 (3) | 0.035 (2) | 0.0035 (18) | 0.0023 (18) | −0.0012 (18) |
C14 | 0.036 (3) | 0.038 (3) | 0.029 (2) | 0.000 (2) | −0.0010 (19) | −0.002 (2) |
C15 | 0.034 (3) | 0.048 (3) | 0.053 (3) | −0.005 (2) | 0.009 (2) | 0.002 (2) |
C16 | 0.027 (2) | 0.052 (3) | 0.057 (3) | −0.004 (2) | 0.002 (2) | −0.011 (3) |
C17 | 0.036 (3) | 0.056 (3) | 0.038 (3) | 0.007 (2) | −0.005 (2) | −0.010 (2) |
C18 | 0.029 (2) | 0.048 (3) | 0.032 (2) | 0.005 (2) | −0.0004 (19) | −0.002 (2) |
C19 | 0.035 (3) | 0.034 (3) | 0.032 (2) | 0.008 (2) | 0.0057 (19) | 0.009 (2) |
C20 | 0.030 (3) | 0.041 (3) | 0.061 (3) | 0.001 (2) | 0.005 (2) | −0.001 (3) |
C21 | 0.029 (3) | 0.050 (4) | 0.116 (6) | 0.004 (3) | 0.017 (3) | −0.002 (4) |
C22 | 0.045 (4) | 0.055 (4) | 0.099 (5) | 0.017 (3) | 0.038 (3) | 0.007 (4) |
C23 | 0.060 (4) | 0.048 (4) | 0.052 (3) | 0.021 (3) | 0.016 (3) | −0.001 (3) |
C24 | 0.042 (3) | 0.047 (3) | 0.032 (2) | 0.016 (2) | 0.000 (2) | 0.001 (2) |
C25 | 0.030 (2) | 0.028 (3) | 0.036 (2) | 0.002 (2) | −0.0036 (19) | 0.001 (2) |
C26 | 0.045 (3) | 0.044 (3) | 0.048 (3) | 0.006 (2) | −0.001 (2) | −0.003 (2) |
C27 | 0.064 (4) | 0.035 (4) | 0.089 (5) | 0.010 (3) | −0.007 (3) | −0.001 (3) |
C28 | 0.051 (3) | 0.046 (4) | 0.071 (4) | −0.007 (3) | −0.021 (3) | 0.023 (3) |
C29 | 0.046 (3) | 0.048 (4) | 0.045 (3) | −0.010 (3) | −0.006 (2) | 0.011 (3) |
C30 | 0.040 (3) | 0.044 (3) | 0.034 (3) | −0.003 (2) | −0.003 (2) | 0.004 (2) |
C31 | 0.026 (2) | 0.032 (3) | 0.026 (2) | 0.0050 (19) | 0.0030 (17) | −0.0022 (18) |
C32 | 0.033 (3) | 0.040 (3) | 0.030 (2) | 0.002 (2) | −0.0031 (19) | −0.002 (2) |
C33 | 0.044 (3) | 0.066 (4) | 0.033 (3) | −0.002 (3) | −0.007 (2) | −0.010 (3) |
C34 | 0.041 (3) | 0.050 (3) | 0.045 (3) | −0.013 (2) | 0.002 (2) | −0.013 (3) |
C35 | 0.050 (3) | 0.039 (3) | 0.044 (3) | −0.009 (2) | 0.004 (2) | −0.006 (2) |
C36 | 0.041 (3) | 0.037 (3) | 0.037 (3) | 0.001 (2) | 0.002 (2) | 0.000 (2) |
Cu2 | 0.0374 (5) | 0.0428 (6) | 0.0508 (5) | −0.0041 (4) | 0.0044 (4) | −0.0060 (4) |
N1 | 0.033 (5) | 0.055 (5) | 0.042 (5) | −0.003 (4) | −0.003 (4) | 0.005 (4) |
N2 | 0.050 (5) | 0.049 (6) | 0.055 (6) | −0.020 (5) | 0.016 (4) | −0.011 (5) |
C37 | 0.054 (7) | 0.053 (7) | 0.084 (8) | 0.002 (5) | 0.012 (5) | 0.005 (6) |
C38 | 0.069 (7) | 0.056 (8) | 0.060 (9) | 0.006 (6) | 0.019 (7) | −0.010 (7) |
C39 | 0.071 (7) | 0.080 (8) | 0.095 (9) | −0.001 (6) | 0.026 (6) | −0.036 (7) |
N1X | 0.042 (7) | 0.061 (8) | 0.057 (8) | −0.023 (8) | 0.008 (6) | 0.008 (7) |
N2X | 0.035 (8) | 0.061 (9) | 0.051 (8) | −0.009 (7) | 0.004 (6) | −0.003 (6) |
C37X | 0.070 (10) | 0.065 (8) | 0.106 (13) | −0.001 (9) | 0.040 (9) | 0.006 (9) |
C38X | 0.067 (10) | 0.054 (8) | 0.076 (14) | 0.007 (9) | 0.030 (12) | −0.005 (9) |
C39X | 0.098 (14) | 0.059 (8) | 0.057 (9) | 0.018 (9) | −0.001 (8) | 0.001 (7) |
N3 | 0.065 (5) | 0.265 (13) | 0.133 (7) | −0.008 (6) | −0.014 (5) | −0.021 (7) |
C40 | 0.057 (4) | 0.117 (6) | 0.059 (4) | −0.009 (4) | 0.001 (3) | −0.007 (4) |
C41 | 0.056 (3) | 0.048 (4) | 0.053 (3) | −0.006 (3) | 0.001 (3) | −0.005 (3) |
Cu1—Cl1 | 2.3553 (13) | C28—H28 | 0.950 |
Cu1—Cl2 | 2.4372 (13) | C28—C29 | 1.374 (8) |
Cu1—P1 | 2.2800 (13) | C29—H29 | 0.950 |
Cu1—P2 | 2.2835 (12) | C29—C30 | 1.388 (7) |
P1—C1 | 1.853 (4) | C30—H30 | 0.950 |
P1—C7 | 1.834 (5) | C31—C32 | 1.400 (6) |
P1—C13 | 1.834 (4) | C31—C36 | 1.406 (7) |
P2—C19 | 1.834 (5) | C32—H32 | 0.950 |
P2—C25 | 1.836 (5) | C32—C33 | 1.403 (7) |
P2—C31 | 1.830 (4) | C33—H33 | 0.950 |
C1—C2 | 1.394 (6) | C33—C34 | 1.378 (8) |
C1—C6 | 1.396 (7) | C34—H34 | 0.950 |
C2—H2 | 0.950 | C34—C35 | 1.381 (7) |
C2—C3 | 1.401 (7) | C35—H35 | 0.950 |
C3—H3 | 0.950 | C35—C36 | 1.379 (7) |
C3—C4 | 1.380 (8) | C36—H36 | 0.950 |
C4—H4 | 0.950 | Cu2—Cl2 | 2.8731 (12) |
C4—C5 | 1.377 (8) | Cu2—Cl2i | 2.8731 (12) |
C5—H5 | 0.950 | Cu2—N1 | 2.042 (10) |
C5—C6 | 1.388 (7) | Cu2—N1i | 2.042 (10) |
C6—H6 | 0.950 | Cu2—N2 | 1.995 (10) |
C7—C8 | 1.400 (7) | Cu2—N2i | 1.995 (10) |
C7—C12 | 1.402 (6) | Cu2—N1X | 2.065 (14) |
C8—H8 | 0.950 | Cu2—N1Xi | 2.065 (14) |
C8—C9 | 1.397 (7) | Cu2—N2X | 1.995 (18) |
C9—H9 | 0.950 | Cu2—N2Xi | 1.995 (18) |
C9—C10 | 1.383 (7) | N1—H1A | 0.920 |
C10—H10 | 0.950 | N1—H1B | 0.920 |
C10—C11 | 1.388 (7) | N1—C37 | 1.482 (15) |
C11—H11 | 0.950 | N2—H2A | 0.920 |
C11—C12 | 1.406 (7) | N2—H2B | 0.920 |
C12—H12 | 0.950 | N2—C38 | 1.50 (2) |
C13—C14 | 1.399 (6) | C37—H37A | 0.990 |
C13—C18 | 1.404 (6) | C37—H37B | 0.990 |
C14—H14 | 0.950 | C37—C38 | 1.46 (2) |
C14—C15 | 1.395 (7) | C38—H38 | 1.000 |
C15—H15 | 0.950 | C38—C39 | 1.54 (2) |
C15—C16 | 1.380 (7) | C39—H39A | 0.980 |
C16—H16 | 0.950 | C39—H39B | 0.980 |
C16—C17 | 1.400 (7) | C39—H39C | 0.980 |
C17—H17 | 0.950 | N1X—H1X1 | 0.920 |
C17—C18 | 1.393 (7) | N1X—H1X2 | 0.920 |
C18—H18 | 0.950 | N1X—C37X | 1.46 (2) |
C19—C20 | 1.388 (7) | N2X—H2X1 | 0.920 |
C19—C24 | 1.396 (7) | N2X—H2X2 | 0.920 |
C20—H20 | 0.950 | N2X—C38X | 1.54 (3) |
C20—C21 | 1.392 (7) | C37X—H37C | 0.990 |
C21—H21 | 0.950 | C37X—H37D | 0.990 |
C21—C22 | 1.376 (9) | C37X—C38X | 1.50 (3) |
C22—H22 | 0.950 | C38X—H38X | 1.000 |
C22—C23 | 1.381 (9) | C38X—C39X | 1.52 (3) |
C23—H23 | 0.950 | C39X—H39D | 0.980 |
C23—C24 | 1.399 (7) | C39X—H39E | 0.980 |
C24—H24 | 0.950 | C39X—H39F | 0.980 |
C25—C26 | 1.392 (7) | N3—C40 | 1.127 (9) |
C25—C30 | 1.398 (7) | C40—C41 | 1.417 (9) |
C26—H26 | 0.950 | C41—H41A | 0.980 |
C26—C27 | 1.397 (8) | C41—H41B | 0.980 |
C27—H27 | 0.950 | C41—H41C | 0.980 |
C27—C28 | 1.382 (9) | ||
Cl1—Cu1—Cl2 | 101.06 (5) | C31—C32—H32 | 119.9 |
Cl1—Cu1—P1 | 111.76 (5) | C31—C32—C33 | 120.3 (5) |
Cl1—Cu1—P2 | 105.75 (5) | H32—C32—C33 | 119.9 |
Cl2—Cu1—P1 | 108.31 (5) | C32—C33—H33 | 119.7 |
Cl2—Cu1—P2 | 105.94 (5) | C32—C33—C34 | 120.5 (5) |
P1—Cu1—P2 | 121.92 (4) | H33—C33—C34 | 119.7 |
Cu1—Cl2—Cu2 | 122.71 (5) | C33—C34—H34 | 120.1 |
Cu1—P1—C1 | 114.74 (14) | C33—C34—C35 | 119.8 (5) |
Cu1—P1—C7 | 115.70 (15) | H34—C34—C35 | 120.1 |
Cu1—P1—C13 | 117.30 (14) | C34—C35—H35 | 119.9 |
C1—P1—C7 | 102.1 (2) | C34—C35—C36 | 120.3 (5) |
C1—P1—C13 | 101.9 (2) | H35—C35—C36 | 119.9 |
C7—P1—C13 | 102.9 (2) | C31—C36—C35 | 121.4 (4) |
Cu1—P2—C19 | 114.63 (15) | C31—C36—H36 | 119.3 |
Cu1—P2—C25 | 116.89 (15) | C35—C36—H36 | 119.3 |
Cu1—P2—C31 | 116.44 (14) | Cl2—Cu2—Cl2i | 180.0 |
C19—P2—C25 | 101.5 (2) | Cl2—Cu2—N1 | 92.9 (3) |
C19—P2—C31 | 102.2 (2) | Cl2i—Cu2—N1i | 92.9 (3) |
C25—P2—C31 | 103.0 (2) | Cl2i—Cu2—N1 | 87.1 (3) |
P1—C1—C2 | 122.9 (3) | Cl2—Cu2—N1i | 87.1 (3) |
P1—C1—C6 | 117.3 (3) | Cl2—Cu2—N2 | 87.4 (3) |
C2—C1—C6 | 119.7 (4) | Cl2i—Cu2—N2i | 87.4 (3) |
C1—C2—H2 | 120.2 | Cl2i—Cu2—N2 | 92.6 (3) |
C1—C2—C3 | 119.6 (5) | Cl2—Cu2—N2i | 92.6 (3) |
H2—C2—C3 | 120.2 | Cl2—Cu2—N1X | 93.6 (4) |
C2—C3—H3 | 119.9 | Cl2i—Cu2—N1Xi | 93.6 (4) |
C2—C3—C4 | 120.2 (5) | Cl2i—Cu2—N1X | 86.4 (4) |
H3—C3—C4 | 119.9 | Cl2—Cu2—N1Xi | 86.4 (4) |
C3—C4—H4 | 120.0 | Cl2—Cu2—N2X | 93.8 (5) |
C3—C4—C5 | 119.9 (5) | Cl2i—Cu2—N2Xi | 93.8 (5) |
H4—C4—C5 | 120.0 | Cl2i—Cu2—N2X | 86.2 (5) |
C4—C5—H5 | 119.5 | Cl2—Cu2—N2Xi | 86.2 (5) |
C4—C5—C6 | 121.0 (5) | N1—Cu2—N1i | 180.0 |
H5—C5—C6 | 119.5 | N1—Cu2—N2 | 84.4 (4) |
C1—C6—C5 | 119.5 (5) | N1i—Cu2—N2i | 84.4 (4) |
C1—C6—H6 | 120.2 | N1i—Cu2—N2 | 95.6 (4) |
C5—C6—H6 | 120.2 | N1—Cu2—N2i | 95.6 (4) |
P1—C7—C8 | 117.8 (3) | N2—Cu2—N2i | 180.0 |
P1—C7—C12 | 123.8 (4) | N1X—Cu2—N1Xi | 180.0 |
C8—C7—C12 | 118.4 (4) | N1X—Cu2—N2X | 84.7 (6) |
C7—C8—H8 | 119.5 | N1Xi—Cu2—N2Xi | 84.7 (6) |
C7—C8—C9 | 120.9 (5) | N1Xi—Cu2—N2X | 95.3 (6) |
H8—C8—C9 | 119.5 | N1X—Cu2—N2Xi | 95.3 (6) |
C8—C9—H9 | 120.0 | N2X—Cu2—N2Xi | 180.0 |
C8—C9—C10 | 120.1 (5) | Cu2—N1—H1A | 110.3 |
H9—C9—C10 | 120.0 | Cu2—N1—H1B | 110.3 |
C9—C10—H10 | 120.0 | Cu2—N1—C37 | 107.2 (7) |
C9—C10—C11 | 120.0 (5) | H1A—N1—H1B | 108.5 |
H10—C10—C11 | 120.0 | H1A—N1—C37 | 110.3 |
C10—C11—H11 | 119.9 | H1B—N1—C37 | 110.3 |
C10—C11—C12 | 120.1 (5) | Cu2—N2—H2A | 109.9 |
H11—C11—C12 | 119.9 | Cu2—N2—H2B | 109.9 |
C7—C12—C11 | 120.4 (5) | Cu2—N2—C38 | 108.9 (10) |
C7—C12—H12 | 119.8 | H2A—N2—H2B | 108.3 |
C11—C12—H12 | 119.8 | H2A—N2—C38 | 109.9 |
P1—C13—C14 | 124.1 (3) | H2B—N2—C38 | 109.9 |
P1—C13—C18 | 118.0 (3) | N1—C37—H37A | 109.8 |
C14—C13—C18 | 117.9 (4) | N1—C37—H37B | 109.8 |
C13—C14—H14 | 119.5 | N1—C37—C38 | 109.3 (12) |
C13—C14—C15 | 121.1 (4) | H37A—C37—H37B | 108.3 |
H14—C14—C15 | 119.5 | H37A—C37—C38 | 109.8 |
C14—C15—H15 | 119.8 | H37B—C37—C38 | 109.8 |
C14—C15—C16 | 120.4 (5) | N2—C38—C37 | 107.9 (13) |
H15—C15—C16 | 119.8 | N2—C38—H38 | 108.5 |
C15—C16—H16 | 120.2 | N2—C38—C39 | 111.5 (15) |
C15—C16—C17 | 119.6 (5) | C37—C38—H38 | 108.5 |
H16—C16—C17 | 120.2 | C37—C38—C39 | 111.9 (14) |
C16—C17—H17 | 120.1 | H38—C38—C39 | 108.5 |
C16—C17—C18 | 119.9 (4) | C38—C39—H39A | 109.5 |
H17—C17—C18 | 120.1 | C38—C39—H39B | 109.5 |
C13—C18—C17 | 121.1 (4) | C38—C39—H39C | 109.5 |
C13—C18—H18 | 119.4 | H39A—C39—H39B | 109.5 |
C17—C18—H18 | 119.4 | H39A—C39—H39C | 109.5 |
P2—C19—C20 | 117.1 (4) | H39B—C39—H39C | 109.5 |
P2—C19—C24 | 124.3 (4) | Cu2—N1X—H1X1 | 110.2 |
C20—C19—C24 | 118.6 (4) | Cu2—N1X—H1X2 | 110.2 |
C19—C20—H20 | 119.8 | Cu2—N1X—C37X | 107.6 (11) |
C19—C20—C21 | 120.4 (5) | H1X1—N1X—H1X2 | 108.5 |
H20—C20—C21 | 119.8 | H1X1—N1X—C37X | 110.2 |
C20—C21—H21 | 119.8 | H1X2—N1X—C37X | 110.2 |
C20—C21—C22 | 120.3 (6) | Cu2—N2X—H2X1 | 110.1 |
H21—C21—C22 | 119.8 | Cu2—N2X—H2X2 | 110.1 |
C21—C22—H22 | 119.7 | Cu2—N2X—C38X | 108.1 (14) |
C21—C22—C23 | 120.5 (5) | H2X1—N2X—H2X2 | 108.4 |
H22—C22—C23 | 119.7 | H2X1—N2X—C38X | 110.1 |
C22—C23—H23 | 120.4 | H2X2—N2X—C38X | 110.1 |
C22—C23—C24 | 119.2 (5) | N1X—C37X—H37C | 109.7 |
H23—C23—C24 | 120.4 | N1X—C37X—H37D | 109.7 |
C19—C24—C23 | 120.9 (5) | N1X—C37X—C38X | 110 (2) |
C19—C24—H24 | 119.5 | H37C—C37X—H37D | 108.2 |
C23—C24—H24 | 119.5 | H37C—C37X—C38X | 109.7 |
P2—C25—C26 | 117.9 (4) | H37D—C37X—C38X | 109.7 |
P2—C25—C30 | 123.4 (4) | N2X—C38X—C37X | 106 (2) |
C26—C25—C30 | 118.7 (5) | N2X—C38X—H38X | 109.4 |
C25—C26—H26 | 120.1 | N2X—C38X—C39X | 111 (2) |
C25—C26—C27 | 119.9 (5) | C37X—C38X—H38X | 109.4 |
H26—C26—C27 | 120.1 | C37X—C38X—C39X | 112 (2) |
C26—C27—H27 | 119.6 | H38X—C38X—C39X | 109.4 |
C26—C27—C28 | 120.9 (6) | C38X—C39X—H39D | 109.5 |
H27—C27—C28 | 119.6 | C38X—C39X—H39E | 109.5 |
C27—C28—H28 | 120.4 | C38X—C39X—H39F | 109.5 |
C27—C28—C29 | 119.2 (5) | H39D—C39X—H39E | 109.5 |
H28—C28—C29 | 120.4 | H39D—C39X—H39F | 109.5 |
C28—C29—H29 | 119.6 | H39E—C39X—H39F | 109.5 |
C28—C29—C30 | 120.7 (5) | N3—C40—C41 | 179.0 (11) |
H29—C29—C30 | 119.6 | C40—C41—H41A | 109.5 |
C25—C30—C29 | 120.5 (5) | C40—C41—H41B | 109.5 |
C25—C30—H30 | 119.7 | C40—C41—H41C | 109.5 |
C29—C30—H30 | 119.7 | H41A—C41—H41B | 109.5 |
P2—C31—C32 | 125.0 (4) | H41A—C41—H41C | 109.5 |
P2—C31—C36 | 117.3 (3) | H41B—C41—H41C | 109.5 |
C32—C31—C36 | 117.7 (4) | ||
Cl1—Cu1—Cl2—Cu2 | −42.00 (6) | C24—C19—C20—C21 | 2.4 (8) |
P1—Cu1—Cl2—Cu2 | 75.56 (6) | C19—C20—C21—C22 | −0.1 (9) |
P2—Cu1—Cl2—Cu2 | −152.08 (5) | C20—C21—C22—C23 | −1.1 (10) |
Cl1—Cu1—P1—C1 | 43.17 (17) | C21—C22—C23—C24 | −0.1 (9) |
Cl1—Cu1—P1—C7 | 161.75 (15) | P2—C19—C24—C23 | 173.8 (4) |
Cl1—Cu1—P1—C13 | −76.36 (16) | C20—C19—C24—C23 | −3.7 (7) |
Cl2—Cu1—P1—C1 | −67.31 (17) | C22—C23—C24—C19 | 2.5 (8) |
Cl2—Cu1—P1—C7 | 51.28 (16) | Cu1—P2—C25—C26 | −26.0 (4) |
Cl2—Cu1—P1—C13 | 173.17 (16) | Cu1—P2—C25—C30 | 154.0 (3) |
P2—Cu1—P1—C1 | 169.53 (17) | C19—P2—C25—C26 | −151.4 (4) |
P2—Cu1—P1—C7 | −71.88 (16) | C19—P2—C25—C30 | 28.6 (4) |
P2—Cu1—P1—C13 | 50.00 (17) | C31—P2—C25—C26 | 103.1 (4) |
Cl1—Cu1—P2—C19 | −36.71 (18) | C31—P2—C25—C30 | −77.0 (4) |
Cl1—Cu1—P2—C25 | −155.27 (17) | P2—C25—C26—C27 | −179.3 (4) |
Cl1—Cu1—P2—C31 | 82.45 (16) | C30—C25—C26—C27 | 0.7 (7) |
Cl2—Cu1—P2—C19 | 70.02 (18) | C25—C26—C27—C28 | 1.2 (9) |
Cl2—Cu1—P2—C25 | −48.54 (17) | C26—C27—C28—C29 | −1.8 (9) |
Cl2—Cu1—P2—C31 | −170.83 (16) | C27—C28—C29—C30 | 0.4 (8) |
P1—Cu1—P2—C19 | −165.73 (17) | C28—C29—C30—C25 | 1.6 (8) |
P1—Cu1—P2—C25 | 75.71 (17) | P2—C25—C30—C29 | 178.0 (4) |
P1—Cu1—P2—C31 | −46.57 (17) | C26—C25—C30—C29 | −2.1 (7) |
Cu1—P1—C1—C2 | 140.6 (3) | Cu1—P2—C31—C32 | 134.9 (3) |
Cu1—P1—C1—C6 | −42.7 (4) | Cu1—P2—C31—C36 | −44.1 (4) |
C7—P1—C1—C2 | 14.6 (4) | C19—P2—C31—C32 | −99.4 (4) |
C7—P1—C1—C6 | −168.7 (4) | C19—P2—C31—C36 | 81.6 (4) |
C13—P1—C1—C2 | −91.6 (4) | C25—P2—C31—C32 | 5.6 (4) |
C13—P1—C1—C6 | 85.1 (4) | C25—P2—C31—C36 | −173.4 (3) |
P1—C1—C2—C3 | 177.5 (4) | P2—C31—C32—C33 | −179.8 (4) |
C6—C1—C2—C3 | 0.8 (7) | C36—C31—C32—C33 | −0.9 (7) |
C1—C2—C3—C4 | −1.6 (8) | C31—C32—C33—C34 | 0.9 (8) |
C2—C3—C4—C5 | 1.5 (9) | C32—C33—C34—C35 | −0.7 (8) |
C3—C4—C5—C6 | −0.6 (9) | C33—C34—C35—C36 | 0.4 (8) |
C4—C5—C6—C1 | −0.2 (9) | C34—C35—C36—C31 | −0.4 (8) |
P1—C1—C6—C5 | −176.7 (4) | P2—C31—C36—C35 | 179.7 (4) |
C2—C1—C6—C5 | 0.1 (7) | C32—C31—C36—C35 | 0.6 (7) |
Cu1—P1—C7—C8 | −41.7 (4) | Cu1—Cl2—Cu2—N1 | −153.1 (3) |
Cu1—P1—C7—C12 | 140.8 (3) | Cu1—Cl2—Cu2—N1i | 26.9 (3) |
C1—P1—C7—C8 | 83.6 (4) | Cu1—Cl2—Cu2—N2 | −68.8 (3) |
C1—P1—C7—C12 | −93.8 (4) | Cu1—Cl2—Cu2—N2i | 111.2 (3) |
C13—P1—C7—C8 | −171.0 (3) | Cu1—Cl2—Cu2—N1X | −47.7 (5) |
C13—P1—C7—C12 | 11.6 (4) | Cu1—Cl2—Cu2—N1Xi | 132.3 (5) |
P1—C7—C8—C9 | −175.8 (4) | Cu1—Cl2—Cu2—N2X | −132.6 (5) |
C12—C7—C8—C9 | 1.8 (7) | Cu1—Cl2—Cu2—N2Xi | 47.4 (5) |
C7—C8—C9—C10 | −1.8 (7) | Cl2—Cu2—N1—C37 | 73.0 (7) |
C8—C9—C10—C11 | 0.1 (7) | Cl2i—Cu2—N1—C37 | −107.0 (7) |
C9—C10—C11—C12 | 1.6 (7) | N2—Cu2—N1—C37 | −14.1 (7) |
P1—C7—C12—C11 | 177.4 (3) | N2i—Cu2—N1—C37 | 165.9 (7) |
C8—C7—C12—C11 | 0.0 (6) | Cl2—Cu2—N2—C38 | −106.5 (9) |
C10—C11—C12—C7 | −1.6 (7) | Cl2i—Cu2—N2—C38 | 73.5 (9) |
Cu1—P1—C13—C14 | 124.8 (4) | N1—Cu2—N2—C38 | −13.3 (9) |
Cu1—P1—C13—C18 | −54.2 (4) | N1i—Cu2—N2—C38 | 166.7 (9) |
C1—P1—C13—C14 | −1.3 (4) | Cu2—N1—C37—C38 | 40.1 (12) |
C1—P1—C13—C18 | 179.7 (4) | N1—C37—C38—N2 | −52.5 (16) |
C7—P1—C13—C14 | −106.9 (4) | N1—C37—C38—C39 | −175.5 (11) |
C7—P1—C13—C18 | 74.1 (4) | Cu2—N2—C38—C37 | 39.0 (15) |
P1—C13—C14—C15 | −178.3 (4) | Cu2—N2—C38—C39 | 162.3 (9) |
C18—C13—C14—C15 | 0.6 (7) | Cl2—Cu2—N1X—C37X | −104.8 (12) |
C13—C14—C15—C16 | −0.7 (8) | Cl2i—Cu2—N1X—C37X | 75.2 (12) |
C14—C15—C16—C17 | −0.3 (8) | N2X—Cu2—N1X—C37X | −11.3 (13) |
C15—C16—C17—C18 | 1.3 (8) | N2Xi—Cu2—N1X—C37X | 168.7 (13) |
C16—C17—C18—C13 | −1.4 (7) | Cl2—Cu2—N2X—C38X | 75.9 (14) |
P1—C13—C18—C17 | 179.4 (4) | Cl2i—Cu2—N2X—C38X | −104.1 (14) |
C14—C13—C18—C17 | 0.4 (7) | N1X—Cu2—N2X—C38X | −17.4 (14) |
Cu1—P2—C19—C20 | −37.6 (4) | N1Xi—Cu2—N2X—C38X | 162.6 (14) |
Cu1—P2—C19—C24 | 145.0 (4) | Cu2—N1X—C37X—C38X | 39 (2) |
C25—P2—C19—C20 | 89.4 (4) | N1X—C37X—C38X—N2X | −54 (3) |
C25—P2—C19—C24 | −88.1 (4) | N1X—C37X—C38X—C39X | −174.9 (19) |
C31—P2—C19—C20 | −164.5 (4) | Cu2—N2X—C38X—C37X | 42 (2) |
C31—P2—C19—C24 | 18.1 (4) | Cu2—N2X—C38X—C39X | 163.5 (14) |
P2—C19—C20—C21 | −175.2 (4) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···Cl1i | 0.92 | 2.45 | 3.330 (9) | 159 |
N2X—H2X1···Cl1i | 0.92 | 2.60 | 3.495 (15) | 163 |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Cu3Cl4(C3H10N2)2(C18H15P)4]·2C2H3N |
Mr | 1611.87 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 150 |
a, b, c (Å) | 15.896 (3), 9.4181 (15), 26.533 (4) |
β (°) | 94.957 (12) |
V (Å3) | 3957.4 (11) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.06 |
Crystal size (mm) | 0.25 × 0.20 × 0.20 |
Data collection | |
Diffractometer | Nonius KappaCCD |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2007) |
Tmin, Tmax | 0.780, 0.820 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 32758, 6923, 5038 |
Rint | 0.074 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.054, 0.158, 1.03 |
No. of reflections | 6923 |
No. of parameters | 496 |
No. of restraints | 136 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.78, −0.81 |
Computer programs: COLLECT (Nonius, 1998), EVALCCD (Duisenberg et al., 2003), EVALCCD, SHELXTL (Sheldrick, 2005), SHELXTL and local programs.
Cu1—Cl1 | 2.3553 (13) | Cu2—N1 | 2.042 (10) |
Cu1—Cl2 | 2.4372 (13) | Cu2—N2 | 1.995 (10) |
Cu1—P1 | 2.2800 (13) | Cu2—N1X | 2.065 (14) |
Cu1—P2 | 2.2835 (12) | Cu2—N2X | 1.995 (18) |
Cu2—Cl2 | 2.8731 (12) | ||
Cl1—Cu1—Cl2 | 101.06 (5) | Cl2—Cu2—N1 | 92.9 (3) |
Cl1—Cu1—P1 | 111.76 (5) | Cl2—Cu2—N2 | 87.4 (3) |
Cl1—Cu1—P2 | 105.75 (5) | Cl2—Cu2—N1X | 93.6 (4) |
Cl2—Cu1—P1 | 108.31 (5) | Cl2—Cu2—N2X | 93.8 (5) |
Cl2—Cu1—P2 | 105.94 (5) | N1—Cu2—N2 | 84.4 (4) |
P1—Cu1—P2 | 121.92 (4) | N1X—Cu2—N2X | 84.7 (6) |
Cu1—Cl2—Cu2 | 122.71 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···Cl1i | 0.92 | 2.45 | 3.330 (9) | 159 |
N2X—H2X1···Cl1i | 0.92 | 2.60 | 3.495 (15) | 163 |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Trinuclear metal complexes can be classified as linear and non-linear. Trinuclear copper complexes with two, three or four bridges (Prins et al., 1996; Feng et al., 2007; Onan et al., 1984; Choi et al., 2006) have been reported. There are also some reported singly-bridged copper complexes (Arrizabalaga et al., 1983; Bailey et al., 1995). We report here the crystal structure of a new linear trinuclear mixed-valence copper compound, (I) (Fig. 1). It contains two CuI atoms with distorted tetrahedral coordination, the four vertices being occupied by two P atoms of PPh3 ligands and two Cl atoms. The largest deviation from ideal tetrahedral geometry is the wide P—Cu—P angle of 121.92 (4)°. The central CuII atom lies on an inversion centre and has octahedral coordination, with two chelating bidentate diamines and two trans-chloro bridges to the CuI atoms. The diamine ligands are disordered over two orientations, with refined occupancy factors of 0.599:0.401 (10). Each of them forms one N—H···Cl hydrogen bond to a terminal Cl atom. The Cu—Cl bonds for the central CuII atom are elongated as a result of a typical Jahn-Teller distortion, and the bridging Cl atoms make longer bonds to the CuI atoms than do the terminal Cl atoms, as expected. There are no significant intermolecular interactions, and acetonitrile solvent molecules simply occupy what would otherwise be voids in the structure.