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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807037567/bi2209sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807037567/bi2209Isup2.hkl
Contains datablock I

CCDC reference: 663545

Key indicators

  • Single-crystal X-ray study
  • T = 294 K
  • Mean [sigma](C-C) = 0.009 Å
  • Disorder in solvent or counterion
  • R factor = 0.049
  • wR factor = 0.194
  • Data-to-parameter ratio = 13.3

checkCIF/PLATON results

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Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 3.26 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for F2' PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for F3 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for F4 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for F3' PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for B1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C38 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 41.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 9 PLAT431_ALERT_2_C Short Inter HL..A Contact F3 .. N1 .. 2.81 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F3' .. N1 .. 2.98 Ang.
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 93
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 7 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

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.

Structure description 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).

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

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-πhenanthroline-κ2N,N')copper(I)] bis(tetrafluoridoborate) dichloromethane solvate top
Crystal data top
[Cu2(C25H21NP2)2(C12H8N2)2](BF4)2·CH2Cl2F(000) = 3088
Mr = 1514.76Dx = 1.385 Mg m3
Orthorhombic, PbcnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2abCell parameters from 9095 reflections
a = 19.8730 (15) Åθ = 2.3–25.5°
b = 17.4039 (13) ŵ = 0.81 mm1
c = 21.0008 (16) ÅT = 294 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)
Graphite monochromatorRint = 0.046
φ and ω scansθmax = 25.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 2323
Tmin = 0.833, Tmax = 0.919k = 2017
34870 measured reflectionsl = 2420
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)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.195H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.1181P)2 + 8.285P]
where P = (Fo2 + 2Fc2)/3
6356 reflections(Δ/σ)max = 0.001
478 parametersΔρmax = 0.96 e Å3
93 restraintsΔρmin = 0.30 e Å3
Crystal data top
[Cu2(C25H21NP2)2(C12H8N2)2](BF4)2·CH2Cl2V = 7263.5 (9) Å3
Mr = 1514.76Z = 4
Orthorhombic, PbcnMo Kα radiation
a = 19.8730 (15) ŵ = 0.81 mm1
b = 17.4039 (13) ÅT = 294 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 Å3
6356 reflectionsΔρmin = 0.30 e Å3
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)
P20.08734 (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*
N10.13374 (19)0.6728 (2)0.28423 (17)0.0402 (9)
C130.1069 (2)0.6535 (3)0.4112 (2)0.0401 (10)
C140.1192 (3)0.5761 (3)0.4043 (3)0.0598 (14)
H140.12120.55400.36410.072*
C150.1285 (4)0.5311 (4)0.4590 (4)0.085 (2)
H150.13770.47890.45490.102*
C160.1244 (4)0.5631 (4)0.5182 (3)0.087 (2)
H160.13040.53270.55410.104*
C170.1116 (3)0.6393 (4)0.5247 (3)0.0733 (17)
H170.10820.66090.56510.088*
C180.1037 (3)0.6842 (3)0.4720 (2)0.0558 (13)
H180.09590.73650.47700.067*
C190.1318 (2)0.8025 (3)0.3631 (2)0.0379 (10)
C200.2006 (3)0.8095 (3)0.3566 (3)0.0542 (13)
H200.22550.76810.34150.065*
C210.2330 (3)0.8772 (3)0.3720 (3)0.0657 (15)
H210.27950.88120.36750.079*
C220.1963 (3)0.9387 (3)0.3940 (3)0.0690 (16)
H220.21780.98460.40370.083*
C230.1283 (3)0.9323 (3)0.4016 (3)0.0708 (17)
H230.10350.97380.41680.085*
C240.0962 (3)0.8639 (3)0.3866 (3)0.0537 (13)
H240.04990.85950.39240.064*
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, º) 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—N1i58.92 (19)Cu1—P2—C13—C1495.0 (4)
N2—Cu1—P1—N1i139.54 (19)N1—P2—C13—C18152.1 (4)
P2—Cu1—P1—N1i97.95 (17)C19—P2—C13—C1843.4 (4)
N3—Cu1—P1—C154.15 (18)Cu1—P2—C13—C1879.4 (4)
N2—Cu1—P1—C126.47 (19)C18—C13—C14—C150.5 (8)
P2—Cu1—P1—C1148.98 (15)P2—C13—C14—C15174.9 (5)
N3—Cu1—P1—C7168.4 (2)C13—C14—C15—C161.1 (10)
N2—Cu1—P1—C787.8 (2)C14—C15—C16—C170.4 (12)
P2—Cu1—P1—C734.70 (19)C15—C16—C17—C180.8 (11)
N3—Cu1—P2—N1118.7 (2)C16—C17—C18—C131.5 (9)
N2—Cu1—P2—N1154.27 (19)C14—C13—C18—C170.8 (8)
P1—Cu1—P2—N133.96 (18)P2—C13—C18—C17173.7 (5)
N3—Cu1—P2—C1911.0 (2)N1—P2—C19—C24151.9 (4)
N2—Cu1—P2—C1976.01 (19)C13—P2—C19—C24102.1 (4)
P1—Cu1—P2—C19163.68 (16)Cu1—P2—C19—C2415.3 (4)
N3—Cu1—P2—C13124.1 (2)N1—P2—C19—C2028.6 (4)
N2—Cu1—P2—C1337.12 (19)C13—P2—C19—C2077.4 (4)
P1—Cu1—P2—C1383.19 (17)Cu1—P2—C19—C20165.3 (4)
N3—Cu1—N2—C25177.5 (4)C24—C19—C20—C211.2 (8)
P2—Cu1—N2—C2561.8 (4)P2—C19—C20—C21179.3 (4)
P1—Cu1—N2—C2580.3 (4)C19—C20—C21—C220.3 (9)
N3—Cu1—N2—C364.7 (3)C20—C21—C22—C231.2 (9)
P2—Cu1—N2—C36125.4 (3)C21—C22—C23—C240.6 (10)
P1—Cu1—N2—C3692.6 (3)C20—C19—C24—C231.9 (8)
N2—Cu1—N3—C34175.7 (4)P2—C19—C24—C23178.6 (4)
P2—Cu1—N3—C3482.9 (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—C271.8 (9)
P1—Cu1—N3—C3591.9 (3)C25—C26—C27—C280.2 (10)
N1i—P1—C1—C641.9 (4)C26—C27—C28—C361.4 (9)
C7—P1—C1—C6151.0 (4)C26—C27—C28—C29176.8 (7)
Cu1—P1—C1—C682.1 (4)C27—C28—C29—C30178.1 (7)
N1i—P1—C1—C2147.0 (4)C36—C28—C29—C300.1 (11)
C7—P1—C1—C237.9 (4)C28—C29—C30—C310.6 (12)
Cu1—P1—C1—C289.0 (4)C29—C30—C31—C32178.5 (8)
C6—C1—C2—C30.7 (8)C29—C30—C31—C350.6 (11)
P1—C1—C2—C3172.0 (4)C35—C31—C32—C330.2 (10)
C1—C2—C3—C40.5 (9)C30—C31—C32—C33178.1 (7)
C2—C3—C4—C50.7 (11)C31—C32—C33—C340.1 (10)
C3—C4—C5—C61.1 (11)C35—N3—C34—C332.1 (8)
C2—C1—C6—C51.0 (8)Cu1—N3—C34—C33171.7 (4)
P1—C1—C6—C5172.3 (5)C32—C33—C34—N31.0 (10)
C4—C5—C6—C11.2 (10)C34—N3—C35—C312.3 (7)
N1i—P1—C7—C12137.2 (4)Cu1—N3—C35—C31173.6 (4)
C1—P1—C7—C12117.0 (4)C34—N3—C35—C36177.3 (4)
Cu1—P1—C7—C120.3 (4)Cu1—N3—C35—C366.0 (5)
N1i—P1—C7—C844.6 (5)C32—C31—C35—N31.4 (8)
C1—P1—C7—C861.1 (4)C30—C31—C35—N3179.5 (6)
Cu1—P1—C7—C8177.8 (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—C281.1 (7)
C7—C8—C9—C100.4 (10)Cu1—N2—C36—C28174.8 (4)
C8—C9—C10—C110.7 (11)C25—N2—C36—C35176.8 (4)
C9—C10—C11—C120.6 (10)Cu1—N2—C36—C353.0 (5)
C8—C7—C12—C111.5 (8)C27—C28—C36—N20.8 (8)
P1—C7—C12—C11179.7 (4)C29—C28—C36—N2177.5 (5)
C10—C11—C12—C70.5 (9)C27—C28—C36—C35178.7 (5)
C19—P2—N1—P1i122.7 (3)C29—C28—C36—C350.3 (8)
C13—P2—N1—P1i132.0 (3)N3—C35—C36—N22.0 (7)
Cu1—P2—N1—P1i11.6 (3)C31—C35—C36—N2177.7 (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 code: (i) x, y, z+1/2.

Experimental details

Crystal data
Chemical formula[Cu2(C25H21NP2)2(C12H8N2)2](BF4)2·CH2Cl2
Mr1514.76
Crystal system, space groupOrthorhombic, Pbcn
Temperature (K)294
a, b, c (Å)19.8730 (15), 17.4039 (13), 21.0008 (16)
V3)7263.5 (9)
Z4
Radiation typeMo Kα
µ (mm1)0.81
Crystal size (mm)0.26 × 0.18 × 0.10
Data collection
DiffractometerBruker SMART CCD area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2003)
Tmin, Tmax0.833, 0.919
No. of measured, independent and
observed [I > 2σ(I)] reflections
34870, 6356, 4243
Rint0.046
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.049, 0.195, 1.01
No. of reflections6356
No. of parameters478
No. of restraints93
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.96, 0.30

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXTL.

Selected geometric parameters (Å, º) 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)
 

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