supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportsimilar papers Open access

Acta Cryst. (2008). E64, m1411    [ doi:10.1107/S1600536808032789 ]

Tris[[mu]-1,2-bis(diphenylphosphino)ethane]-1:2[kappa]2P:P';1:3[kappa]2P:P';2:3[kappa]2P:P'-di-[mu]-bromido-1:2[kappa]4Br:Br-bromido-3[kappa]Br-tricopper(I) acetone hemisolvate

W.-J. Shi

Abstract top

In the crystal structure of the title compound, [Cu3Br3(C26H24P2)3]·0.5CH3COCH3, two of the Cu centers are bridged by two bromide anions forming a Cu([mu]-Br)2Cu core, which is further bridged by a 1,2-bis(diphenylphosphino)ethane (dppe) ligand. The third Cu center is terminally bound to another bromide ligand and is connected to the other two Cu atoms by bridging dppe ligands, forming a triangular cluster unit. The acetone solvent molecule exhibits twofold disorder about an inversion centre at (1\over2, 1, 0). The crystal structure is stabilized by intermolecular C-H...Br hydrogen bonds.

Comment top

Copper(I) halides react with bidentate phosphine ligands dppe [dppe is 1,2-bis(diphenylphosphino)ethane, C26H24P2] to give a series with the compounds of general formula [Cu2X2(dppe)3.solvate] (X is a halide anion) (Albano et al., 1972; Comba et al., 1999; Darensbourg et al., 1990; Effendy et al., 2006; Eller et al., 1977; Leoni et al., 1983; Mohr et al., 1991; Nicola et al., 2006). In these compounds Cu centers are bridged by a dppe ligand and each metal center carries one chelating dppe unit, with the fourth coordination site available for the Br- anions. We now report the crystal structure of a triangular cluster (I), Fig 1, obtained by reaction of CuBr with dppe ligand in acetone as solvent.

The asymmetric unit of the structure consists of a trinuclear molecule Cu3Br3(dppe)3 and half an acetone solvate molecule. In the molecule Cu3 Br3(dppe)3, two copper(I) centers are bridged by the bromide ligands forming a Cu(µ-Br)2Cu core, while the third copper(I) is terminally bonded to another bromide ligand. In the dinuclear Cu(µ-Br)2Cu core, the Cu(1)···Cu(2) separation is 3.169 (2) Å, while Cu(1)···Cu(3) and Cu(2)···Cu(3) separations are 6.606 (2)Å and 6.537 (1) Å, respectively. The Cu2Br2 core does not lie in a plane but is bent with a dihedral angle of 27.4 (1) ° between the planes formed by Cu(1), Br(1), Cu(2), and Cu(1), Br(2), Cu2. Each copper cation binds to two bridging dppe ligands forming a triangular tri-copper cluster system. It is interesting that Cu centers have two different coordination environments in this compound, that is CuBr2P2 in a distorted tetrahedral geometry and CuBrP2 in a slightly distorted trigonal planar geometry. In the tetrahedral CuBr2P2 core, the largest deviation from the ideal geometry is reflected in the P(1)—Cu(1)—P(3) [126.48 (5) °] and P(2)—Cu(2)—P(5) [126.48 (5) °] angles. These values are markedly higher than the normal tetrahedral value of 109.4 °.

The crystal structure is stabilized by intermolecular C—H···Br hydrogen bonds between the Br(1)- anions and –CH groups from phenyl rings, forming a one-dimensional supramolecular array (Fig. 2).

Related literature top

For related structures, see: Albano et al. (1972); Comba et al. (1999); Darensbourg et al. (1990); Effendy et al. (2006); Eller et al. (1977); Leoni et al. (1983); Mohr et al. (1991); Nicola et al. (2006).

Experimental top

A solution of 1,2-bis(diphenylphosphino)ethane (0.0181 g, 0.05 mmol) was added to a stirred suspension of CuBr (0.0079 g, 0.05 mmol) in acetone (7 ml) and the mixture was stirred and moderately heated. After the formation of a completely clear solution, 5-methoxy-2-benzimidazolethiol (0.0095 g, 0.05 mmol) was added slowly and the stirring was continued for half an hour. The resulting solution was filtered off and stand at room temperature. Colorless crystals were formed after several days. Yield: 7 mg (18%).

Refinement top

All H-atoms were positioned geometrically and refined using a riding model with d(C—H) = 0.93 Å or 0.97 Å, Uiso=1.2Ueq (C) for aromatic and methylene H atoms; 0.96 Å, Uiso= 1.5Ueq (C) for CH3 groups. The acetone solvate molecule exhibits 2-fold disorder about an inversion centre at (0.5, 1, 0) and its atoms are refined with occupancy factors of 0.5.

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of (I), with displacement ellipsoids drawn at the 30% probability level. H atoms are omitted for clarity.
[Figure 2] Fig. 2. Crystal packing of (I) showing the intermolecular C—H···Br hydrogen bonds as dashed lines.
Tris[µ-1,2-bis(diphenylphosphino)ethane]-1:2κ2P:P'; 1:3κ2P:P';2:3κ2P:P'-di-µ-bromido- 1:2κ4Br:Br-bromido-3κBr-tricopper(I) acetone hemisolvate top
Crystal data top
[Cu3Br3(C26H24P2)3]·0.5C3H6OF(000) = 3352
Mr = 1654.56Dx = 1.447 Mg m−3
Monoclinic, P21/aMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yabCell parameters from 4594 reflections
a = 18.6878 (10) Åθ = 2.3–22.5°
b = 17.1080 (9) ŵ = 2.58 mm−1
c = 25.2742 (13) ÅT = 295 K
β = 109.924 (1)°Block, colorless
V = 7596.8 (7) Å30.22 × 0.20 × 0.18 mm
Z = 4
Data collection top
Bruker SMART APEX area-detector
diffractometer		13376 independent reflections
Radiation source: fine-focus sealed tube8616 reflections with I > 2σ(I)
graphiteRint = 0.050
φ and ω scansθmax = 25.0°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −22→16
Tmin = 0.569, Tmax = 0.625k = −20→20
38020 measured reflectionsl = −30→30
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.140H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0665P)2]
where P = (Fo2 + 2Fc2)/3
13376 reflections(Δ/σ)max = 0.001
715 parametersΔρmax = 0.69 e Å−3
29 restraintsΔρmin = −0.57 e Å−3
Crystal data top
[Cu3Br3(C26H24P2)3]·0.5C3H6OV = 7596.8 (7) Å3
Mr = 1654.56Z = 4
Monoclinic, P21/aMo Kα radiation
a = 18.6878 (10) ŵ = 2.58 mm−1
b = 17.1080 (9) ÅT = 295 K
c = 25.2742 (13) Å0.22 × 0.20 × 0.18 mm
β = 109.924 (1)°
Data collection top
Bruker SMART APEX area-detector
diffractometer		13376 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		8616 reflections with I > 2σ(I)
Tmin = 0.569, Tmax = 0.625Rint = 0.050
38020 measured reflectionsθmax = 25.0°
Refinement top
R[F2 > 2σ(F2)] = 0.051H-atom parameters constrained
wR(F2) = 0.140Δρmax = 0.69 e Å−3
S = 1.03Δρmin = −0.57 e Å−3
13376 reflectionsAbsolute structure: ?
715 parametersFlack parameter: ?
29 restraintsRogers parameter: ?
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*/UeqOcc. (<1)
Br10.55058 (3)0.56272 (3)0.69646 (2)0.04792 (16)
Br20.41451 (3)0.54440 (3)0.78244 (2)0.04919 (16)
Br30.48724 (5)0.07267 (4)0.73962 (3)0.0786 (2)
Cu10.55200 (4)0.58726 (4)0.79497 (3)0.04737 (19)
Cu20.41075 (4)0.57525 (3)0.68183 (3)0.04719 (19)
Cu30.50461 (4)0.20927 (4)0.74107 (3)0.04982 (19)
P10.54401 (8)0.71311 (8)0.81736 (6)0.0436 (3)
P20.38504 (8)0.70347 (8)0.66503 (6)0.0446 (3)
P30.64042 (8)0.50050 (8)0.84372 (6)0.0437 (3)
P40.51958 (8)0.27137 (8)0.82242 (6)0.0421 (3)
P50.34513 (8)0.47459 (8)0.63000 (6)0.0455 (4)
P60.50801 (9)0.27597 (8)0.66601 (6)0.0471 (4)
C10.5387 (2)0.7255 (3)0.88786 (13)0.0616 (15)
C20.5996 (2)0.7566 (3)0.93130 (17)0.0910 (17)
H20.64250.77440.92420.109*
C30.5965 (2)0.7611 (3)0.98538 (15)0.112 (2)
H30.63720.78191.01440.135*
C40.5324 (3)0.7345 (3)0.99601 (14)0.113 (2)
H40.53030.73751.03220.136*
C50.4715 (2)0.7034 (3)0.95257 (19)0.093 (2)
H50.42860.68560.95970.111*
C60.4746 (2)0.6989 (2)0.89850 (16)0.0715 (18)
H60.43390.67810.86940.086*
C70.61863 (19)0.7810 (2)0.81621 (17)0.0513 (13)
C80.6873 (2)0.7492 (2)0.81675 (18)0.0713 (15)
H80.69350.69520.81720.086*
C90.74670 (18)0.7980 (3)0.81660 (19)0.0900 (19)
H90.79260.77660.81700.108*
C100.7375 (3)0.8786 (3)0.81591 (18)0.099 (3)
H100.77720.91120.81580.119*
C110.6688 (3)0.91048 (19)0.81537 (19)0.094 (2)
H110.66260.96440.81490.112*
C120.6094 (2)0.8617 (2)0.81552 (18)0.077 (2)
H120.56340.88300.81520.092*
C130.4555 (3)0.7617 (3)0.7733 (2)0.0490 (14)
H13A0.41200.73100.77380.059*
H13B0.45200.81270.78900.059*
C140.4530 (3)0.7714 (3)0.7123 (2)0.0537 (15)
H14A0.50330.76190.71050.064*
H14B0.43860.82460.70000.064*
C150.3770 (3)0.7384 (3)0.59432 (14)0.0662 (16)
C160.4259 (2)0.7941 (3)0.5855 (2)0.0971 (19)
H160.46330.81660.61600.116*
C170.4189 (3)0.8162 (3)0.5310 (2)0.113 (2)
H170.45160.85350.52510.135*
C180.3629 (4)0.7826 (3)0.48539 (16)0.112 (3)
H180.35820.79740.44900.135*
C190.3140 (3)0.7269 (3)0.49421 (15)0.116 (3)
H190.27660.70440.46370.139*
C200.3211 (3)0.7047 (2)0.5487 (2)0.091 (2)
H200.28840.66750.55460.109*
C210.29389 (16)0.7331 (2)0.67018 (15)0.0451 (13)
C220.27554 (19)0.81068 (17)0.67562 (16)0.0577 (15)
H220.31130.84980.67860.069*
C230.2037 (2)0.82991 (16)0.67656 (17)0.0670 (17)
H230.19140.88180.68020.080*
C240.15025 (16)0.7715 (2)0.67207 (17)0.0652 (17)
H240.10220.78440.67270.078*
C250.16860 (19)0.6939 (2)0.66663 (17)0.0696 (18)
H250.13280.65480.66360.084*
C260.2404 (2)0.67467 (15)0.66568 (16)0.0599 (16)
H260.25270.62270.66200.072*
C270.6597 (2)0.4920 (2)0.91964 (12)0.0501 (14)
C280.60622 (19)0.5235 (2)0.94068 (17)0.0642 (17)
H280.56530.55190.91720.077*
C290.6140 (3)0.5124 (3)0.99685 (19)0.090 (2)
H290.57820.53351.01090.108*
C300.6751 (3)0.4699 (3)1.03198 (12)0.091 (3)
H300.68030.46251.06960.110*
C310.7286 (2)0.4384 (2)1.01093 (17)0.092 (3)
H310.76950.41001.03440.110*
C320.7208 (2)0.4495 (2)0.95476 (19)0.0667 (18)
H320.75660.42840.94070.080*
C330.73388 (18)0.5171 (2)0.83686 (18)0.0540 (15)
C340.7868 (3)0.5656 (2)0.87456 (17)0.082 (2)
H340.77630.58710.90490.098*
C350.8555 (2)0.5819 (2)0.8669 (2)0.105 (3)
H350.89100.61430.89210.126*
C360.8713 (2)0.5497 (3)0.8216 (3)0.105 (3)
H360.91720.56060.81650.126*
C370.8183 (3)0.5013 (3)0.78388 (19)0.096 (3)
H370.82880.47980.75350.115*
C380.7496 (2)0.4850 (2)0.79152 (16)0.0681 (18)
H380.71420.45260.76630.082*
C390.6189 (3)0.3980 (3)0.8223 (2)0.0452 (13)
H39A0.61570.39150.78340.054*
H39B0.65900.36440.84560.054*
C400.5426 (3)0.3758 (3)0.8288 (2)0.0422 (13)
H40A0.50220.40380.80060.051*
H40B0.54310.39360.86540.051*
C410.59175 (19)0.2275 (2)0.88371 (14)0.0481 (14)
C420.6206 (2)0.26543 (19)0.93530 (16)0.0654 (17)
H420.60240.31460.94000.079*
C430.6766 (2)0.2299 (3)0.97987 (13)0.086 (2)
H430.69590.25521.01440.103*
C440.7038 (2)0.1564 (3)0.97285 (17)0.089 (2)
H440.74130.13261.00270.107*
C450.6750 (3)0.1185 (2)0.9213 (2)0.095 (2)
H450.69320.06930.91660.114*
C460.6190 (2)0.1540 (2)0.87669 (15)0.0705 (18)
H460.59970.12870.84220.085*
C470.43185 (17)0.2678 (2)0.83960 (15)0.0470 (13)
C480.3915 (2)0.33457 (17)0.84338 (18)0.0682 (18)
H480.40920.38360.83770.082*
C490.3246 (2)0.3281 (2)0.8556 (2)0.084 (2)
H490.29760.37280.85810.101*
C500.29816 (19)0.2549 (3)0.86409 (19)0.084 (2)
H500.25340.25050.87230.101*
C510.3385 (2)0.1881 (2)0.86031 (18)0.0749 (19)
H510.32080.13910.86600.090*
C520.4054 (2)0.19459 (17)0.84807 (16)0.0584 (16)
H520.43240.14990.84550.070*
C530.60662 (17)0.2952 (2)0.67069 (17)0.0560 (14)
C540.6285 (2)0.3606 (2)0.64729 (18)0.085 (2)
H540.59230.39690.62750.102*
C550.7046 (3)0.3716 (2)0.6534 (2)0.097 (2)
H550.71930.41530.63780.116*
C560.75884 (18)0.3172 (3)0.6830 (2)0.0881 (19)
H560.80980.32460.68710.106*
C570.7369 (2)0.2519 (2)0.70636 (19)0.0943 (18)
H570.77320.21550.72610.113*
C580.6608 (2)0.2409 (2)0.70022 (18)0.0813 (16)
H580.64620.19710.71590.098*
C590.4608 (2)0.2340 (2)0.59617 (14)0.0631 (16)
C600.4242 (3)0.1626 (3)0.59348 (17)0.0912 (19)
H600.42580.13730.62640.109*
C610.3853 (3)0.1290 (2)0.5415 (2)0.116 (2)
H610.36090.08120.53970.139*
C620.3830 (3)0.1668 (3)0.49229 (16)0.120 (3)
H620.35700.14430.45750.144*
C630.4196 (3)0.2382 (3)0.49499 (14)0.106 (3)
H630.41800.26350.46200.127*
C640.4584 (3)0.2718 (2)0.54693 (19)0.086 (2)
H640.48290.31960.54870.104*
C650.4670 (3)0.3739 (3)0.6582 (2)0.0485 (14)
H65A0.49720.40550.68980.058*
H65B0.47070.39710.62430.058*
C660.3841 (3)0.3771 (3)0.6551 (2)0.0486 (14)
H66A0.38080.36730.69200.058*
H66B0.35490.33720.62950.058*
C670.3434 (2)0.4706 (2)0.55747 (13)0.0544 (15)
C680.3903 (2)0.5223 (2)0.54227 (17)0.079 (2)
H680.41770.56000.56770.095*
C690.3964 (3)0.5179 (3)0.4891 (2)0.109 (3)
H690.42790.55250.47890.130*
C700.3556 (3)0.4616 (3)0.45105 (14)0.113 (3)
H700.35970.45860.41540.135*
C710.3086 (3)0.4098 (3)0.46625 (16)0.101 (3)
H710.28130.37220.44080.121*
C720.3025 (2)0.4143 (2)0.51946 (19)0.0725 (19)
H720.27110.37970.52960.087*
C730.2464 (3)0.4682 (3)0.6269 (3)0.0545 (15)
C740.1840 (4)0.4800 (4)0.5787 (3)0.084 (2)
H740.19060.48750.54420.101*
C750.1099 (4)0.4803 (5)0.5824 (4)0.101 (2)
H750.06800.48710.54980.121*
C760.0989 (5)0.4715 (4)0.6308 (4)0.096 (2)
H760.04970.47210.63200.116*
C770.1591 (4)0.4614 (4)0.6789 (4)0.092 (2)
H770.15090.45630.71310.110*
C780.2337 (4)0.4585 (4)0.6777 (3)0.0746 (19)
H780.27440.45020.71080.089*
O10.5092 (15)1.0605 (12)−0.0348 (9)0.224 (8)0.50
C790.447 (2)1.018 (2)0.0349 (17)0.255 (14)0.50
H79A0.41041.05840.02070.382*0.50
H79B0.47411.02620.07430.382*0.50
H79C0.42220.96800.02970.382*0.50
C800.5029 (15)1.0187 (13)0.0038 (8)0.256 (11)0.50
C810.5630 (17)0.9567 (19)0.0236 (18)0.254 (13)0.50
H81A0.59570.95870.00140.381*0.50
H81B0.53920.90620.01950.381*0.50
H81C0.59250.96540.06240.381*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br10.0362 (3)0.0551 (3)0.0565 (3)−0.0032 (2)0.0210 (3)−0.0022 (3)
Br20.0351 (3)0.0609 (4)0.0527 (3)0.0019 (3)0.0165 (3)0.0054 (3)
Br30.1066 (6)0.0527 (4)0.0905 (5)−0.0089 (4)0.0519 (5)−0.0050 (3)
Cu10.0386 (4)0.0478 (4)0.0532 (4)0.0049 (3)0.0125 (3)−0.0006 (3)
Cu20.0392 (4)0.0463 (4)0.0537 (4)0.0049 (3)0.0126 (3)−0.0005 (3)
Cu30.0511 (4)0.0495 (4)0.0530 (4)0.0031 (3)0.0230 (4)−0.0004 (3)
P10.0336 (8)0.0491 (8)0.0471 (8)0.0011 (6)0.0126 (7)−0.0051 (6)
P20.0386 (8)0.0498 (8)0.0453 (8)0.0104 (7)0.0141 (7)0.0044 (6)
P30.0321 (8)0.0473 (8)0.0502 (8)0.0014 (6)0.0121 (7)0.0022 (6)
P40.0394 (8)0.0432 (8)0.0451 (8)0.0007 (6)0.0163 (7)0.0025 (6)
P50.0369 (8)0.0456 (8)0.0533 (9)0.0010 (6)0.0144 (7)−0.0009 (6)
P60.0505 (9)0.0472 (8)0.0443 (8)0.0070 (7)0.0170 (7)−0.0016 (6)
C10.057 (3)0.087 (4)0.046 (3)−0.016 (3)0.024 (3)−0.017 (3)
C20.084 (4)0.136 (4)0.056 (3)−0.040 (3)0.028 (3)−0.022 (3)
C30.106 (4)0.167 (5)0.064 (3)−0.052 (4)0.029 (3)−0.030 (3)
C40.113 (5)0.173 (5)0.061 (4)−0.052 (5)0.038 (4)−0.032 (4)
C50.080 (6)0.131 (6)0.083 (5)−0.019 (5)0.048 (5)−0.014 (5)
C60.059 (4)0.101 (5)0.061 (4)−0.008 (4)0.028 (4)−0.017 (3)
C70.043 (3)0.061 (3)0.049 (3)−0.010 (3)0.015 (3)−0.005 (2)
C80.050 (3)0.089 (4)0.076 (3)−0.013 (3)0.024 (3)−0.007 (3)
C90.057 (4)0.117 (5)0.098 (4)−0.017 (3)0.028 (3)−0.011 (4)
C100.091 (6)0.138 (7)0.072 (5)−0.070 (6)0.032 (5)−0.024 (5)
C110.110 (7)0.074 (5)0.100 (6)−0.030 (5)0.040 (5)−0.002 (4)
C120.064 (5)0.065 (4)0.104 (5)−0.017 (4)0.031 (4)−0.009 (4)
C130.032 (3)0.053 (3)0.059 (3)0.010 (2)0.012 (3)−0.007 (3)
C140.045 (3)0.058 (4)0.057 (4)0.008 (3)0.015 (3)0.009 (3)
C150.060 (4)0.080 (4)0.068 (3)0.031 (3)0.034 (3)0.023 (3)
C160.082 (4)0.125 (4)0.089 (4)0.015 (3)0.034 (3)0.037 (3)
C170.097 (5)0.149 (5)0.100 (4)0.010 (4)0.043 (4)0.049 (4)
C180.141 (9)0.138 (8)0.085 (6)0.066 (6)0.073 (6)0.040 (5)
C190.164 (10)0.117 (7)0.052 (5)0.036 (6)0.019 (5)0.009 (4)
C200.121 (7)0.093 (5)0.045 (4)0.013 (5)0.011 (4)0.005 (4)
C210.043 (3)0.053 (3)0.039 (3)0.011 (3)0.013 (3)−0.001 (2)
C220.053 (4)0.050 (3)0.073 (4)0.010 (3)0.025 (3)0.004 (3)
C230.064 (4)0.059 (4)0.089 (5)0.016 (3)0.041 (4)0.006 (3)
C240.048 (4)0.081 (5)0.074 (4)0.015 (3)0.030 (3)−0.001 (3)
C250.050 (4)0.068 (4)0.096 (5)−0.010 (3)0.031 (4)−0.015 (4)
C260.045 (4)0.058 (4)0.080 (4)0.006 (3)0.025 (3)−0.010 (3)
C270.042 (3)0.050 (3)0.052 (3)−0.009 (3)0.009 (3)−0.003 (3)
C280.060 (4)0.076 (4)0.053 (4)−0.007 (3)0.015 (3)0.004 (3)
C290.091 (6)0.116 (6)0.071 (5)−0.019 (5)0.039 (5)−0.014 (4)
C300.117 (7)0.089 (5)0.050 (4)−0.032 (5)0.005 (5)0.002 (4)
C310.092 (6)0.082 (5)0.069 (5)−0.012 (4)−0.013 (5)0.008 (4)
C320.062 (4)0.065 (4)0.060 (4)0.002 (3)0.003 (4)0.004 (3)
C330.035 (3)0.047 (3)0.076 (4)0.008 (3)0.014 (3)0.015 (3)
C340.046 (4)0.083 (5)0.111 (6)−0.013 (4)0.020 (4)−0.007 (4)
C350.049 (5)0.102 (6)0.159 (9)−0.024 (4)0.028 (5)0.005 (5)
C360.051 (5)0.101 (6)0.175 (9)0.001 (4)0.055 (6)0.047 (6)
C370.079 (6)0.092 (6)0.144 (7)0.010 (4)0.074 (6)0.031 (5)
C380.055 (4)0.067 (4)0.092 (5)−0.001 (3)0.037 (4)0.016 (4)
C390.038 (3)0.049 (3)0.052 (3)0.002 (2)0.019 (3)0.003 (2)
C400.037 (3)0.044 (3)0.045 (3)−0.002 (2)0.013 (3)0.002 (2)
C410.031 (3)0.053 (3)0.057 (4)0.002 (2)0.011 (3)0.017 (3)
C420.056 (4)0.080 (4)0.056 (4)0.007 (3)0.013 (3)0.015 (3)
C430.077 (5)0.115 (6)0.055 (4)0.001 (4)0.009 (4)0.015 (4)
C440.070 (5)0.101 (6)0.084 (6)0.015 (4)0.011 (5)0.043 (5)
C450.091 (6)0.082 (5)0.109 (6)0.033 (5)0.029 (5)0.034 (5)
C460.064 (4)0.062 (4)0.075 (4)0.017 (3)0.011 (4)0.014 (3)
C470.039 (3)0.061 (3)0.040 (3)−0.003 (3)0.011 (3)−0.002 (3)
C480.049 (4)0.064 (4)0.103 (5)−0.003 (3)0.040 (4)−0.003 (4)
C490.060 (5)0.076 (5)0.129 (6)−0.001 (4)0.047 (5)−0.019 (4)
C500.059 (5)0.105 (6)0.100 (5)−0.033 (4)0.043 (4)−0.032 (5)
C510.068 (5)0.076 (5)0.091 (5)−0.028 (4)0.041 (4)−0.013 (4)
C520.057 (4)0.055 (4)0.072 (4)−0.019 (3)0.033 (3)−0.010 (3)
C530.044 (3)0.068 (3)0.059 (3)0.011 (3)0.021 (3)0.001 (3)
C540.052 (4)0.097 (5)0.107 (6)0.010 (4)0.031 (4)0.040 (4)
C550.071 (5)0.106 (6)0.118 (6)0.002 (5)0.040 (5)0.029 (5)
C560.056 (4)0.108 (5)0.103 (4)0.007 (4)0.029 (3)−0.007 (4)
C570.062 (3)0.101 (4)0.114 (4)0.016 (3)0.022 (3)0.008 (3)
C580.057 (3)0.085 (3)0.098 (4)0.014 (3)0.021 (3)0.012 (3)
C590.058 (4)0.072 (4)0.052 (3)0.008 (3)0.010 (3)−0.013 (3)
C600.089 (4)0.096 (4)0.069 (3)−0.012 (3)0.001 (3)−0.016 (3)
C610.114 (5)0.116 (5)0.089 (4)−0.022 (4)−0.003 (4)−0.022 (4)
C620.115 (8)0.144 (8)0.073 (6)0.007 (6)−0.005 (5)−0.027 (6)
C630.129 (8)0.126 (7)0.046 (4)0.023 (6)0.011 (5)−0.005 (4)
C640.110 (6)0.093 (5)0.054 (4)0.001 (4)0.025 (4)−0.005 (4)
C650.046 (3)0.049 (3)0.051 (3)0.003 (3)0.017 (3)0.001 (2)
C660.047 (3)0.049 (3)0.053 (3)−0.001 (3)0.020 (3)0.003 (2)
C670.054 (4)0.054 (3)0.051 (3)0.008 (3)0.012 (3)0.004 (3)
C680.113 (6)0.068 (4)0.059 (4)−0.012 (4)0.033 (4)0.004 (3)
C690.165 (7)0.105 (6)0.069 (5)−0.016 (5)0.057 (5)0.012 (4)
C700.162 (7)0.112 (6)0.061 (4)0.007 (5)0.034 (5)0.003 (4)
C710.128 (7)0.094 (5)0.066 (5)0.001 (5)0.013 (5)−0.014 (4)
C720.074 (5)0.069 (4)0.067 (4)−0.003 (4)0.014 (4)−0.008 (3)
C730.044 (4)0.045 (3)0.075 (4)0.000 (3)0.019 (3)−0.008 (3)
C740.047 (4)0.102 (5)0.098 (5)0.014 (4)0.017 (4)−0.010 (4)
C750.049 (4)0.115 (5)0.125 (6)0.008 (4)0.013 (4)−0.014 (5)
C760.055 (4)0.094 (4)0.140 (6)−0.007 (4)0.034 (4)−0.017 (5)
C770.076 (5)0.089 (5)0.130 (6)−0.011 (4)0.061 (5)−0.005 (4)
C780.043 (4)0.080 (5)0.109 (6)−0.013 (3)0.036 (4)−0.010 (4)
O10.216 (19)0.203 (18)0.246 (19)−0.043 (15)0.069 (16)0.061 (14)
C790.23 (3)0.23 (2)0.29 (3)−0.08 (2)0.07 (2)0.02 (2)
C800.24 (2)0.212 (19)0.28 (2)−0.059 (18)0.033 (19)−0.001 (18)
C810.25 (3)0.18 (2)0.27 (3)−0.05 (2)0.00 (2)−0.03 (2)
Geometric parameters (Å, °) top
Br1—Cu12.5162 (9)C35—C361.3900
Br1—Cu22.5204 (8)C35—H350.9300
Br2—Cu22.5746 (9)C36—C371.3900
Br2—Cu12.5855 (9)C36—H360.9300
Br3—Cu32.3581 (9)C37—C381.3900
Cu1—P12.2440 (15)C37—H370.9300
Cu1—P32.2502 (15)C38—H380.9300
Cu2—P22.2547 (15)C39—C401.539 (7)
Cu2—P52.2561 (15)C39—H39A0.9700
Cu3—P62.2332 (16)C39—H39B0.9700
Cu3—P42.2454 (15)C40—H40A0.9700
P1—C71.823 (3)C40—H40B0.9700
P1—C11.830 (3)C41—C421.3900
P1—C131.847 (5)C41—C461.3900
P2—C211.824 (3)C42—C431.3900
P2—C141.831 (5)C42—H420.9300
P2—C151.841 (3)C43—C441.3900
P3—C271.833 (3)C43—H430.9300
P3—C331.835 (3)C44—C451.3900
P3—C391.838 (5)C44—H440.9300
P4—C401.832 (5)C45—C461.3900
P4—C411.832 (3)C45—H450.9300
P4—C471.835 (3)C46—H460.9300
P5—C731.823 (6)C47—C481.3900
P5—C671.824 (3)C47—C521.3900
P5—C661.845 (5)C48—C491.3900
P6—C651.824 (5)C48—H480.9300
P6—C591.830 (3)C49—C501.3900
P6—C531.836 (3)C49—H490.9300
C1—C21.3900C50—C511.3900
C1—C61.3900C50—H500.9300
C2—C31.3900C51—C521.3900
C2—H20.9300C51—H510.9300
C3—C41.3900C52—H520.9300
C3—H30.9300C53—C541.3900
C4—C51.3900C53—C581.3900
C4—H40.9300C54—C551.3900
C5—C61.3900C54—H540.9300
C5—H50.9300C55—C561.3900
C6—H60.9300C55—H550.9300
C7—C81.3900C56—C571.3900
C7—C121.3900C56—H560.9300
C8—C91.3900C57—C581.3900
C8—H80.9300C57—H570.9300
C9—C101.3900C58—H580.9300
C9—H90.9300C59—C601.3900
C10—C111.3900C59—C641.3900
C10—H100.9300C60—C611.3900
C11—C121.3900C60—H600.9300
C11—H110.9300C61—C621.3900
C12—H120.9300C61—H610.9300
C13—C141.537 (7)C62—C631.3900
C13—H13A0.9700C62—H620.9300
C13—H13B0.9700C63—C641.3900
C14—H14A0.9700C63—H630.9300
C14—H14B0.9700C64—H640.9300
C15—C161.3900C65—C661.525 (7)
C15—C201.3900C65—H65A0.9700
C16—C171.3900C65—H65B0.9700
C16—H160.9300C66—H66A0.9700
C17—C181.3900C66—H66B0.9700
C17—H170.9300C67—C681.3900
C18—C191.3900C67—C721.3900
C18—H180.9300C68—C691.3900
C19—C201.3900C68—H680.9300
C19—H190.9300C69—C701.3900
C20—H200.9300C69—H690.9300
C21—C221.3900C70—C711.3900
C21—C261.3900C70—H700.9300
C22—C231.3900C71—C721.3900
C22—H220.9300C71—H710.9300
C23—C241.3900C72—H720.9300
C23—H230.9300C73—C741.385 (8)
C24—C251.3900C73—C781.393 (8)
C24—H240.9300C74—C751.420 (10)
C25—C261.3900C74—H740.9300
C25—H250.9300C75—C761.316 (10)
C26—H260.9300C75—H750.9300
C27—C281.3900C76—C771.358 (10)
C27—C321.3900C76—H760.9300
C28—C291.3900C77—C781.404 (9)
C28—H280.9300C77—H770.9300
C29—C301.3900C78—H780.9300
C29—H290.9300O1—C801.248 (10)
C30—C311.3900C79—C801.500 (10)
C30—H300.9300C79—H79A0.9600
C31—C321.3900C79—H79B0.9600
C31—H310.9300C79—H79C0.9600
C32—H320.9300C80—C811.502 (10)
C33—C341.3900C81—H81A0.9600
C33—C381.3900C81—H81B0.9600
C34—C351.3900C81—H81C0.9600
C34—H340.9300
Cu1—Br1—Cu277.99 (3)C35—C34—H34120.0
Cu2—Br2—Cu175.78 (3)C36—C35—C34120.0
P1—Cu1—P3126.47 (6)C36—C35—H35120.0
P1—Cu1—Br1115.49 (5)C34—C35—H35120.0
P3—Cu1—Br1100.95 (5)C37—C36—C35120.0
P1—Cu1—Br298.87 (4)C37—C36—H36120.0
P3—Cu1—Br2113.18 (5)C35—C36—H36120.0
Br1—Cu1—Br299.00 (3)C36—C37—C38120.0
P2—Cu2—P5126.48 (6)C36—C37—H37120.0
P2—Cu2—Br1104.72 (5)C38—C37—H37120.0
P5—Cu2—Br1110.58 (5)C37—C38—C33120.0
P2—Cu2—Br2108.52 (5)C37—C38—H38120.0
P5—Cu2—Br2104.09 (5)C33—C38—H38120.0
Br1—Cu2—Br299.19 (3)C40—C39—P3108.8 (3)
P6—Cu3—P4120.35 (6)C40—C39—H39A109.9
P6—Cu3—Br3122.47 (5)P3—C39—H39A109.9
P4—Cu3—Br3117.18 (5)C40—C39—H39B109.9
C7—P1—C1103.71 (19)P3—C39—H39B109.9
C7—P1—C13103.7 (2)H39A—C39—H39B108.3
C1—P1—C13101.5 (2)C39—C40—P4115.4 (3)
C7—P1—Cu1119.38 (14)C39—C40—H40A108.4
C1—P1—Cu1112.77 (15)P4—C40—H40A108.4
C13—P1—Cu1113.77 (17)C39—C40—H40B108.4
C21—P2—C14103.6 (2)P4—C40—H40B108.4
C21—P2—C15102.11 (19)H40A—C40—H40B107.5
C14—P2—C15103.7 (2)C42—C41—C46120.0
C21—P2—Cu2113.64 (13)C42—C41—P4122.7 (2)
C14—P2—Cu2115.99 (18)C46—C41—P4117.3 (2)
C15—P2—Cu2116.10 (15)C41—C42—C43120.0
C27—P3—C33104.93 (19)C41—C42—H42120.0
C27—P3—C39100.2 (2)C43—C42—H42120.0
C33—P3—C39103.9 (2)C44—C43—C42120.0
C27—P3—Cu1118.09 (15)C44—C43—H43120.0
C33—P3—Cu1113.00 (13)C42—C43—H43120.0
C39—P3—Cu1114.92 (17)C45—C44—C43120.0
C40—P4—C41104.0 (2)C45—C44—H44120.0
C40—P4—C47102.3 (2)C43—C44—H44120.0
C41—P4—C47104.24 (18)C46—C45—C44120.0
C40—P4—Cu3119.66 (17)C46—C45—H45120.0
C41—P4—Cu3113.99 (14)C44—C45—H45120.0
C47—P4—Cu3111.01 (13)C45—C46—C41120.0
C73—P5—C67106.5 (2)C45—C46—H46120.0
C73—P5—C66103.6 (2)C41—C46—H46120.0
C67—P5—C66100.4 (2)C48—C47—C52120.0
C73—P5—Cu2114.33 (18)C48—C47—P4122.6 (2)
C67—P5—Cu2115.63 (15)C52—C47—P4117.4 (2)
C66—P5—Cu2114.70 (18)C47—C48—C49120.0
C65—P6—C59102.1 (2)C47—C48—H48120.0
C65—P6—C53102.6 (2)C49—C48—H48120.0
C59—P6—C53106.0 (2)C50—C49—C48120.0
C65—P6—Cu3115.36 (18)C50—C49—H49120.0
C59—P6—Cu3118.36 (16)C48—C49—H49120.0
C53—P6—Cu3110.82 (15)C49—C50—C51120.0
C2—C1—C6120.0C49—C50—H50120.0
C2—C1—P1120.8 (2)C51—C50—H50120.0
C6—C1—P1119.1 (2)C52—C51—C50120.0
C3—C2—C1120.0C52—C51—H51120.0
C3—C2—H2120.0C50—C51—H51120.0
C1—C2—H2120.0C51—C52—C47120.0
C4—C3—C2120.0C51—C52—H52120.0
C4—C3—H3120.0C47—C52—H52120.0
C2—C3—H3120.0C54—C53—C58120.0
C3—C4—C5120.0C54—C53—P6123.5 (2)
C3—C4—H4120.0C58—C53—P6116.5 (2)
C5—C4—H4120.0C55—C54—C53120.0
C6—C5—C4120.0C55—C54—H54120.0
C6—C5—H5120.0C53—C54—H54120.0
C4—C5—H5120.0C54—C55—C56120.0
C5—C6—C1120.0C54—C55—H55120.0
C5—C6—H6120.0C56—C55—H55120.0
C1—C6—H6120.0C55—C56—C57120.0
C8—C7—C12120.0C55—C56—H56120.0
C8—C7—P1117.3 (3)C57—C56—H56120.0
C12—C7—P1122.7 (3)C58—C57—C56120.0
C9—C8—C7120.0C58—C57—H57120.0
C9—C8—H8120.0C56—C57—H57120.0
C7—C8—H8120.0C57—C58—C53120.0
C10—C9—C8120.0C57—C58—H58120.0
C10—C9—H9120.0C53—C58—H58120.0
C8—C9—H9120.0C60—C59—C64120.0
C9—C10—C11120.0C60—C59—P6117.4 (3)
C9—C10—H10120.0C64—C59—P6122.6 (3)
C11—C10—H10120.0C61—C60—C59120.0
C12—C11—C10120.0C61—C60—H60120.0
C12—C11—H11120.0C59—C60—H60120.0
C10—C11—H11120.0C60—C61—C62120.0
C11—C12—C7120.0C60—C61—H61120.0
C11—C12—H12120.0C62—C61—H61120.0
C7—C12—H12120.0C63—C62—C61120.0
C14—C13—P1111.6 (4)C63—C62—H62120.0
C14—C13—H13A109.3C61—C62—H62120.0
P1—C13—H13A109.3C62—C63—C64120.0
C14—C13—H13B109.3C62—C63—H63120.0
P1—C13—H13B109.3C64—C63—H63120.0
H13A—C13—H13B108.0C63—C64—C59120.0
C13—C14—P2111.3 (4)C63—C64—H64120.0
C13—C14—H14A109.4C59—C64—H64120.0
P2—C14—H14A109.4C66—C65—P6114.9 (4)
C13—C14—H14B109.4C66—C65—H65A108.6
P2—C14—H14B109.4P6—C65—H65A108.6
H14A—C14—H14B108.0C66—C65—H65B108.6
C16—C15—C20120.0P6—C65—H65B108.6
C16—C15—P2122.5 (3)H65A—C65—H65B107.5
C20—C15—P2117.5 (3)C65—C66—P5109.0 (3)
C15—C16—C17120.0C65—C66—H66A109.9
C15—C16—H16120.0P5—C66—H66A109.9
C17—C16—H16120.0C65—C66—H66B109.9
C18—C17—C16120.0P5—C66—H66B109.9
C18—C17—H17120.0H66A—C66—H66B108.3
C16—C17—H17120.0C68—C67—C72120.0
C17—C18—C19120.0C68—C67—P5117.2 (3)
C17—C18—H18120.0C72—C67—P5122.6 (3)
C19—C18—H18120.0C67—C68—C69120.0
C20—C19—C18120.0C67—C68—H68120.0
C20—C19—H19120.0C69—C68—H68120.0
C18—C19—H19120.0C68—C69—C70120.0
C19—C20—C15120.0C68—C69—H69120.0
C19—C20—H20120.0C70—C69—H69120.0
C15—C20—H20120.0C71—C70—C69120.0
C22—C21—C26120.0C71—C70—H70120.0
C22—C21—P2122.7 (2)C69—C70—H70120.0
C26—C21—P2117.2 (2)C70—C71—C72120.0
C21—C22—C23120.0C70—C71—H71120.0
C21—C22—H22120.0C72—C71—H71120.0
C23—C22—H22120.0C71—C72—C67120.0
C22—C23—C24120.0C71—C72—H72120.0
C22—C23—H23120.0C67—C72—H72120.0
C24—C23—H23120.0C74—C73—C78118.1 (6)
C25—C24—C23120.0C74—C73—P5124.4 (5)
C25—C24—H24120.0C78—C73—P5117.2 (5)
C23—C24—H24120.0C73—C74—C75119.3 (7)
C24—C25—C26120.0C73—C74—H74120.3
C24—C25—H25120.0C75—C74—H74120.3
C26—C25—H25120.0C76—C75—C74121.7 (8)
C25—C26—C21120.0C76—C75—H75119.1
C25—C26—H26120.0C74—C75—H75119.1
C21—C26—H26120.0C75—C76—C77120.2 (8)
C28—C27—C32120.0C75—C76—H76119.9
C28—C27—P3117.3 (3)C77—C76—H76119.9
C32—C27—P3122.4 (3)C76—C77—C78120.7 (8)
C27—C28—C29120.0C76—C77—H77119.7
C27—C28—H28120.0C78—C77—H77119.7
C29—C28—H28120.0C73—C78—C77119.9 (7)
C30—C29—C28120.0C73—C78—H78120.0
C30—C29—H29120.0C77—C78—H78120.0
C28—C29—H29120.0C80—C79—H79A109.5
C29—C30—C31120.0C80—C79—H79B109.5
C29—C30—H30120.0H79A—C79—H79B109.5
C31—C30—H30120.0C80—C79—H79C109.5
C32—C31—C30120.0H79A—C79—H79C109.5
C32—C31—H31120.0H79B—C79—H79C109.5
C30—C31—H31120.0O1—C80—C79133 (3)
C31—C32—C27120.0O1—C80—C81114 (2)
C31—C32—H32120.0C79—C80—C81112.9 (10)
C27—C32—H32120.0C80—C81—H81A109.5
C34—C33—C38120.0C80—C81—H81B109.5
C34—C33—P3120.4 (3)H81A—C81—H81B109.5
C38—C33—P3119.5 (3)C80—C81—H81C109.5
C33—C34—C35120.0H81A—C81—H81C109.5
C33—C34—H34120.0H81B—C81—H81C109.5
Cu2—Br1—Cu1—P1−82.86 (5)Cu1—P3—C27—C2816.4 (3)
Cu2—Br1—Cu1—P3137.42 (4)C33—P3—C27—C32−42.8 (3)
Cu2—Br1—Cu1—Br221.53 (3)C39—P3—C27—C3264.6 (3)
Cu2—Br2—Cu1—P196.50 (4)Cu1—P3—C27—C32−169.77 (17)
Cu2—Br2—Cu1—P3−127.34 (5)C32—C27—C28—C290.0
Cu2—Br2—Cu1—Br1−21.26 (3)P3—C27—C28—C29174.0 (3)
Cu1—Br1—Cu2—P290.40 (5)C27—C28—C29—C300.0
Cu1—Br1—Cu2—P5−130.56 (5)C28—C29—C30—C310.0
Cu1—Br1—Cu2—Br2−21.64 (3)C29—C30—C31—C320.0
Cu1—Br2—Cu2—P2−87.77 (5)C30—C31—C32—C270.0
Cu1—Br2—Cu2—P5135.29 (5)C28—C27—C32—C310.0
Cu1—Br2—Cu2—Br121.23 (3)P3—C27—C32—C31−173.6 (3)
P3—Cu1—P1—C765.97 (18)C27—P3—C33—C34−39.8 (3)
Br1—Cu1—P1—C7−61.92 (17)C39—P3—C33—C34−144.6 (3)
Br2—Cu1—P1—C7−166.39 (16)Cu1—P3—C33—C3490.2 (2)
P3—Cu1—P1—C1−56.12 (17)C27—P3—C33—C38144.3 (2)
Br1—Cu1—P1—C1176.00 (15)C39—P3—C33—C3839.5 (3)
Br2—Cu1—P1—C171.53 (16)Cu1—P3—C33—C38−85.7 (2)
P3—Cu1—P1—C13−171.1 (2)C38—C33—C34—C350.0
Br1—Cu1—P1—C1361.1 (2)P3—C33—C34—C35−175.8 (3)
Br2—Cu1—P1—C13−43.4 (2)C33—C34—C35—C360.0
P5—Cu2—P2—C2164.16 (16)C34—C35—C36—C370.0
Br1—Cu2—P2—C21−165.59 (14)C35—C36—C37—C380.0
Br2—Cu2—P2—C21−60.39 (14)C36—C37—C38—C330.0
P5—Cu2—P2—C14−176.0 (2)C34—C33—C38—C370.0
Br1—Cu2—P2—C14−45.7 (2)P3—C33—C38—C37175.9 (3)
Br2—Cu2—P2—C1459.5 (2)C27—P3—C39—C4069.2 (4)
P5—Cu2—P2—C15−53.84 (19)C33—P3—C39—C40177.5 (3)
Br1—Cu2—P2—C1576.42 (18)Cu1—P3—C39—C40−58.5 (4)
Br2—Cu2—P2—C15−178.39 (17)P3—C39—C40—P4−168.9 (3)
P1—Cu1—P3—C2749.44 (17)C41—P4—C40—C3966.2 (4)
Br1—Cu1—P3—C27−177.08 (15)C47—P4—C40—C39174.5 (4)
Br2—Cu1—P3—C27−72.24 (15)Cu3—P4—C40—C39−62.4 (4)
P1—Cu1—P3—C33−73.51 (18)C40—P4—C41—C4234.5 (3)
Br1—Cu1—P3—C3359.97 (16)C47—P4—C41—C42−72.3 (3)
Br2—Cu1—P3—C33164.81 (16)Cu3—P4—C41—C42166.5 (2)
P1—Cu1—P3—C39167.50 (19)C40—P4—C41—C46−144.0 (3)
Br1—Cu1—P3—C39−59.02 (19)C47—P4—C41—C46109.2 (2)
Br2—Cu1—P3—C3945.8 (2)Cu3—P4—C41—C46−12.0 (2)
P6—Cu3—P4—C40−5.1 (2)C46—C41—C42—C430.0
Br3—Cu3—P4—C40174.09 (19)P4—C41—C42—C43−178.5 (3)
P6—Cu3—P4—C41−129.00 (15)C41—C42—C43—C440.0
Br3—Cu3—P4—C4150.18 (16)C42—C43—C44—C450.0
P6—Cu3—P4—C47113.66 (14)C43—C44—C45—C460.0
Br3—Cu3—P4—C47−67.17 (14)C44—C45—C46—C410.0
P2—Cu2—P5—C73−62.1 (2)C42—C41—C46—C450.0
Br1—Cu2—P5—C73169.9 (2)P4—C41—C46—C45178.5 (3)
Br2—Cu2—P5—C7364.2 (2)C40—P4—C47—C4811.7 (3)
P2—Cu2—P5—C6762.10 (17)C41—P4—C47—C48119.8 (2)
Br1—Cu2—P5—C67−65.86 (16)Cu3—P4—C47—C48−117.0 (2)
Br2—Cu2—P5—C67−171.53 (15)C40—P4—C47—C52−169.3 (2)
P2—Cu2—P5—C66178.3 (2)C41—P4—C47—C52−61.2 (2)
Br1—Cu2—P5—C6650.4 (2)Cu3—P4—C47—C5261.9 (2)
Br2—Cu2—P5—C66−55.3 (2)C52—C47—C48—C490.0
P4—Cu3—P6—C65−35.5 (2)P4—C47—C48—C49178.9 (3)
Br3—Cu3—P6—C65145.41 (19)C47—C48—C49—C500.0
P4—Cu3—P6—C59−156.70 (18)C48—C49—C50—C510.0
Br3—Cu3—P6—C5924.17 (19)C49—C50—C51—C520.0
P4—Cu3—P6—C5380.54 (16)C50—C51—C52—C470.0
Br3—Cu3—P6—C53−98.59 (16)C48—C47—C52—C510.0
C7—P1—C1—C2−21.3 (3)P4—C47—C52—C51−179.0 (3)
C13—P1—C1—C2−128.6 (3)C65—P6—C53—C54−26.2 (3)
Cu1—P1—C1—C2109.2 (2)C59—P6—C53—C5480.5 (3)
C7—P1—C1—C6162.7 (3)Cu3—P6—C53—C54−149.8 (2)
C13—P1—C1—C655.3 (3)C65—P6—C53—C58152.9 (3)
Cu1—P1—C1—C6−66.8 (3)C59—P6—C53—C58−100.5 (3)
C6—C1—C2—C30.0Cu3—P6—C53—C5829.2 (3)
P1—C1—C2—C3−176.0 (3)C58—C53—C54—C550.0
C1—C2—C3—C40.0P6—C53—C54—C55179.0 (3)
C2—C3—C4—C50.0C53—C54—C55—C560.0
C3—C4—C5—C60.0C54—C55—C56—C570.0
C4—C5—C6—C10.0C55—C56—C57—C580.0
C2—C1—C6—C50.0C56—C57—C58—C530.0
P1—C1—C6—C5176.1 (3)C54—C53—C58—C570.0
C1—P1—C7—C8109.2 (3)P6—C53—C58—C57−179.0 (3)
C13—P1—C7—C8−145.1 (3)C65—P6—C59—C60−127.1 (3)
Cu1—P1—C7—C8−17.3 (3)C53—P6—C59—C60125.8 (3)
C1—P1—C7—C12−70.1 (3)Cu3—P6—C59—C600.7 (3)
C13—P1—C7—C1235.7 (3)C65—P6—C59—C6450.8 (3)
Cu1—P1—C7—C12163.46 (19)C53—P6—C59—C64−56.2 (3)
C12—C7—C8—C90.0Cu3—P6—C59—C64178.7 (2)
P1—C7—C8—C9−179.2 (3)C64—C59—C60—C610.0
C7—C8—C9—C100.0P6—C59—C60—C61178.0 (3)
C8—C9—C10—C110.0C59—C60—C61—C620.0
C9—C10—C11—C120.0C60—C61—C62—C630.0
C10—C11—C12—C70.0C61—C62—C63—C640.0
C8—C7—C12—C110.0C62—C63—C64—C590.0
P1—C7—C12—C11179.2 (3)C60—C59—C64—C630.0
C7—P1—C13—C1463.0 (4)P6—C59—C64—C63−177.9 (4)
C1—P1—C13—C14170.4 (4)C59—P6—C65—C6672.2 (4)
Cu1—P1—C13—C14−68.2 (4)C53—P6—C65—C66−178.1 (4)
P1—C13—C14—P2107.0 (4)Cu3—P6—C65—C66−57.5 (4)
C21—P2—C14—C1362.5 (4)P6—C65—C66—P5−166.1 (3)
C15—P2—C14—C13168.8 (3)C73—P5—C66—C65178.6 (4)
Cu2—P2—C14—C13−62.7 (4)C67—P5—C66—C6568.6 (4)
C21—P2—C15—C16118.2 (3)Cu2—P5—C66—C65−56.0 (4)
C14—P2—C15—C1610.8 (3)C73—P5—C67—C68136.8 (3)
Cu2—P2—C15—C16−117.7 (2)C66—P5—C67—C68−115.5 (3)
C21—P2—C15—C20−64.1 (3)Cu2—P5—C67—C688.6 (3)
C14—P2—C15—C20−171.5 (3)C73—P5—C67—C72−48.7 (3)
Cu2—P2—C15—C2060.1 (3)C66—P5—C67—C7259.0 (3)
C20—C15—C16—C170.0Cu2—P5—C67—C72−177.0 (2)
P2—C15—C16—C17177.7 (3)C72—C67—C68—C690.0
C15—C16—C17—C180.0P5—C67—C68—C69174.6 (3)
C16—C17—C18—C190.0C67—C68—C69—C700.0
C17—C18—C19—C200.0C68—C69—C70—C710.0
C18—C19—C20—C150.0C69—C70—C71—C720.0
C16—C15—C20—C190.0C70—C71—C72—C670.0
P2—C15—C20—C19−177.8 (3)C68—C67—C72—C710.0
C14—P2—C21—C2236.5 (3)P5—C67—C72—C71−174.3 (3)
C15—P2—C21—C22−71.0 (3)C67—P5—C73—C74−15.8 (6)
Cu2—P2—C21—C22163.24 (17)C66—P5—C73—C74−121.2 (5)
C14—P2—C21—C26−146.6 (2)Cu2—P5—C73—C74113.2 (5)
C15—P2—C21—C26106.0 (2)C67—P5—C73—C78170.8 (4)
Cu2—P2—C21—C26−19.9 (2)C66—P5—C73—C7865.3 (5)
C26—C21—C22—C230.0Cu2—P5—C73—C78−60.3 (5)
P2—C21—C22—C23176.8 (3)C78—C73—C74—C75−1.0 (9)
C21—C22—C23—C240.0P5—C73—C74—C75−174.4 (5)
C22—C23—C24—C250.0C73—C74—C75—C761.4 (12)
C23—C24—C25—C260.0C74—C75—C76—C77−0.2 (13)
C24—C25—C26—C210.0C75—C76—C77—C78−1.4 (12)
C22—C21—C26—C250.0C74—C73—C78—C77−0.5 (9)
P2—C21—C26—C25−177.0 (3)P5—C73—C78—C77173.4 (5)
C33—P3—C27—C28143.4 (2)C76—C77—C78—C731.8 (11)
C39—P3—C27—C28−109.2 (3)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
C24—H24···Br1i0.932.923.560 (3)127
C65—H65A···Br10.972.853.576 (5)132
C40—H40A···Br20.972.863.675 (5)142
Symmetry codes: (i) x−1/2, −y+3/2, z.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
C24—H24···Br1i0.932.923.560 (3)127
C65—H65A···Br10.972.853.576 (5)132
C40—H40A···Br20.972.863.675 (5)142
Symmetry codes: (i) x−1/2, −y+3/2, z.
Acknowledgements top

The author thanks Jiangxi Science and Technology Normal University for supporting this study.

references
References top

Albano, V. G., Bellon, P. L. & Ciani, G. (1972). Dalton Trans. pp. 1938–1943.

Bruker (2002). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.

Comba, P., Katsichtis, C., Nuber, B. & Pritzkow, H. (1999). Eur. J. Inorg. Chem. pp. 777–783.

Darensbourg, D. J., Chao, C. C., Reibenspies, J. H. & Bischoff, C. J. (1990). Inorg. Chem. 29, 2153–2157.

Effendy, Nicola, C. D., Pettinari, C., Pizzabiocca, A., Skelton, B. W., Somers, N. & White, A. H. (2006). Inorg. Chim. Acta, 359, 64–80.

Eller, P. G., Kubas, G. J. & Ryan, R. R. (1977). Inorg. Chem. 16, 2454–2462.

Leoni, P., Pasquali, M. & Ghilardi, C. A. (1983). Chem. Commun. pp. 240–241.

Mohr, B., Brooks, E. E., Rath, N. & Deutsch, E. (1991). Inorg. Chem. 30, 4541–4545.

Nicola, C. D., Effendy, Pettinari, C., Skelton, B. W., Somers, N. & White, A. H. (2006). Inorg. Chim. Acta, 359, 53–63.

Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.