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Acta Cryst. (2007). E63, m1993-m1994    [ doi:10.1107/S1600536807030450 ]

Bis(1,10-phenanthroline-[kappa]2N,N')copper(I) chloridobis(1,10-phenanthroline-[kappa]2N,N')copper(II) hexacosaoxidooctamolybdate(VI) dihydrate

W.-J. Wang and L. Xu

Abstract top

The title complex, [CuIICl(C12H8N2)2]2[CuI(C12H8N2)2]2[Mo8O26]·2H2O, features a centrosymmetric [alpha]-type octamolybdate anion, two complex copper counter-cations with Cu in oxidation states +II and +I, and two water molecules of crystallization. The CuII ion exhibits a distorted CuN4Cl square-pyramidal coordination, whereas the CuI ion is in a distorted tetrahedral CuN4 coordination. The anions, cations and uncoordinated water molecules are linked into a three-dimensional network by O-H...O and C-H...O hydrogen bonds.

Comment top

Recently, polyoxomolybdates (POM) containing transition-metal complexes have been extensively investigated (Allis et al., 2004). Among the syntheses of these inorganic-organic hybrids, the hydrothermal method is an effective method. To further explore this synthetic approach for new POM structures, the title complex, (I), is reported here.

The structure of complex (I) contains a [Mo8O26]4− anion, two [CuII(phen)2Cl]+ and [CuI(phen)2]+ (phen = 1,10-phenantroline) counter cations, and isolated water molecules. The centrosymmetric [Mo8O26]4− cluster (Fig. 1) is of the α-type and is made up of a ring of six edge-sharing MoO6 octahedra, bicapped by two trans-MoO4 tetrahedra. In the [CuII(phen)2Cl]+ complex cation, Cu1II exhibits a distorted CuN4Cl square-pyramidal coordination to four N atoms from two phen ligands and to one Cl atom. The Cu2I cation in the [CuI(phen)2]+ complex is coordinated by four N atoms from two phen ligands forming a considerably distorted CuN4 tetrahedron. The Mo—O, Cu—N, and Cu—Cl distances are in the range 1.692 (2) to 2.499 (3) Å, 1.984 (3) to 2.177 (3) Å, and 2.2750 (12) Å, respectively. Bond valence sum (BVS) calculations (Brown & Altermatt, 1985) are close to the expected oxidation states, with 5.95 to 6.07 valence units (v.u.) for the Mo atoms (expected 6), 2.25 v.u. for Cu1II (expected 2), and 0.99 for Cu2I (expected 1).

Hydrogen bonding (Table 2) of the type O—H···O and C—H···O between the anions, cations, and the isolated water molecules consolidates the structure into a three-dimensional framework, as shown in Fig. 2.

Related literature top

For recent studies of other polyoxamolybdates, see Allis et al. (2004). The bond valence sums (BVS) were calculated according to Brown & Altermatt (1985).

Experimental top

All employed reagents were purchased from Shanghai Reagent Company with analytical purity. Na2MoO4.2H2O (1 g, 4.1 mmol), Cu(CH3COO)2.2H2O (0.1 g, 0.5 mmol), and phen (0.4 g, 2 mmol) were dissolved in 10 ml 0.2 M HCl under stirring. The suspension was then placed in a 20-ml Teflon-lined reactor. After heating the mixture for 7 d at 413 K, blue block-like crystals of (I) were obtained.

Refinement top

The aromatic H atoms were placed at calculated positions (C—H = 0.93 Å) and were allowed to ride on their carrier atoms with U(H)iso=1.2U(C)eq. The H atoms of the water molecules were located in difference Fourier maps and refined in their as-found relative positions with distances between 0.86–0.93 Å using a riding model with U(H)iso = 1.2U(O)eq.

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The cationic and anionic moieties of (I). Displacement ellipsoids are drawn at the 30% probability level. [Symmetry code: (i) 1 − x, −y, 1 − z.]
[Figure 2] Fig. 2. The unit cell packing of (I).
Bis(1,10-phenanthroline-κ2N,N')copper(I) chloridobis(1,10-phenanthroline-κ2N,N')copper(II) hexacosaoxidooctamolybdate(VI) dihydrate top
Crystal data top
[CuCl(C12H8N2)2]2[Cu(C12H8N2)2]2[Mo8O26]·2H2OZ = 1
Mr = 2986.29F000 = 1466
Triclinic, P1Dx = 2.016 Mg m−3
Hall symbol: -P 1Mo Kα radiation
λ = 0.71073 Å
a = 12.442 (2) ÅCell parameters from 13762 reflections
b = 13.604 (2) Åθ = 1.8–27.5º
c = 14.902 (3) ŵ = 1.97 mm−1
α = 101.115 (4)ºT = 295 (2) K
β = 91.514 (3)ºBlock, blue
γ = 95.880 (3)º0.21 × 0.20 × 0.12 mm
V = 2459.2 (7) Å3
Data collection top
Bruker SMART CCD APEXII
diffractometer		9614 independent reflections
Radiation source: fine-focus sealed tube7435 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.038
T = 295(2) Kθmax = 26.0º
ω and φ scansθmin = 3.1º
Absorption correction: multi-scan
(SADABS; Bruker, 2002)		h = −15→15
Tmin = 0.665, Tmax = 0.780k = −16→16
21242 measured reflectionsl = −18→18
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.032H-atom parameters constrained
wR(F2) = 0.072  w = 1/[σ2(Fo2) + (0.0315P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max < 0.001
9614 reflectionsΔρmax = 0.41 e Å−3
694 parametersΔρmin = −0.61 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[CuCl(C12H8N2)2]2[Cu(C12H8N2)2]2[Mo8O26]·2H2Oγ = 95.880 (3)º
Mr = 2986.29V = 2459.2 (7) Å3
Triclinic, P1Z = 1
a = 12.442 (2) ÅMo Kα
b = 13.604 (2) ŵ = 1.97 mm−1
c = 14.902 (3) ÅT = 295 (2) K
α = 101.115 (4)º0.21 × 0.20 × 0.12 mm
β = 91.514 (3)º
Data collection top
Bruker SMART CCD APEXII
diffractometer		9614 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2002)		7435 reflections with I > 2σ(I)
Tmin = 0.665, Tmax = 0.780Rint = 0.038
21242 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.032694 parameters
wR(F2) = 0.072H-atom parameters constrained
S = 1.05Δρmax = 0.41 e Å−3
9614 reflectionsΔρmin = −0.61 e Å−3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo10.55938 (2)0.120262 (19)0.47442 (2)0.02134 (8)
Mo20.74571 (3)−0.07803 (2)0.51262 (2)0.02540 (8)
Mo30.39186 (3)0.11660 (2)0.69193 (2)0.02685 (8)
Mo40.64840 (3)0.05475 (2)0.70119 (2)0.02548 (8)
Cu10.18668 (4)0.53747 (3)0.73391 (3)0.02875 (11)
Cu20.21367 (5)0.27923 (4)0.09753 (4)0.04924 (15)
Cl0.11512 (10)0.56271 (8)0.87436 (8)0.0495 (3)
O10.6114 (2)0.23538 (17)0.45726 (19)0.0366 (7)
O20.5459 (2)0.14846 (16)0.70242 (17)0.0288 (6)
O30.6537 (2)0.07276 (16)0.54355 (16)0.0275 (6)
O40.6891 (2)−0.06733 (16)0.63143 (16)0.0265 (5)
O50.3618 (2)0.07120 (18)0.78738 (18)0.0384 (7)
O60.4365 (2)0.13368 (17)0.53276 (17)0.0302 (6)
O70.8682 (2)−0.0108 (2)0.5401 (2)0.0426 (7)
O80.7720 (2)−0.19996 (18)0.49288 (19)0.0397 (7)
O90.4689 (2)−0.03415 (16)0.63208 (17)0.0288 (6)
O100.2756 (2)0.05199 (17)0.60866 (17)0.0294 (6)
O110.6279 (2)0.01793 (19)0.80289 (18)0.0377 (7)
O120.3585 (2)0.23607 (17)0.7153 (2)0.0402 (7)
O130.7656 (2)0.13251 (19)0.71968 (19)0.0390 (7)
OW0.0927 (6)0.8909 (4)0.6132 (4)0.165 (3)
H1W0.12920.95320.61080.198*
H2W0.02890.88850.58800.198*
N10.3242 (2)0.49721 (19)0.6666 (2)0.0248 (6)
N20.1075 (3)0.3999 (2)0.6983 (2)0.0336 (8)
N30.0507 (3)0.5696 (2)0.6534 (2)0.0360 (8)
N40.2758 (3)0.4229 (2)0.1511 (2)0.0386 (8)
N50.2740 (3)0.6711 (2)0.7577 (2)0.0322 (8)
N60.3669 (3)0.2700 (2)0.0528 (2)0.0395 (8)
N70.0811 (3)0.2755 (2)0.0120 (2)0.0381 (8)
N80.1195 (3)0.1703 (2)0.1429 (2)0.0363 (8)
C10.5395 (3)0.3730 (3)0.0581 (3)0.0402 (10)
C20.4044 (3)0.5759 (2)0.6806 (2)0.0252 (8)
C3−0.0922 (4)0.1766 (3)−0.0322 (3)0.0433 (10)
C40.0147 (3)0.3924 (3)0.6471 (3)0.0342 (9)
C50.3761 (3)0.6697 (2)0.7290 (2)0.0268 (8)
C60.4517 (3)0.7547 (3)0.7449 (3)0.0311 (9)
C70.4304 (3)0.3587 (3)0.0796 (3)0.0328 (9)
C8−0.1153 (4)0.4805 (4)0.5745 (3)0.0467 (11)
C90.3806 (3)0.4410 (3)0.1307 (3)0.0325 (9)
C100.2811 (5)0.5963 (3)0.2206 (3)0.0585 (14)
H100.24450.64820.25090.070*
C110.3486 (3)0.4095 (2)0.6197 (3)0.0320 (9)
H110.29470.35530.60770.038*
C12−0.0767 (4)0.6581 (4)0.5864 (3)0.0593 (15)
H12−0.09570.71920.57550.071*
C130.5502 (4)0.5474 (3)0.1329 (3)0.0499 (12)
H130.58980.61040.14970.060*
C140.4405 (4)0.5360 (3)0.1564 (3)0.0408 (10)
C150.3139 (4)0.8467 (3)0.8150 (3)0.0557 (14)
H150.28950.90710.84280.067*
C16−0.0132 (4)0.2146 (3)0.6412 (4)0.0569 (14)
H16−0.05310.15210.62190.068*
C17−0.0180 (3)0.4838 (3)0.6247 (3)0.0355 (9)
C180.0585 (4)0.3337 (3)−0.0460 (3)0.0521 (12)
H180.10920.3875−0.05080.062*
C190.0269 (3)0.1424 (3)0.0902 (3)0.0326 (9)
C200.1382 (4)0.3162 (3)0.7199 (3)0.0415 (11)
H200.20140.32090.75590.050*
C21−0.0245 (4)0.0114 (3)0.1713 (4)0.0543 (13)
H21−0.0721−0.04230.18140.065*
C22−0.1800 (4)0.3849 (4)0.5459 (3)0.0597 (14)
H22−0.24530.38190.51310.072*
C230.0041 (3)0.1999 (3)0.0214 (3)0.0329 (9)
C24−0.1094 (4)0.2405 (4)−0.0941 (3)0.0562 (13)
H24−0.17220.2285−0.13160.067*
C250.4181 (4)0.8454 (3)0.7888 (3)0.0454 (12)
H250.46570.90410.80000.054*
C260.5586 (3)0.7450 (3)0.7127 (3)0.0417 (10)
H260.60970.80130.72300.050*
C27−0.1482 (4)0.3006 (4)0.5655 (3)0.0621 (15)
H27−0.19070.23970.54440.075*
C280.0799 (4)0.2219 (3)0.6910 (4)0.0522 (13)
H280.10510.16480.70590.063*
C290.5081 (3)0.5680 (3)0.6501 (3)0.0343 (9)
C30−0.0352 (5)0.3193 (4)−0.0994 (3)0.0611 (14)
H30−0.04780.3628−0.13860.073*
C310.4503 (4)0.3952 (3)0.5881 (3)0.0459 (12)
H310.46440.33200.55710.055*
C320.0673 (4)0.0393 (3)0.2246 (4)0.0558 (13)
H320.08300.00550.27120.067*
C33−0.1430 (4)0.5724 (5)0.5569 (3)0.0626 (15)
H33−0.20740.57430.52450.075*
C34−0.0503 (4)0.3012 (3)0.6183 (3)0.0454 (11)
C350.5864 (3)0.6571 (3)0.6685 (3)0.0445 (11)
H350.65650.65270.64920.053*
C360.5200 (5)0.2028 (4)−0.0215 (4)0.0658 (15)
H360.54780.1482−0.05710.079*
C370.5992 (4)0.4702 (4)0.0870 (3)0.0522 (13)
H370.67170.48020.07410.063*
C380.0218 (4)0.6541 (3)0.6342 (3)0.0484 (12)
H380.06800.71320.65270.058*
C390.1380 (4)0.1196 (3)0.2086 (3)0.0460 (11)
H390.20100.13860.24560.055*
C400.3853 (5)0.6149 (3)0.2028 (3)0.0539 (13)
H400.42110.67950.22090.065*
C410.5838 (4)0.2910 (4)0.0069 (3)0.0550 (13)
H410.65610.2968−0.00760.066*
C42−0.0492 (3)0.0616 (3)0.1013 (3)0.0407 (10)
C430.2444 (4)0.7583 (3)0.8004 (3)0.0494 (12)
H430.17470.76010.82120.059*
C440.5293 (4)0.4732 (3)0.6022 (3)0.0478 (12)
H440.59750.46410.58020.057*
C45−0.1650 (4)0.0919 (4)−0.0218 (3)0.0529 (12)
H45−0.22800.0746−0.05880.063*
C460.2274 (4)0.5000 (3)0.1941 (3)0.0542 (13)
H460.15490.48900.20680.065*
C47−0.1435 (4)0.0372 (3)0.0408 (4)0.0525 (13)
H47−0.1915−0.01860.04520.063*
C480.4124 (4)0.1944 (3)0.0030 (3)0.0561 (13)
H480.37040.1330−0.01650.067*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.02267 (17)0.01487 (13)0.02523 (17)−0.00025 (11)−0.00352 (13)0.00268 (12)
Mo20.02224 (18)0.02282 (15)0.02934 (18)0.00244 (12)−0.00481 (14)0.00147 (13)
Mo30.02799 (19)0.02052 (15)0.03045 (18)0.00442 (12)−0.00292 (14)0.00071 (13)
Mo40.02487 (18)0.02240 (15)0.02754 (18)0.00159 (12)−0.00516 (14)0.00228 (13)
Cu10.0234 (3)0.0210 (2)0.0403 (3)−0.00076 (17)0.0026 (2)0.00364 (19)
Cu20.0349 (3)0.0446 (3)0.0647 (4)−0.0091 (2)−0.0045 (3)0.0101 (3)
Cl0.0579 (8)0.0440 (5)0.0462 (7)0.0020 (5)0.0203 (6)0.0074 (5)
O10.0411 (18)0.0226 (12)0.0440 (17)−0.0079 (11)−0.0104 (14)0.0091 (12)
O20.0283 (15)0.0196 (11)0.0344 (15)0.0022 (10)−0.0070 (12)−0.0036 (10)
O30.0306 (15)0.0258 (12)0.0265 (14)0.0068 (10)−0.0041 (11)0.0045 (10)
O40.0275 (15)0.0244 (12)0.0277 (14)0.0034 (10)−0.0055 (11)0.0060 (10)
O50.0496 (19)0.0359 (14)0.0289 (15)0.0059 (13)0.0032 (13)0.0038 (12)
O60.0264 (15)0.0298 (12)0.0306 (15)0.0023 (11)−0.0051 (12)−0.0022 (11)
O70.0272 (16)0.0446 (15)0.0515 (19)−0.0059 (12)−0.0045 (14)0.0045 (14)
O80.0445 (19)0.0272 (13)0.0468 (18)0.0123 (12)−0.0096 (14)0.0027 (12)
O90.0369 (16)0.0223 (11)0.0268 (14)0.0074 (11)−0.0029 (12)0.0023 (10)
O100.0287 (15)0.0292 (12)0.0286 (14)0.0003 (11)0.0019 (12)0.0031 (11)
O110.0388 (17)0.0405 (14)0.0347 (16)0.0041 (12)−0.0017 (13)0.0101 (12)
O120.0381 (18)0.0266 (13)0.0524 (19)0.0079 (12)−0.0054 (14)−0.0019 (12)
O130.0331 (17)0.0385 (14)0.0398 (17)−0.0067 (12)−0.0082 (13)0.0006 (12)
OW0.213 (7)0.127 (4)0.152 (6)−0.030 (4)0.083 (5)0.037 (4)
N10.0259 (17)0.0219 (14)0.0268 (17)0.0028 (12)0.0002 (13)0.0054 (12)
N20.0262 (19)0.0266 (15)0.046 (2)−0.0013 (13)0.0060 (16)0.0047 (15)
N30.031 (2)0.0383 (17)0.040 (2)0.0071 (15)0.0026 (16)0.0089 (15)
N40.044 (2)0.0366 (17)0.033 (2)0.0022 (16)0.0020 (17)0.0031 (15)
N50.033 (2)0.0191 (14)0.042 (2)−0.0008 (13)0.0083 (16)0.0000 (13)
N60.037 (2)0.0353 (17)0.043 (2)0.0013 (15)−0.0011 (17)0.0006 (15)
N70.037 (2)0.0401 (18)0.038 (2)0.0047 (15)0.0007 (16)0.0075 (16)
N80.030 (2)0.0353 (17)0.044 (2)0.0050 (14)−0.0040 (16)0.0077 (16)
C10.032 (2)0.056 (2)0.034 (2)−0.0001 (19)−0.0048 (19)0.016 (2)
C20.024 (2)0.0277 (17)0.0243 (19)0.0025 (15)0.0012 (16)0.0062 (15)
C30.036 (3)0.054 (2)0.034 (2)0.015 (2)−0.003 (2)−0.011 (2)
C40.025 (2)0.038 (2)0.035 (2)−0.0075 (16)0.0064 (18)0.0011 (17)
C50.027 (2)0.0281 (17)0.026 (2)−0.0007 (15)0.0005 (16)0.0085 (15)
C60.036 (2)0.0279 (18)0.029 (2)−0.0078 (16)−0.0032 (18)0.0108 (16)
C70.031 (2)0.036 (2)0.028 (2)−0.0037 (17)−0.0052 (18)0.0059 (17)
C80.026 (2)0.081 (3)0.032 (2)0.013 (2)0.006 (2)0.007 (2)
C90.038 (2)0.0321 (19)0.026 (2)0.0010 (17)−0.0038 (18)0.0062 (16)
C100.091 (5)0.037 (2)0.048 (3)0.021 (3)0.007 (3)0.001 (2)
C110.045 (3)0.0215 (17)0.029 (2)0.0092 (16)0.0017 (18)0.0023 (15)
C120.061 (4)0.079 (4)0.052 (3)0.041 (3)0.013 (3)0.030 (3)
C130.057 (3)0.040 (2)0.049 (3)−0.018 (2)−0.018 (2)0.016 (2)
C140.053 (3)0.036 (2)0.031 (2)−0.0075 (19)−0.008 (2)0.0090 (18)
C150.066 (4)0.026 (2)0.069 (3)−0.005 (2)0.025 (3)−0.005 (2)
C160.062 (4)0.032 (2)0.066 (3)−0.020 (2)0.029 (3)−0.009 (2)
C170.025 (2)0.050 (2)0.030 (2)0.0003 (18)0.0040 (18)0.0051 (18)
C180.058 (3)0.054 (3)0.047 (3)0.007 (2)0.006 (3)0.018 (2)
C190.025 (2)0.0356 (19)0.037 (2)0.0085 (16)0.0054 (18)0.0047 (17)
C200.037 (3)0.033 (2)0.057 (3)0.0056 (18)0.010 (2)0.014 (2)
C210.053 (3)0.040 (2)0.074 (4)0.004 (2)0.022 (3)0.020 (2)
C220.023 (3)0.106 (4)0.039 (3)−0.012 (3)−0.002 (2)−0.002 (3)
C230.029 (2)0.036 (2)0.032 (2)0.0106 (17)0.0017 (18)−0.0024 (17)
C240.047 (3)0.086 (4)0.032 (3)0.027 (3)−0.009 (2)−0.005 (2)
C250.063 (3)0.0262 (19)0.042 (3)−0.0152 (19)0.007 (2)0.0037 (18)
C260.032 (2)0.041 (2)0.053 (3)−0.0110 (18)−0.007 (2)0.020 (2)
C270.042 (3)0.078 (3)0.050 (3)−0.028 (3)0.009 (3)−0.013 (3)
C280.062 (4)0.028 (2)0.069 (3)−0.001 (2)0.031 (3)0.013 (2)
C290.031 (2)0.037 (2)0.040 (2)0.0072 (17)0.0056 (19)0.0187 (19)
C300.075 (4)0.080 (4)0.034 (3)0.025 (3)0.001 (3)0.017 (3)
C310.064 (3)0.030 (2)0.048 (3)0.020 (2)0.021 (2)0.0067 (19)
C320.057 (3)0.055 (3)0.064 (3)0.010 (2)0.009 (3)0.029 (3)
C330.040 (3)0.112 (4)0.040 (3)0.028 (3)−0.001 (2)0.015 (3)
C340.036 (3)0.051 (3)0.039 (3)−0.015 (2)0.011 (2)−0.007 (2)
C350.020 (2)0.052 (3)0.066 (3)−0.0026 (18)0.009 (2)0.026 (2)
C360.069 (4)0.061 (3)0.066 (4)0.025 (3)0.013 (3)−0.001 (3)
C370.033 (3)0.071 (3)0.054 (3)−0.016 (2)−0.012 (2)0.030 (3)
C380.053 (3)0.050 (3)0.048 (3)0.020 (2)0.010 (2)0.015 (2)
C390.038 (3)0.054 (3)0.049 (3)0.010 (2)−0.009 (2)0.015 (2)
C400.089 (4)0.029 (2)0.039 (3)0.001 (2)−0.011 (3)−0.0011 (19)
C410.039 (3)0.081 (3)0.051 (3)0.016 (3)0.011 (2)0.021 (3)
C420.032 (2)0.033 (2)0.054 (3)0.0048 (18)0.011 (2)0.0014 (19)
C430.052 (3)0.0266 (19)0.068 (3)0.0042 (19)0.028 (3)0.003 (2)
C440.045 (3)0.048 (2)0.061 (3)0.027 (2)0.027 (2)0.025 (2)
C450.034 (3)0.067 (3)0.046 (3)0.009 (2)−0.005 (2)−0.017 (2)
C460.064 (4)0.049 (3)0.051 (3)0.019 (2)0.014 (3)0.006 (2)
C470.030 (3)0.046 (2)0.070 (4)−0.004 (2)0.011 (2)−0.014 (2)
C480.054 (3)0.046 (3)0.059 (3)0.004 (2)0.004 (3)−0.011 (2)
Geometric parameters (Å, °) top
Mo1—O11.701 (2)C8—C331.399 (7)
Mo1—O9i1.784 (2)C8—C221.441 (7)
Mo1—O61.786 (3)C9—C141.403 (5)
Mo1—O31.790 (2)C10—C401.338 (7)
Mo2—O71.693 (3)C10—C461.388 (6)
Mo2—O81.695 (2)C10—H100.9300
Mo2—O41.908 (2)C11—C311.382 (6)
Mo2—O10i1.924 (2)C11—H110.9300
Mo2—O6i2.354 (3)C12—C331.349 (7)
Mo2—O32.424 (2)C12—C381.411 (7)
Mo3—O121.692 (2)C12—H120.9300
Mo3—O51.692 (3)C13—C371.348 (7)
Mo3—O101.905 (3)C13—C141.418 (6)
Mo3—O21.917 (3)C13—H130.9300
Mo3—O92.380 (2)C14—C401.411 (6)
Mo3—O62.499 (3)C15—C251.364 (6)
Mo4—O131.694 (3)C15—C431.385 (6)
Mo4—O111.703 (3)C15—H150.9300
Mo4—O21.891 (2)C16—C281.343 (7)
Mo4—O41.905 (2)C16—C341.407 (7)
Mo4—O32.410 (2)C16—H160.9300
Cu1—N51.984 (3)C18—C301.369 (7)
Cu1—N21.992 (3)C18—H180.9300
Cu1—N12.075 (3)C19—C421.413 (5)
Cu1—N32.177 (3)C19—C231.443 (5)
Cu1—Cl2.2750 (12)C20—C281.391 (6)
Cu2—N82.025 (3)C20—H200.9300
Cu2—N42.028 (3)C21—C321.352 (7)
Cu2—N62.044 (4)C21—C421.397 (6)
Cu2—N72.047 (4)C21—H210.9300
O6—Mo2i2.354 (3)C22—C271.332 (7)
O9—Mo1i1.784 (2)C22—H220.9300
O10—Mo2i1.924 (2)C24—C301.358 (7)
OW—H1W0.9273C24—H240.9300
OW—H2W0.8637C25—H250.9300
N1—C111.329 (4)C26—C351.333 (6)
N1—C21.367 (4)C26—H260.9300
N2—C201.331 (5)C27—C341.430 (7)
N2—C41.351 (5)C27—H270.9300
N3—C381.318 (5)C28—H280.9300
N3—C171.364 (5)C29—C441.403 (6)
N4—C461.328 (5)C29—C351.451 (5)
N4—C91.355 (5)C30—H300.9300
N5—C431.326 (5)C31—C441.351 (6)
N5—C51.352 (5)C31—H310.9300
N6—C481.333 (5)C32—C391.392 (6)
N6—C71.357 (5)C32—H320.9300
N7—C181.323 (5)C33—H330.9300
N7—C231.362 (5)C35—H350.9300
N8—C391.330 (5)C36—C411.356 (7)
N8—C191.356 (5)C36—C481.396 (7)
C1—C411.397 (6)C36—H360.9300
C1—C71.405 (6)C37—H370.9300
C1—C371.431 (6)C38—H380.9300
C2—C291.387 (5)C39—H390.9300
C2—C51.422 (5)C40—H400.9300
C3—C231.396 (6)C41—H410.9300
C3—C241.409 (6)C42—C471.430 (6)
C3—C451.426 (6)C43—H430.9300
C4—C341.396 (5)C44—H440.9300
C4—C171.443 (5)C45—C471.339 (7)
C5—C61.392 (5)C45—H450.9300
C6—C251.391 (5)C46—H460.9300
C6—C261.435 (6)C47—H470.9300
C7—C91.434 (5)C48—H480.9300
C8—C171.398 (6)
O1—Mo1—O9i110.77 (12)N4—C9—C14122.9 (4)
O1—Mo1—O6108.63 (12)N4—C9—C7117.6 (3)
O9i—Mo1—O6108.98 (12)C14—C9—C7119.6 (4)
O1—Mo1—O3109.46 (12)C40—C10—C46120.4 (4)
O9i—Mo1—O3109.75 (11)C40—C10—H10119.8
O6—Mo1—O3109.22 (11)C46—C10—H10119.8
O7—Mo2—O8104.51 (14)N1—C11—C31122.9 (4)
O7—Mo2—O499.96 (13)N1—C11—H11118.6
O8—Mo2—O4100.05 (12)C31—C11—H11118.6
O7—Mo2—O10i98.57 (12)C33—C12—C38119.3 (4)
O8—Mo2—O10i103.19 (12)C33—C12—H12120.3
O4—Mo2—O10i145.44 (10)C38—C12—H12120.3
O7—Mo2—O6i165.89 (11)C37—C13—C14122.5 (4)
O8—Mo2—O6i88.84 (11)C37—C13—H13118.8
O4—Mo2—O6i81.81 (10)C14—C13—H13118.8
O10i—Mo2—O6i73.50 (10)C9—C14—C40116.7 (4)
O7—Mo2—O391.97 (11)C9—C14—C13118.8 (4)
O8—Mo2—O3162.84 (11)C40—C14—C13124.5 (4)
O4—Mo2—O371.92 (8)C25—C15—C43120.1 (4)
O10i—Mo2—O378.54 (9)C25—C15—H15119.9
O6i—Mo2—O375.18 (8)C43—C15—H15119.9
O12—Mo3—O5104.20 (13)C28—C16—C34120.1 (4)
O12—Mo3—O10100.90 (12)C28—C16—H16119.9
O5—Mo3—O10102.03 (12)C34—C16—H16119.9
O12—Mo3—O297.65 (12)N3—C17—C8123.7 (4)
O5—Mo3—O2104.17 (13)N3—C17—C4116.7 (4)
O10—Mo3—O2142.88 (11)C8—C17—C4119.6 (4)
O12—Mo3—O9165.05 (11)N7—C18—C30123.7 (5)
O5—Mo3—O989.52 (10)N7—C18—H18118.1
O10—Mo3—O981.60 (9)C30—C18—H18118.1
O2—Mo3—O972.83 (9)N8—C19—C42123.0 (4)
O12—Mo3—O690.89 (11)N8—C19—C23118.2 (3)
O5—Mo3—O6164.31 (10)C42—C19—C23118.8 (4)
O10—Mo3—O670.35 (9)N2—C20—C28122.9 (5)
O2—Mo3—O677.53 (10)N2—C20—H20118.6
O9—Mo3—O675.97 (8)C28—C20—H20118.6
O13—Mo4—O11104.46 (13)C32—C21—C42121.2 (4)
O13—Mo4—O2101.17 (12)C32—C21—H21119.4
O11—Mo4—O2101.42 (12)C42—C21—H21119.4
O13—Mo4—O4103.89 (12)C27—C22—C8121.3 (5)
O11—Mo4—O499.44 (11)C27—C22—H22119.3
O2—Mo4—O4142.00 (10)C8—C22—H22119.3
O13—Mo4—O386.90 (11)N7—C23—C3123.2 (4)
O11—Mo4—O3167.48 (11)N7—C23—C19116.5 (4)
O2—Mo4—O381.10 (9)C3—C23—C19120.3 (4)
O4—Mo4—O372.28 (8)C30—C24—C3120.6 (5)
N5—Cu1—N2174.07 (13)C30—C24—H24119.7
N5—Cu1—N180.90 (12)C3—C24—H24119.7
N2—Cu1—N193.84 (12)C15—C25—C6118.9 (4)
N5—Cu1—N3100.17 (13)C15—C25—H25120.6
N2—Cu1—N379.86 (13)C6—C25—H25120.6
N1—Cu1—N3118.23 (12)C35—C26—C6121.6 (4)
N5—Cu1—Cl93.57 (10)C35—C26—H26119.2
N2—Cu1—Cl92.28 (10)C6—C26—H26119.2
N1—Cu1—Cl142.65 (9)C22—C27—C34121.7 (5)
N3—Cu1—Cl99.12 (10)C22—C27—H27119.2
N8—Cu2—N4135.47 (14)C34—C27—H27119.2
N8—Cu2—N6126.33 (13)C16—C28—C20119.1 (4)
N4—Cu2—N682.10 (13)C16—C28—H28120.4
N8—Cu2—N782.78 (13)C20—C28—H28120.4
N4—Cu2—N7111.32 (13)C2—C29—C44116.8 (4)
N6—Cu2—N7123.38 (14)C2—C29—C35118.7 (4)
Mo4—O2—Mo3125.75 (12)C44—C29—C35124.5 (4)
Mo1—O3—Mo4130.38 (12)C24—C30—C18118.9 (5)
Mo1—O3—Mo2131.05 (12)C24—C30—H30120.5
Mo4—O3—Mo288.10 (7)C18—C30—H30120.5
Mo4—O4—Mo2123.63 (11)C44—C31—C11119.9 (4)
Mo1—O6—Mo2i132.46 (13)C44—C31—H31120.1
Mo1—O6—Mo3130.64 (12)C11—C31—H31120.1
Mo2i—O6—Mo388.22 (8)C21—C32—C39118.9 (4)
Mo1i—O9—Mo3129.93 (12)C21—C32—H32120.6
Mo3—O10—Mo2i123.90 (12)C39—C32—H32120.6
H1W—OW—H2W107.4C12—C33—C8120.4 (5)
C11—N1—C2117.0 (3)C12—C33—H33119.8
C11—N1—Cu1131.6 (3)C8—C33—H33119.8
C2—N1—Cu1111.2 (2)C4—C34—C16117.2 (4)
C20—N2—C4118.0 (3)C4—C34—C27118.7 (4)
C20—N2—Cu1125.9 (3)C16—C34—C27124.0 (4)
C4—N2—Cu1116.1 (2)C26—C35—C29120.6 (4)
C38—N3—C17117.6 (4)C26—C35—H35119.7
C38—N3—Cu1132.4 (3)C29—C35—H35119.7
C17—N3—Cu1109.8 (2)C41—C36—C48119.8 (5)
C46—N4—C9118.0 (4)C41—C36—H36120.1
C46—N4—Cu2129.9 (3)C48—C36—H36120.1
C9—N4—Cu2111.8 (2)C13—C37—C1120.0 (4)
C43—N5—C5118.0 (3)C13—C37—H37120.0
C43—N5—Cu1127.5 (3)C1—C37—H37120.0
C5—N5—Cu1114.5 (2)N3—C38—C12122.4 (5)
C48—N6—C7116.8 (4)N3—C38—H38118.8
C48—N6—Cu2131.6 (3)C12—C38—H38118.8
C7—N6—Cu2111.6 (3)N8—C39—C32122.9 (4)
C18—N7—C23117.4 (4)N8—C39—H39118.5
C18—N7—Cu2131.5 (3)C32—C39—H39118.5
C23—N7—Cu2111.0 (3)C10—C40—C14119.7 (4)
C39—N8—C19117.9 (3)C10—C40—H40120.2
C39—N8—Cu2130.9 (3)C14—C40—H40120.2
C19—N8—Cu2110.9 (2)C36—C41—C1119.2 (5)
C41—C1—C7117.6 (4)C36—C41—H41120.4
C41—C1—C37123.0 (4)C1—C41—H41120.4
C7—C1—C37119.3 (4)C21—C42—C19116.1 (4)
N1—C2—C29123.6 (3)C21—C42—C47125.4 (4)
N1—C2—C5116.1 (3)C19—C42—C47118.5 (4)
C29—C2—C5120.2 (3)N5—C43—C15122.2 (4)
C23—C3—C24115.9 (4)N5—C43—H43118.9
C23—C3—C45119.2 (4)C15—C43—H43118.9
C24—C3—C45124.8 (4)C31—C44—C29119.8 (4)
N2—C4—C34122.5 (4)C31—C44—H44120.1
N2—C4—C17117.4 (3)C29—C44—H44120.1
C34—C4—C17120.0 (4)C47—C45—C3120.7 (4)
N5—C5—C6122.9 (3)C47—C45—H45119.7
N5—C5—C2116.8 (3)C3—C45—H45119.7
C6—C5—C2120.3 (3)N4—C46—C10122.3 (5)
C25—C6—C5117.8 (4)N4—C46—H46118.8
C25—C6—C26123.6 (4)C10—C46—H46118.8
C5—C6—C26118.6 (3)C45—C47—C42122.2 (4)
N6—C7—C1123.3 (4)C45—C47—H47118.9
N6—C7—C9116.8 (4)C42—C47—H47118.9
C1—C7—C9119.8 (4)N6—C48—C36123.3 (5)
C17—C8—C33116.5 (5)N6—C48—H48118.4
C17—C8—C22118.6 (4)C36—C48—H48118.4
C33—C8—C22124.9 (5)
O13—Mo4—O2—Mo3−176.59 (16)N1—C2—C5—C6−178.6 (3)
O11—Mo4—O2—Mo3−69.16 (18)C29—C2—C5—C61.1 (5)
O4—Mo4—O2—Mo352.9 (3)N5—C5—C6—C25−2.9 (6)
O3—Mo4—O2—Mo398.39 (16)C2—C5—C6—C25177.0 (3)
O12—Mo3—O2—Mo4171.57 (17)N5—C5—C6—C26179.1 (3)
O5—Mo3—O2—Mo464.75 (18)C2—C5—C6—C26−1.0 (5)
O10—Mo3—O2—Mo4−68.9 (2)C48—N6—C7—C1−0.6 (6)
O9—Mo3—O2—Mo4−20.25 (14)Cu2—N6—C7—C1179.9 (3)
O6—Mo3—O2—Mo4−99.21 (16)C48—N6—C7—C9178.0 (4)
O1—Mo1—O3—Mo4107.35 (17)Cu2—N6—C7—C9−1.4 (4)
O9i—Mo1—O3—Mo4−130.89 (15)C41—C1—C7—N6−0.3 (6)
O6—Mo1—O3—Mo4−11.47 (18)C37—C1—C7—N6178.0 (4)
O1—Mo1—O3—Mo2−119.58 (16)C41—C1—C7—C9−178.9 (4)
O9i—Mo1—O3—Mo22.18 (19)C37—C1—C7—C9−0.6 (6)
O6—Mo1—O3—Mo2121.60 (15)C46—N4—C9—C142.8 (6)
O13—Mo4—O3—Mo1−120.29 (17)Cu2—N4—C9—C14177.1 (3)
O11—Mo4—O3—Mo184.2 (5)C46—N4—C9—C7−176.4 (4)
O2—Mo4—O3—Mo1−18.47 (16)Cu2—N4—C9—C7−2.2 (4)
O4—Mo4—O3—Mo1134.07 (18)N6—C7—C9—N42.5 (5)
O13—Mo4—O3—Mo293.16 (11)C1—C7—C9—N4−178.8 (3)
O11—Mo4—O3—Mo2−62.3 (5)N6—C7—C9—C14−176.8 (3)
O2—Mo4—O3—Mo2−165.02 (10)C1—C7—C9—C141.9 (5)
O4—Mo4—O3—Mo2−12.48 (9)C2—N1—C11—C311.9 (5)
O7—Mo2—O3—Mo1126.49 (18)Cu1—N1—C11—C31−172.5 (3)
O8—Mo2—O3—Mo1−69.5 (4)N4—C9—C14—C40−2.1 (6)
O4—Mo2—O3—Mo1−133.67 (18)C7—C9—C14—C40177.1 (4)
O10i—Mo2—O3—Mo128.14 (16)N4—C9—C14—C13179.3 (4)
O6i—Mo2—O3—Mo1−47.60 (16)C7—C9—C14—C13−1.5 (6)
O7—Mo2—O3—Mo4−87.34 (12)C37—C13—C14—C9−0.2 (6)
O8—Mo2—O3—Mo476.7 (4)C37—C13—C14—C40−178.8 (4)
O4—Mo2—O3—Mo412.49 (9)C38—N3—C17—C81.5 (6)
O10i—Mo2—O3—Mo4174.31 (10)Cu1—N3—C17—C8177.4 (3)
O6i—Mo2—O3—Mo498.56 (9)C38—N3—C17—C4−179.5 (3)
O13—Mo4—O4—Mo2−62.85 (17)Cu1—N3—C17—C4−3.6 (4)
O11—Mo4—O4—Mo2−170.42 (16)C33—C8—C17—N3−2.3 (6)
O2—Mo4—O4—Mo267.0 (2)C22—C8—C17—N3178.5 (4)
O3—Mo4—O4—Mo219.25 (13)C33—C8—C17—C4178.7 (4)
O7—Mo2—O4—Mo469.65 (17)C22—C8—C17—C4−0.5 (6)
O8—Mo2—O4—Mo4176.47 (16)N2—C4—C17—N33.1 (5)
O10i—Mo2—O4—Mo4−51.8 (3)C34—C4—C17—N3−178.6 (4)
O6i—Mo2—O4—Mo4−96.18 (15)N2—C4—C17—C8−177.8 (4)
O3—Mo2—O4—Mo4−19.18 (13)C34—C4—C17—C80.4 (6)
O1—Mo1—O6—Mo2i111.78 (16)C23—N7—C18—C30−2.9 (7)
O9i—Mo1—O6—Mo2i−8.99 (18)Cu2—N7—C18—C30179.2 (4)
O3—Mo1—O6—Mo2i−128.88 (15)C39—N8—C19—C42−0.9 (6)
O1—Mo1—O6—Mo3−111.36 (16)Cu2—N8—C19—C42174.2 (3)
O9i—Mo1—O6—Mo3127.87 (14)C39—N8—C19—C23177.4 (4)
O3—Mo1—O6—Mo37.98 (18)Cu2—N8—C19—C23−7.5 (4)
O12—Mo3—O6—Mo1121.68 (17)C4—N2—C20—C281.0 (6)
O5—Mo3—O6—Mo1−74.0 (5)Cu1—N2—C20—C28−178.6 (3)
O10—Mo3—O6—Mo1−137.05 (17)C17—C8—C22—C27−0.7 (7)
O2—Mo3—O6—Mo124.05 (15)C33—C8—C22—C27−179.8 (5)
O9—Mo3—O6—Mo1−51.10 (15)C18—N7—C23—C35.3 (6)
O12—Mo3—O6—Mo2i−88.63 (11)Cu2—N7—C23—C3−176.4 (3)
O5—Mo3—O6—Mo2i75.7 (4)C18—N7—C23—C19−175.2 (4)
O10—Mo3—O6—Mo2i12.63 (8)Cu2—N7—C23—C193.0 (4)
O2—Mo3—O6—Mo2i173.73 (9)C24—C3—C23—N7−3.9 (6)
O9—Mo3—O6—Mo2i98.59 (9)C45—C3—C23—N7175.9 (4)
O12—Mo3—O9—Mo1i−77.2 (5)C24—C3—C23—C19176.7 (4)
O5—Mo3—O9—Mo1i125.84 (18)C45—C3—C23—C19−3.5 (6)
O10—Mo3—O9—Mo1i23.61 (16)N8—C19—C23—N73.0 (5)
O2—Mo3—O9—Mo1i−129.16 (18)C42—C19—C23—N7−178.6 (3)
O6—Mo3—O9—Mo1i−48.12 (15)N8—C19—C23—C3−177.5 (4)
O12—Mo3—O10—Mo2i68.23 (17)C42—C19—C23—C30.8 (6)
O5—Mo3—O10—Mo2i175.48 (15)C23—C3—C24—C30−0.1 (7)
O2—Mo3—O10—Mo2i−50.4 (2)C45—C3—C24—C30−179.8 (5)
O9—Mo3—O10—Mo2i−96.82 (15)C43—C15—C25—C61.9 (7)
O6—Mo3—O10—Mo2i−18.79 (12)C5—C6—C25—C150.8 (6)
N5—Cu1—N1—C11−179.1 (3)C26—C6—C25—C15178.7 (4)
N2—Cu1—N1—C11−1.8 (3)C25—C6—C26—C35−177.9 (4)
N3—Cu1—N1—C11−82.4 (3)C5—C6—C26—C350.0 (6)
Cl—Cu1—N1—C1197.0 (3)C8—C22—C27—C342.0 (7)
N5—Cu1—N1—C26.3 (2)C34—C16—C28—C200.5 (7)
N2—Cu1—N1—C2−176.5 (2)N2—C20—C28—C16−2.0 (7)
N3—Cu1—N1—C2103.0 (2)N1—C2—C29—C440.3 (5)
Cl—Cu1—N1—C2−77.6 (2)C5—C2—C29—C44−179.4 (4)
N1—Cu1—N2—C2060.7 (3)N1—C2—C29—C35179.6 (3)
N3—Cu1—N2—C20178.7 (3)C5—C2—C29—C35−0.1 (5)
Cl—Cu1—N2—C20−82.5 (3)C3—C24—C30—C182.3 (8)
N1—Cu1—N2—C4−118.9 (3)N7—C18—C30—C24−0.8 (8)
N3—Cu1—N2—C4−0.9 (3)N1—C11—C31—C44−1.9 (6)
Cl—Cu1—N2—C497.9 (3)C42—C21—C32—C39−0.2 (8)
N5—Cu1—N3—C38−8.5 (4)C38—C12—C33—C81.0 (7)
N2—Cu1—N3—C38177.5 (4)C17—C8—C33—C121.0 (7)
N1—Cu1—N3—C38−93.5 (4)C22—C8—C33—C12−179.9 (4)
Cl—Cu1—N3—C3886.8 (4)N2—C4—C34—C16−2.8 (6)
N5—Cu1—N3—C17176.5 (3)C17—C4—C34—C16179.1 (4)
N2—Cu1—N3—C172.5 (3)N2—C4—C34—C27179.0 (4)
N1—Cu1—N3—C1791.4 (3)C17—C4—C34—C270.8 (6)
Cl—Cu1—N3—C17−88.2 (3)C28—C16—C34—C41.7 (7)
N8—Cu2—N4—C46−50.1 (5)C28—C16—C34—C27179.9 (5)
N6—Cu2—N4—C46174.5 (4)C22—C27—C34—C4−2.1 (7)
N7—Cu2—N4—C4651.6 (4)C22—C27—C34—C16179.8 (4)
N8—Cu2—N4—C9136.4 (3)C6—C26—C35—C290.9 (6)
N6—Cu2—N4—C91.0 (3)C2—C29—C35—C26−0.9 (6)
N7—Cu2—N4—C9−121.8 (3)C44—C29—C35—C26178.4 (4)
N1—Cu1—N5—C43176.6 (4)C14—C13—C37—C11.6 (7)
N3—Cu1—N5—C4359.4 (4)C41—C1—C37—C13177.1 (4)
Cl—Cu1—N5—C43−40.5 (4)C7—C1—C37—C13−1.2 (6)
N1—Cu1—N5—C5−5.8 (3)C17—N3—C38—C120.7 (6)
N3—Cu1—N5—C5−123.0 (3)Cu1—N3—C38—C12−174.1 (3)
Cl—Cu1—N5—C5137.0 (3)C33—C12—C38—N3−1.9 (7)
N8—Cu2—N6—C4838.6 (5)C19—N8—C39—C320.7 (7)
N4—Cu2—N6—C48−179.1 (4)Cu2—N8—C39—C32−173.4 (4)
N7—Cu2—N6—C48−68.8 (5)C21—C32—C39—N8−0.1 (8)
N8—Cu2—N6—C7−142.1 (3)C46—C10—C40—C140.3 (7)
N4—Cu2—N6—C70.2 (3)C9—C14—C40—C100.5 (6)
N7—Cu2—N6—C7110.6 (3)C13—C14—C40—C10179.1 (4)
N8—Cu2—N7—C18172.5 (4)C48—C36—C41—C1−1.8 (8)
N4—Cu2—N7—C1836.3 (4)C7—C1—C41—C361.5 (7)
N6—Cu2—N7—C18−58.3 (4)C37—C1—C41—C36−176.7 (4)
N8—Cu2—N7—C23−5.4 (3)C32—C21—C42—C19−0.1 (7)
N4—Cu2—N7—C23−141.7 (3)C32—C21—C42—C47179.3 (5)
N6—Cu2—N7—C23123.7 (3)N8—C19—C42—C210.6 (6)
N4—Cu2—N8—C39−65.5 (4)C23—C19—C42—C21−177.6 (4)
N6—Cu2—N8—C3954.8 (4)N8—C19—C42—C47−178.8 (4)
N7—Cu2—N8—C39−178.7 (4)C23—C19—C42—C472.9 (6)
N4—Cu2—N8—C19120.1 (3)C5—N5—C43—C150.8 (7)
N6—Cu2—N8—C19−119.6 (3)Cu1—N5—C43—C15178.3 (4)
N7—Cu2—N8—C196.9 (3)C25—C15—C43—N5−2.8 (8)
C11—N1—C2—C29−1.1 (5)C11—C31—C44—C291.0 (7)
Cu1—N1—C2—C29174.4 (3)C2—C29—C44—C31−0.2 (6)
C11—N1—C2—C5178.6 (3)C35—C29—C44—C31−179.4 (4)
Cu1—N1—C2—C5−5.9 (4)C23—C3—C45—C472.3 (7)
C20—N2—C4—C341.4 (6)C24—C3—C45—C47−177.9 (4)
Cu1—N2—C4—C34−178.9 (3)C9—N4—C46—C10−1.9 (7)
C20—N2—C4—C17179.6 (3)Cu2—N4—C46—C10−175.0 (3)
Cu1—N2—C4—C17−0.8 (5)C40—C10—C46—N40.4 (8)
C43—N5—C5—C62.1 (6)C3—C45—C47—C421.6 (7)
Cu1—N5—C5—C6−175.7 (3)C21—C42—C47—C45176.4 (4)
C43—N5—C5—C2−177.8 (4)C19—C42—C47—C45−4.2 (6)
Cu1—N5—C5—C24.4 (4)C7—N6—C48—C360.3 (7)
N1—C2—C5—N51.3 (5)Cu2—N6—C48—C36179.6 (4)
C29—C2—C5—N5−179.0 (3)C41—C36—C48—N60.9 (8)
Symmetry codes: (i) −x+1, −y, −z+1.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
OW—H1W···O7ii0.932.523.074 (6)119
OW—H1W···O10iii0.932.153.005 (6)152
C11—H11···O8i0.932.403.215 (5)146
C12—H12···O8iv0.932.493.295 (5)145
C16—H16···O7v0.932.413.320 (5)166
C20—H20···O120.932.403.049 (5)127
C22—H22···O1v0.932.533.213 (5)131
C24—H24···O13vi0.932.413.164 (6)138
C25—H25···O11iii0.932.413.301 (5)161
C26—H26···O4iii0.932.583.327 (4)137
C38—H38···OW0.932.593.328 (6)137
C40—H40···O2ii0.932.393.273 (5)159
Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) x, y+1, z; (i) −x+1, −y, −z+1; (iv) x−1, y+1, z; (v) x−1, y, z; (vi) x−1, y, z−1.
Table 1
Selected geometric parameters (Å) top
Mo1—O11.701 (2)Mo3—O62.499 (3)
Mo1—O9i1.784 (2)Mo4—O131.694 (3)
Mo1—O61.786 (3)Mo4—O111.703 (3)
Mo1—O31.790 (2)Mo4—O21.891 (2)
Mo2—O71.693 (3)Mo4—O41.905 (2)
Mo2—O81.695 (2)Mo4—O32.410 (2)
Mo2—O41.908 (2)Cu1—N51.984 (3)
Mo2—O10i1.924 (2)Cu1—N21.992 (3)
Mo2—O6i2.354 (3)Cu1—N12.075 (3)
Mo2—O32.424 (2)Cu1—N32.177 (3)
Mo3—O121.692 (2)Cu1—Cl2.2750 (12)
Mo3—O51.692 (3)Cu2—N82.025 (3)
Mo3—O101.905 (3)Cu2—N42.028 (3)
Mo3—O21.917 (3)Cu2—N62.044 (4)
Mo3—O92.380 (2)Cu2—N72.047 (4)
Symmetry codes: (i) −x+1, −y, −z+1.
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
OW—H1W···O7ii0.932.523.074 (6)119
OW—H1W···O10iii0.932.153.005 (6)152
C11—H11···O8i0.932.403.215 (5)146
C12—H12···O8iv0.932.493.295 (5)145
C16—H16···O7v0.932.413.320 (5)166
C20—H20···O120.932.403.049 (5)127
C22—H22···O1v0.932.533.213 (5)131
C24—H24···O13vi0.932.413.164 (6)138
C25—H25···O11iii0.932.413.301 (5)161
C26—H26···O4iii0.932.583.327 (4)137
C38—H38···OW0.932.593.328 (6)137
C40—H40···O2ii0.932.393.273 (5)159
Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) x, y+1, z; (i) −x+1, −y, −z+1; (iv) x−1, y+1, z; (v) x−1, y, z; (vi) x−1, y, z−1.
Acknowledgements top

This work received financial support from the National Natural Science Foundation of China (grant No. 20371010) and the State Key Laboratory for Structural Chemistry of Unstable and Stable Species in Peking University (No. 03–12).

references
References top

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