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Acta Cryst. (2007). E63, m2449    [ doi:10.1107/S1600536807037567 ]

Bis[[mu]-bis(diphenylphosphino)amine-[kappa]2P:P']bis[(1,10-phenanthroline-[kappa]2N,N')copper(I)] bis(tetrafluoridoborate) dichloromethane solvate

J. Mo, H.-Y. Qian, X.-D. Du and W. Chen

Abstract top

In the title compound, [Cu2(C25H21NP2)2(C12H8N2)2](BF4)2·CH2Cl2, two CuI atoms are bridged by two bis(diphenylphosphino)amine (dppa) ligands to form an eight-membered Cu2P4N2 ring with crystallographic twofold rotation symmetry. The coordination polyhedron of each CuI atom is distorted tetrahedral. Four F atoms are disordered equally over two sites.

Comment top

Diphosphinoamine ligands can bind to metals in monodentate, bidentate, chelating and bridging modes and their complexes find application in diverse areas such as supramolecular design, photophysics and catalysis (Liu et al., 2002; İrişli & Şen, 2005; Ahuja et al., 2007; Sekabunga et al., 2002). The title compound is a new CuI complex with bis(diphenylphosphino)amine (dppa).

The compound consists of [Cu2(phen)2(dppa)2]2+ cations (phen is 1,10-phenanthroline) located on 2-fold rotation axes. The two CuI atoms are bridged by two dppa ligands to form an eight-membered Cu2P4N2 ring. The distance between the two metal centres is 3.616 (4) Å, which is too long for any significant metal–metal bonding interaction. Each CuI atom adopts a distorted tetrahedral coordination geometry, with the angles around CuI ranging from 79.5 (2) ° for N2—Cu1—N3 to 135.28 (5) ° for P1—Cu1—P2A (where the suffix A denotes the symmetry operator −x, y, 1/2 − z).

Related literature top

For related literature concerning diphospinoamine complexes, see: Ahuja et al. (2007); İrişli & Şen (2005); Liu et al. (2002); Sekabunga et al. (2002).

Experimental top

[Cu(CH3CN)4](BF4) (0.372 g, 1.0 mmol) was dissolved in CH2Cl2 (15 ml) under nitrogen, and a solution of dppa (0.385 g, 1.0 mmol) and phen (0.18 g, 1.0 mmol) in CH2Cl2 (10 ml) was added at room temperature. The filtrate was kept under a diethyl ether atmosphere for three weeks, during which time yellow block-shaped crystals were formed.

Refinement top

H atoms were placed geometrically and allowed to ride during refinement with C—H = 0.93 Å or 0.97 Å for the CH2Cl2 molecule and with Uiso(H) = 1.2Ueq(C). The tetrafluoroborate anion is modelled as disordered over two orientations with equal site occupancies. All B—F distances were restrained to be 1.38 (1) Å, and the F···F distances within each component were restrained to be equal with an effective standard uncertainty of 0.02 Å (SADI instruction in SHELXL). The C—Cl distances in the CH2Cl2 molecule were restrained to be 1.74 (1) Å.

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. Molecular structure of the title compound with displacement ellipsoids drawn at the 40% probability level for non-H atoms. The suffix A denotes the symmetry operator −x, y, 1/2 − z. The BF4− anions and CH2Cl2 solvent molecule are omitted.
Bis[µ-bis(diphenylphosphino)amine-κ2P:P']bis[(1,10-\ phenanthroline-κ2N,N')copper(I)] bis(tetrafluoridoborate) dichloromethane solvate top
Crystal data top
[Cu2(C25H21N1P2)2(C12H8N2)2](BF4)2·CH2Cl2F000 = 3088
Mr = 1514.76Dx = 1.385 Mg m−3
Orthorhombic, PbcnMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2n 2abCell parameters from 9095 reflections
a = 19.8730 (15) Åθ = 2.3–25.5º
b = 17.4039 (13) ŵ = 0.81 mm−1
c = 21.0008 (16) ÅT = 294 (2) K
V = 7263.5 (9) Å3Block, yellow
Z = 40.26 × 0.18 × 0.10 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer		6356 independent reflections
Radiation source: fine-focus sealed tube4243 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.046
T = 294(2) Kθmax = 25.0º
φ and ω scansθmin = 1.8º
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)		h = −23→23
Tmin = 0.833, Tmax = 0.919k = −20→17
34870 measured reflectionsl = −24→20
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)] = 0.049H-atom parameters constrained
wR(F2) = 0.195  w = 1/[σ2(Fo2) + (0.1181P)2 + 8.285P]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.001
6356 reflectionsΔρmax = 0.96 e Å−3
478 parametersΔρmin = −0.29 e Å−3
93 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Crystal data top
[Cu2(C25H21N1P2)2(C12H8N2)2](BF4)2·CH2Cl2V = 7263.5 (9) Å3
Mr = 1514.76Z = 4
Orthorhombic, PbcnMo Kα
a = 19.8730 (15) ŵ = 0.81 mm−1
b = 17.4039 (13) ÅT = 294 (2) K
c = 21.0008 (16) Å0.26 × 0.18 × 0.10 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer		6356 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)		4243 reflections with I > 2σ(I)
Tmin = 0.833, Tmax = 0.919Rint = 0.046
34870 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04993 restraints
wR(F2) = 0.195H-atom parameters constrained
S = 1.01Δρmax = 0.96 e Å−3
6356 reflectionsΔρmin = −0.29 e Å−3
478 parameters
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)
Cu10.02403 (3)0.72312 (3)0.33303 (2)0.0378 (2)
P10.10615 (5)0.64958 (6)0.28923 (5)0.0348 (3)
P2−0.08734 (6)0.71415 (6)0.34225 (5)0.0333 (3)
N20.0610 (2)0.7281 (2)0.42839 (17)0.0428 (9)
N30.07362 (19)0.8288 (2)0.33142 (17)0.0410 (9)
C10.1811 (2)0.6657 (3)0.3371 (2)0.0381 (10)
C20.1936 (3)0.6201 (3)0.3902 (2)0.0523 (12)
H20.16650.57750.39800.063*
C30.2450 (3)0.6370 (4)0.4311 (3)0.0688 (16)
H30.25270.60550.46620.083*
C40.2851 (4)0.6993 (4)0.4213 (3)0.084 (2)
H40.31960.71080.44950.101*
C50.2737 (3)0.7454 (4)0.3686 (3)0.0790 (19)
H50.30130.78760.36110.095*
C60.2215 (3)0.7291 (3)0.3270 (3)0.0553 (13)
H60.21370.76090.29220.066*
C70.1003 (2)0.5451 (3)0.2906 (2)0.0424 (11)
C80.1512 (3)0.4987 (3)0.2659 (3)0.0644 (15)
H80.18930.52100.24790.077*
C90.1450 (4)0.4195 (4)0.2682 (3)0.083 (2)
H90.17890.38860.25150.100*
C100.0898 (5)0.3868 (4)0.2948 (4)0.088 (2)
H100.08580.33360.29580.106*
C110.0402 (4)0.4314 (4)0.3200 (4)0.080 (2)
H110.00280.40840.33850.096*
C120.0453 (3)0.5111 (3)0.3183 (3)0.0554 (13)
H120.01150.54130.33590.067*
N1−0.13374 (19)0.6728 (2)0.28423 (17)0.0402 (9)
C13−0.1069 (2)0.6535 (3)0.4112 (2)0.0401 (10)
C14−0.1192 (3)0.5761 (3)0.4043 (3)0.0598 (14)
H14−0.12120.55400.36410.072*
C15−0.1285 (4)0.5311 (4)0.4590 (4)0.085 (2)
H15−0.13770.47890.45490.102*
C16−0.1244 (4)0.5631 (4)0.5182 (3)0.087 (2)
H16−0.13040.53270.55410.104*
C17−0.1116 (3)0.6393 (4)0.5247 (3)0.0733 (17)
H17−0.10820.66090.56510.088*
C18−0.1037 (3)0.6842 (3)0.4720 (2)0.0558 (13)
H18−0.09590.73650.47700.067*
C19−0.1318 (2)0.8025 (3)0.3631 (2)0.0379 (10)
C20−0.2006 (3)0.8095 (3)0.3566 (3)0.0542 (13)
H20−0.22550.76810.34150.065*
C21−0.2330 (3)0.8772 (3)0.3720 (3)0.0657 (15)
H21−0.27950.88120.36750.079*
C22−0.1963 (3)0.9387 (3)0.3940 (3)0.0690 (16)
H22−0.21780.98460.40370.083*
C23−0.1283 (3)0.9323 (3)0.4016 (3)0.0708 (17)
H23−0.10350.97380.41680.085*
C24−0.0962 (3)0.8639 (3)0.3866 (3)0.0537 (13)
H24−0.04990.85950.39240.064*
C250.0563 (3)0.6769 (3)0.4752 (2)0.0530 (12)
H250.03080.63280.46860.064*
C260.0880 (3)0.6868 (4)0.5337 (3)0.0669 (16)
H260.08250.65050.56580.080*
C270.1265 (4)0.7492 (4)0.5435 (3)0.0778 (19)
H270.14760.75590.58260.093*
C280.1353 (3)0.8041 (3)0.4956 (3)0.0648 (15)
C290.1773 (4)0.8697 (4)0.5002 (3)0.088 (2)
H290.20030.87870.53800.106*
C300.1850 (4)0.9189 (4)0.4521 (4)0.091 (2)
H300.21330.96090.45690.109*
C310.1503 (3)0.9080 (3)0.3931 (3)0.0663 (15)
C320.1572 (4)0.9563 (4)0.3403 (3)0.0786 (19)
H320.18480.99940.34280.094*
C330.1238 (3)0.9406 (3)0.2854 (3)0.0710 (17)
H330.12820.97250.25010.085*
C340.0835 (3)0.8769 (3)0.2829 (3)0.0526 (12)
H340.06150.86640.24480.063*
C350.1080 (2)0.8435 (3)0.3865 (2)0.0453 (11)
C360.1003 (3)0.7908 (3)0.4380 (2)0.0452 (11)
B10.1709 (3)0.1415 (3)0.2016 (3)0.0675 (19)
F10.1630 (2)0.2187 (2)0.2035 (2)0.0981 (13)
F20.1308 (7)0.1095 (8)0.1551 (7)0.106 (6)0.50
F30.2349 (5)0.1189 (8)0.1952 (6)0.124 (6)0.50
F40.1463 (7)0.1148 (7)0.2595 (5)0.132 (5)0.50
F4'0.1836 (6)0.1066 (6)0.2591 (4)0.106 (4)0.50
F3'0.2306 (4)0.1295 (6)0.1665 (5)0.079 (3)0.50
F2'0.1202 (7)0.1039 (9)0.1708 (8)0.116 (7)0.50
C380.9690 (8)0.1159 (5)0.1366 (5)0.101 (5)0.50
H38A0.92980.10190.16150.122*0.50
H38B1.00870.09720.15870.122*0.50
Cl10.9641 (3)0.0732 (5)0.0619 (3)0.163 (2)0.50
Cl20.9731 (2)0.2138 (2)0.1298 (4)0.139 (2)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0379 (3)0.0375 (4)0.0380 (3)−0.0015 (2)0.0012 (2)−0.0012 (2)
P10.0355 (6)0.0346 (6)0.0343 (6)0.0007 (5)0.0006 (5)0.0041 (5)
P20.0365 (6)0.0327 (6)0.0308 (6)−0.0001 (5)0.0019 (4)−0.0031 (4)
N20.042 (2)0.051 (2)0.0350 (19)0.0004 (19)0.0016 (17)−0.0008 (17)
N30.044 (2)0.037 (2)0.042 (2)−0.0030 (17)0.0016 (16)−0.0014 (17)
C10.034 (2)0.039 (2)0.041 (2)0.0019 (19)0.0031 (18)−0.0007 (19)
C20.055 (3)0.049 (3)0.053 (3)0.000 (2)−0.009 (2)0.009 (2)
C30.075 (4)0.071 (4)0.060 (3)0.010 (3)−0.027 (3)0.008 (3)
C40.071 (4)0.104 (5)0.078 (4)−0.011 (4)−0.031 (3)−0.003 (4)
C50.067 (4)0.090 (5)0.080 (4)−0.033 (4)−0.016 (3)0.005 (4)
C60.046 (3)0.064 (4)0.056 (3)−0.007 (3)−0.003 (2)0.005 (3)
C70.055 (3)0.033 (2)0.038 (2)0.000 (2)−0.009 (2)0.0076 (19)
C80.077 (4)0.050 (3)0.066 (3)0.014 (3)0.008 (3)0.009 (3)
C90.127 (6)0.052 (4)0.071 (4)0.023 (4)−0.001 (4)0.004 (3)
C100.141 (7)0.043 (4)0.080 (5)−0.011 (4)−0.035 (5)0.012 (3)
C110.092 (5)0.062 (4)0.086 (5)−0.031 (4)−0.025 (4)0.027 (4)
C120.058 (3)0.051 (3)0.057 (3)−0.011 (3)−0.008 (3)0.012 (3)
N10.044 (2)0.041 (2)0.0348 (19)−0.0029 (17)0.0031 (16)−0.0101 (16)
C130.034 (2)0.041 (3)0.045 (3)0.0016 (19)0.0036 (19)0.006 (2)
C140.072 (4)0.043 (3)0.064 (3)−0.007 (3)−0.003 (3)0.005 (3)
C150.100 (5)0.049 (4)0.105 (6)−0.012 (3)−0.005 (4)0.030 (4)
C160.103 (5)0.091 (5)0.066 (4)−0.003 (4)0.008 (4)0.041 (4)
C170.090 (5)0.083 (5)0.047 (3)0.006 (4)0.016 (3)0.015 (3)
C180.070 (3)0.056 (3)0.042 (3)0.007 (3)0.009 (2)0.006 (2)
C190.046 (3)0.035 (2)0.032 (2)0.001 (2)0.0057 (19)0.0000 (18)
C200.055 (3)0.046 (3)0.062 (3)0.003 (2)0.002 (3)−0.011 (3)
C210.056 (3)0.070 (4)0.071 (4)0.021 (3)0.006 (3)−0.007 (3)
C220.085 (5)0.045 (3)0.077 (4)0.019 (3)0.010 (3)−0.008 (3)
C230.079 (4)0.046 (3)0.088 (4)−0.005 (3)0.009 (3)−0.024 (3)
C240.052 (3)0.046 (3)0.063 (3)−0.003 (2)0.004 (2)−0.014 (2)
C250.053 (3)0.059 (3)0.047 (3)0.009 (3)0.004 (2)0.007 (2)
C260.086 (4)0.071 (4)0.044 (3)0.011 (3)−0.002 (3)0.002 (3)
C270.103 (5)0.088 (5)0.042 (3)0.020 (4)−0.016 (3)−0.009 (3)
C280.075 (4)0.064 (4)0.056 (3)0.007 (3)−0.017 (3)−0.019 (3)
C290.112 (6)0.075 (4)0.077 (4)−0.008 (4)−0.044 (4)−0.021 (4)
C300.105 (6)0.066 (4)0.101 (5)−0.030 (4)−0.034 (4)−0.016 (4)
C310.073 (4)0.054 (3)0.072 (4)−0.012 (3)−0.009 (3)−0.011 (3)
C320.096 (5)0.051 (4)0.088 (5)−0.026 (3)0.001 (4)−0.003 (3)
C330.083 (4)0.050 (3)0.079 (4)−0.016 (3)0.002 (3)0.010 (3)
C340.060 (3)0.045 (3)0.053 (3)−0.002 (2)0.005 (2)−0.001 (2)
C350.045 (3)0.040 (3)0.051 (3)−0.002 (2)−0.001 (2)−0.010 (2)
C360.054 (3)0.044 (3)0.038 (2)0.004 (2)−0.002 (2)−0.008 (2)
B10.068 (5)0.064 (5)0.071 (5)−0.015 (4)−0.010 (4)0.015 (4)
F10.112 (3)0.073 (3)0.110 (3)−0.003 (2)−0.003 (2)0.004 (2)
F20.090 (8)0.116 (9)0.113 (8)−0.001 (6)−0.029 (6)−0.023 (6)
F30.086 (7)0.134 (8)0.151 (10)0.002 (6)−0.035 (6)−0.025 (7)
F40.156 (9)0.128 (8)0.113 (7)−0.030 (7)0.039 (7)0.033 (6)
F4'0.129 (7)0.097 (6)0.091 (6)−0.035 (6)−0.028 (5)0.033 (5)
F3'0.046 (5)0.091 (6)0.100 (7)−0.016 (4)−0.012 (4)−0.006 (5)
F2'0.064 (7)0.144 (13)0.139 (12)−0.038 (7)−0.028 (7)−0.034 (9)
C380.090 (11)0.079 (10)0.135 (14)−0.024 (8)−0.022 (9)0.037 (10)
Cl10.129 (4)0.217 (6)0.143 (4)−0.018 (4)−0.006 (3)−0.062 (4)
Cl20.101 (3)0.079 (3)0.238 (6)0.010 (2)0.051 (3)0.018 (3)
Geometric parameters (Å, °) top
Cu1—N22.135 (4)C17—C181.364 (7)
Cu1—N32.088 (4)C17—H170.930
Cu1—P12.2687 (12)C18—H180.930
Cu1—P22.2272 (13)C19—C241.373 (7)
P1—N1i1.686 (4)C19—C201.380 (7)
P1—C11.818 (4)C20—C211.382 (7)
P1—C71.822 (5)C20—H200.930
P2—N11.689 (4)C21—C221.374 (9)
P2—C191.826 (4)C21—H210.930
P2—C131.833 (4)C22—C231.366 (9)
N2—C251.329 (6)C22—H220.930
N2—C361.358 (6)C23—C241.388 (8)
N3—C341.332 (6)C23—H230.930
N3—C351.368 (6)C24—H240.930
C1—C61.380 (7)C25—C261.391 (7)
C1—C21.392 (6)C25—H250.930
C2—C31.367 (7)C26—C271.345 (9)
C2—H20.930C26—H260.930
C3—C41.362 (9)C27—C281.399 (9)
C3—H30.930C27—H270.930
C4—C51.384 (9)C28—C361.415 (7)
C4—H40.930C28—C291.417 (9)
C5—C61.385 (8)C29—C301.333 (10)
C5—H50.930C29—H290.930
C6—H60.930C30—C311.431 (9)
C7—C121.372 (7)C30—H300.930
C7—C81.394 (7)C31—C321.398 (9)
C8—C91.385 (8)C31—C351.408 (7)
C8—H80.930C32—C331.360 (9)
C9—C101.357 (11)C32—H320.930
C9—H90.930C33—C341.369 (8)
C10—C111.360 (11)C33—H330.930
C10—H100.930C34—H340.930
C11—C121.392 (9)C35—C361.426 (7)
C11—H110.930B1—F11.353 (6)
C12—H120.930B1—F21.379 (9)
N1—P1i1.686 (4)B1—F31.339 (9)
C13—C141.377 (7)B1—F41.389 (8)
C13—C181.385 (7)B1—F2'1.366 (8)
C14—C151.402 (8)B1—F4'1.374 (8)
C14—H140.930B1—F3'1.414 (8)
C15—C161.366 (10)C38—Cl21.711 (9)
C15—H150.930C38—Cl11.739 (10)
C16—C171.357 (10)C38—H38A0.970
C16—H160.930C38—H38B0.970
P1—Cu1—N298.96 (11)C17—C18—C13121.5 (5)
P1—Cu1—N398.69 (11)C17—C18—H18119.2
P1—Cu1—P2135.28 (5)C13—C18—H18119.2
P2—Cu1—N2105.24 (11)C24—C19—C20118.5 (4)
P2—Cu1—N3122.16 (11)C24—C19—P2119.4 (4)
N2—Cu1—N379.47 (15)C20—C19—P2122.0 (4)
N1i—P1—C1101.66 (19)C19—C20—C21121.0 (5)
N1i—P1—C7105.9 (2)C19—C20—H20119.5
C1—P1—C7101.4 (2)C21—C20—H20119.5
N1i—P1—Cu1117.99 (14)C22—C21—C20119.6 (5)
C1—P1—Cu1106.13 (14)C22—C21—H21120.2
C7—P1—Cu1120.71 (17)C20—C21—H21120.2
N1—P2—C19105.5 (2)C23—C22—C21120.2 (5)
N1—P2—C13102.1 (2)C23—C22—H22119.9
C19—P2—C13101.1 (2)C21—C22—H22119.9
N1—P2—Cu1120.64 (14)C22—C23—C24119.8 (5)
C19—P2—Cu1116.27 (15)C22—C23—H23120.1
C13—P2—Cu1108.62 (15)C24—C23—H23120.1
C25—N2—C36117.9 (4)C19—C24—C23120.9 (5)
C25—N2—Cu1130.0 (3)C19—C24—H24119.6
C36—N2—Cu1111.7 (3)C23—C24—H24119.6
C34—N3—C35117.1 (4)N2—C25—C26122.7 (5)
C34—N3—Cu1129.4 (3)N2—C25—H25118.7
C35—N3—Cu1112.8 (3)C26—C25—H25118.7
C6—C1—C2118.3 (4)C27—C26—C25119.5 (6)
C6—C1—P1121.1 (4)C27—C26—H26120.3
C2—C1—P1120.0 (4)C25—C26—H26120.3
C3—C2—C1121.0 (5)C26—C27—C28120.9 (5)
C3—C2—H2119.5C26—C27—H27119.6
C1—C2—H2119.5C28—C27—H27119.6
C4—C3—C2120.8 (6)C27—C28—C36116.2 (6)
C4—C3—H3119.6C27—C28—C29125.1 (6)
C2—C3—H3119.6C36—C28—C29118.6 (6)
C3—C4—C5119.2 (6)C30—C29—C28122.2 (6)
C3—C4—H4120.4C30—C29—H29118.9
C5—C4—H4120.4C28—C29—H29118.9
C4—C5—C6120.4 (6)C29—C30—C31121.1 (6)
C4—C5—H5119.8C29—C30—H30119.5
C6—C5—H5119.8C31—C30—H30119.5
C1—C6—C5120.3 (5)C32—C31—C35117.4 (5)
C1—C6—H6119.9C32—C31—C30124.0 (6)
C5—C6—H6119.9C35—C31—C30118.5 (6)
C12—C7—C8119.1 (5)C33—C32—C31120.2 (6)
C12—C7—P1119.2 (4)C33—C32—H32119.9
C8—C7—P1121.7 (4)C31—C32—H32119.9
C9—C8—C7119.9 (6)C32—C33—C34118.7 (6)
C9—C8—H8120.0C32—C33—H33120.6
C7—C8—H8120.0C34—C33—H33120.6
C10—C9—C8120.3 (7)N3—C34—C33124.5 (5)
C10—C9—H9119.9N3—C34—H34117.7
C8—C9—H9119.9C33—C34—H34117.7
C9—C10—C11120.4 (6)N3—C35—C31122.0 (5)
C9—C10—H10119.8N3—C35—C36117.8 (4)
C11—C10—H10119.8C31—C35—C36120.2 (5)
C10—C11—C12120.4 (7)N2—C36—C28122.8 (5)
C10—C11—H11119.8N2—C36—C35117.8 (4)
C12—C11—H11119.8C28—C36—C35119.3 (5)
C7—C12—C11120.0 (6)F3—B1—F1113.9 (8)
C7—C12—H12120.0F3—B1—F2111.0 (8)
C11—C12—H12120.0F1—B1—F2110.8 (8)
P1i—N1—P2125.8 (2)F3—B1—F4108.9 (8)
C14—C13—C18118.8 (5)F1—B1—F4105.4 (7)
C14—C13—P2121.2 (4)F2—B1—F4106.4 (9)
C18—C13—P2119.8 (4)F1—B1—F2'113.8 (8)
C13—C14—C15119.0 (6)F1—B1—F4'115.7 (7)
C13—C14—H14120.5F2'—B1—F4'109.9 (8)
C15—C14—H14120.5F1—B1—F3'105.1 (6)
C16—C15—C14120.6 (6)F2'—B1—F3'107.5 (9)
C16—C15—H15119.7F4'—B1—F3'103.8 (7)
C14—C15—H15119.7Cl2—C38—Cl1110.7 (7)
C17—C16—C15120.2 (6)Cl2—C38—H38A109.5
C17—C16—H16119.9Cl1—C38—H38A109.5
C15—C16—H16119.9Cl2—C38—H38B109.5
C16—C17—C18119.9 (6)Cl1—C38—H38B109.5
C16—C17—H17120.1H38A—C38—H38B108.1
C18—C17—H17120.1
N3—Cu1—P1—N1i−58.92 (19)Cu1—P2—C13—C14−95.0 (4)
N2—Cu1—P1—N1i−139.54 (19)N1—P2—C13—C18−152.1 (4)
P2—Cu1—P1—N1i97.95 (17)C19—P2—C13—C18−43.4 (4)
N3—Cu1—P1—C154.15 (18)Cu1—P2—C13—C1879.4 (4)
N2—Cu1—P1—C1−26.47 (19)C18—C13—C14—C150.5 (8)
P2—Cu1—P1—C1−148.98 (15)P2—C13—C14—C15174.9 (5)
N3—Cu1—P1—C7168.4 (2)C13—C14—C15—C16−1.1 (10)
N2—Cu1—P1—C787.8 (2)C14—C15—C16—C170.4 (12)
P2—Cu1—P1—C7−34.70 (19)C15—C16—C17—C180.8 (11)
N3—Cu1—P2—N1118.7 (2)C16—C17—C18—C13−1.5 (9)
N2—Cu1—P2—N1−154.27 (19)C14—C13—C18—C170.8 (8)
P1—Cu1—P2—N1−33.96 (18)P2—C13—C18—C17−173.7 (5)
N3—Cu1—P2—C19−11.0 (2)N1—P2—C19—C24−151.9 (4)
N2—Cu1—P2—C1976.01 (19)C13—P2—C19—C24102.1 (4)
P1—Cu1—P2—C19−163.68 (16)Cu1—P2—C19—C24−15.3 (4)
N3—Cu1—P2—C13−124.1 (2)N1—P2—C19—C2028.6 (4)
N2—Cu1—P2—C13−37.12 (19)C13—P2—C19—C20−77.4 (4)
P1—Cu1—P2—C1383.19 (17)Cu1—P2—C19—C20165.3 (4)
N3—Cu1—N2—C25−177.5 (4)C24—C19—C20—C211.2 (8)
P2—Cu1—N2—C2561.8 (4)P2—C19—C20—C21−179.3 (4)
P1—Cu1—N2—C25−80.3 (4)C19—C20—C21—C220.3 (9)
N3—Cu1—N2—C36−4.7 (3)C20—C21—C22—C23−1.2 (9)
P2—Cu1—N2—C36−125.4 (3)C21—C22—C23—C240.6 (10)
P1—Cu1—N2—C3692.6 (3)C20—C19—C24—C23−1.9 (8)
N2—Cu1—N3—C34175.7 (4)P2—C19—C24—C23178.6 (4)
P2—Cu1—N3—C34−82.9 (4)C22—C23—C24—C191.0 (9)
P1—Cu1—N3—C3478.1 (4)C36—N2—C25—C262.4 (7)
N2—Cu1—N3—C355.7 (3)Cu1—N2—C25—C26174.9 (4)
P2—Cu1—N3—C35107.2 (3)N2—C25—C26—C27−1.8 (9)
P1—Cu1—N3—C35−91.9 (3)C25—C26—C27—C28−0.2 (10)
N1i—P1—C1—C641.9 (4)C26—C27—C28—C361.4 (9)
C7—P1—C1—C6151.0 (4)C26—C27—C28—C29−176.8 (7)
Cu1—P1—C1—C6−82.1 (4)C27—C28—C29—C30178.1 (7)
N1i—P1—C1—C2−147.0 (4)C36—C28—C29—C30−0.1 (11)
C7—P1—C1—C2−37.9 (4)C28—C29—C30—C310.6 (12)
Cu1—P1—C1—C289.0 (4)C29—C30—C31—C32−178.5 (8)
C6—C1—C2—C3−0.7 (8)C29—C30—C31—C35−0.6 (11)
P1—C1—C2—C3−172.0 (4)C35—C31—C32—C330.2 (10)
C1—C2—C3—C40.5 (9)C30—C31—C32—C33178.1 (7)
C2—C3—C4—C5−0.7 (11)C31—C32—C33—C340.1 (10)
C3—C4—C5—C61.1 (11)C35—N3—C34—C33−2.1 (8)
C2—C1—C6—C51.0 (8)Cu1—N3—C34—C33−171.7 (4)
P1—C1—C6—C5172.3 (5)C32—C33—C34—N31.0 (10)
C4—C5—C6—C1−1.2 (10)C34—N3—C35—C312.3 (7)
N1i—P1—C7—C12−137.2 (4)Cu1—N3—C35—C31173.6 (4)
C1—P1—C7—C12117.0 (4)C34—N3—C35—C36−177.3 (4)
Cu1—P1—C7—C120.3 (4)Cu1—N3—C35—C36−6.0 (5)
N1i—P1—C7—C844.6 (5)C32—C31—C35—N3−1.4 (8)
C1—P1—C7—C8−61.1 (4)C30—C31—C35—N3−179.5 (6)
Cu1—P1—C7—C8−177.8 (4)C32—C31—C35—C36178.2 (5)
C12—C7—C8—C91.5 (8)C30—C31—C35—C360.2 (9)
P1—C7—C8—C9179.6 (5)C25—N2—C36—C28−1.1 (7)
C7—C8—C9—C10−0.4 (10)Cu1—N2—C36—C28−174.8 (4)
C8—C9—C10—C11−0.7 (11)C25—N2—C36—C35176.8 (4)
C9—C10—C11—C120.6 (10)Cu1—N2—C36—C353.0 (5)
C8—C7—C12—C11−1.5 (8)C27—C28—C36—N2−0.8 (8)
P1—C7—C12—C11−179.7 (4)C29—C28—C36—N2177.5 (5)
C10—C11—C12—C70.5 (9)C27—C28—C36—C35−178.7 (5)
C19—P2—N1—P1i122.7 (3)C29—C28—C36—C35−0.3 (8)
C13—P2—N1—P1i−132.0 (3)N3—C35—C36—N22.0 (7)
Cu1—P2—N1—P1i−11.6 (3)C31—C35—C36—N2−177.7 (5)
N1—P2—C13—C1433.5 (4)N3—C35—C36—C28179.9 (5)
C19—P2—C13—C14142.2 (4)C31—C35—C36—C280.3 (7)
Symmetry codes: (i) −x, y, −z+1/2.
Table 1
Selected geometric parameters (Å, °) top
Cu1—N22.135 (4)Cu1—P12.2687 (12)
Cu1—N32.088 (4)Cu1—P22.2272 (13)
P1—Cu1—N298.96 (11)P2—Cu1—N2105.24 (11)
P1—Cu1—N398.69 (11)P2—Cu1—N3122.16 (11)
P1—Cu1—P2135.28 (5)N2—Cu1—N379.47 (15)
Acknowledgements top

The authors thank Henan Agricultural University and Zhengzhou University of Light Industry for generous support of this study.

references
References top

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