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The title complex, [Cu2(C10H4N4)(C41H39P3)2](BF4)2·CH2Cl2, was synthesized and characterized. Two copper(I) ions are bridged by 4,4′-di-4-pyridyl­diazene (more commonly as 4,4′-azobi­pyridine). The discrete dinuclear cation contains two distorted tetrahedral copper(I) centers. Each CuI atom is coordinated by one 1,1,1-tris­(di­phenyl­phosphino­methyl)­ethane mol­ecule and one 4,4′-azobi­pyridine ligand. The complex sits on a center of symmetry; the solvent molecule is disordered across another center of symmetry. On irradiation of the copper(I) complex in di­chloro­methane at 365 nm, the trans/cis ratio of the complex is reversed.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804031903/fl6133sup1.cif
Contains datablocks global, publication_text

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804031903/fl6133Isup2.hkl
Contains datablock I

CCDC reference: 262253

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.009 Å
  • H-atom completeness 98%
  • Disorder in solvent or counterion
  • R factor = 0.048
  • wR factor = 0.146
  • Data-to-parameter ratio = 16.4

checkCIF/PLATON results

No syntax errors found




Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.100 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.63 Ratio PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for B1 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 11.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C93 H88 B2 Cl2 Cu2 F8 N4 P6 Atom count from _chemical_formula_moiety:C93 H88 B2 Cl2 Cu2 F2 N4 P6 FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C93 H88 B2 Cl2 Cu2 F8 N4 P6 Atom count from the _atom_site data: C93 H86 B2 Cl2 Cu2 F8 N4 P6 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C93 H88 B2 Cl2 Cu2 F8 N4 P6 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 186.00 186.00 0.00 H 176.00 172.00 4.00 B 4.00 4.00 0.00 Cl 4.00 4.00 0.00 Cu 4.00 4.00 0.00 F 16.00 16.00 0.00 N 8.00 8.00 0.00 P 12.00 12.00 0.00
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

µ-4,4'-Di-4-pyridyldiazene-κ2N:N'- bis{[1,1,1-tris(diphenylphosphinomethyl)ethane-κP3]copper(I)} bis(tetrafluoroboride) dichloromethane solvate top
Crystal data top
[Cu2(C10H4N4)(C41H39P3)2](BF4)2·CH2Cl2F(000) = 1876
Mr = 1819.09Dx = 1.416 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 16.029 (11) ÅCell parameters from 933 reflections
b = 12.985 (9) Åθ = 3.4–23.2°
c = 21.106 (14) ŵ = 0.74 mm1
β = 103.768 (12)°T = 293 K
V = 4267 (5) Å3Block, brown
Z = 20.22 × 0.20 × 0.16 mm
Data collection top
Bruker CCD area-detector
diffractometer
8715 independent reflections
Radiation source: fine-focus sealed tube4513 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.100
φ and ω scansθmax = 26.4°, θmin = 1.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1819
Tmin = 0.834, Tmax = 0.883k = 1416
23889 measured reflectionsl = 2626
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)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.146H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0727P)2]
where P = (Fo2 + 2Fc2)/3
8715 reflections(Δ/σ)max < 0.001
533 parametersΔρmax = 0.75 e Å3
13 restraintsΔρmin = 0.58 e Å3
Special details top

Experimental. Element analysis was measured on Carlo Erba Corporation Model 1104 element analysis instrument. IR spectra were recorded on a Bio-Rad FTS 165 F T—IR spectrum spectrometer.

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)
Cu10.31419 (4)0.91277 (5)0.34514 (3)0.0329 (2)
P10.16792 (8)0.88993 (11)0.29806 (7)0.0305 (3)
P20.33827 (9)0.99731 (11)0.25460 (7)0.0309 (3)
P30.30151 (9)1.06800 (11)0.39745 (7)0.0318 (4)
N10.3836 (3)0.7904 (3)0.3945 (2)0.0328 (11)
N20.5210 (3)0.5320 (3)0.4881 (2)0.0380 (11)
C10.3420 (3)0.7055 (4)0.4073 (3)0.0384 (14)
H10.28230.70530.39480.046*
C20.3826 (3)0.6190 (4)0.4376 (3)0.0361 (14)
H20.35080.56230.44530.043*
C30.4710 (3)0.6179 (4)0.4565 (3)0.0331 (13)
C40.5149 (3)0.7035 (4)0.4435 (3)0.0390 (14)
H40.57460.70490.45520.047*
C50.4694 (3)0.7868 (4)0.4132 (3)0.0422 (15)
H50.50010.84410.40520.051*
C60.1008 (3)0.8840 (4)0.3574 (3)0.0306 (12)
C70.1386 (4)0.8817 (5)0.4229 (3)0.0489 (16)
H70.19820.88200.43660.059*
C80.0899 (5)0.8787 (6)0.4691 (3)0.065 (2)
H80.11680.87910.51330.078*
C90.0027 (4)0.8753 (5)0.4496 (3)0.0567 (18)
H90.03020.87220.48040.068*
C100.0360 (4)0.8763 (5)0.3845 (3)0.0491 (17)
H100.09560.87370.37110.059*
C110.0120 (3)0.8812 (4)0.3383 (3)0.0399 (14)
H110.01540.88270.29420.048*
C120.1176 (3)0.7931 (4)0.2379 (3)0.0309 (13)
C130.0563 (3)0.8156 (5)0.1816 (3)0.0409 (14)
H130.03720.88300.17370.049*
C140.0229 (4)0.7403 (5)0.1371 (3)0.0509 (17)
H140.01810.75770.09940.061*
C150.0490 (4)0.6409 (5)0.1473 (3)0.0566 (18)
H150.02680.59040.11660.068*
C160.1095 (4)0.6156 (5)0.2043 (3)0.0566 (18)
H160.12730.54760.21240.068*
C170.1428 (4)0.6911 (5)0.2487 (3)0.0431 (15)
H170.18310.67350.28670.052*
C180.1352 (3)1.0092 (4)0.2521 (2)0.0332 (13)
H18A0.13520.99560.20700.040*
H18B0.07621.02290.25350.040*
C190.1865 (3)1.1093 (4)0.2721 (2)0.0311 (13)
C200.1297 (4)1.1986 (5)0.2390 (3)0.0506 (17)
H20A0.11281.18670.19280.076*
H20B0.16131.26200.24740.076*
H20C0.07941.20300.25620.076*
C210.2694 (3)1.1135 (4)0.2462 (3)0.0361 (13)
H21A0.30451.16970.26830.043*
H21B0.25271.13110.20030.043*
C220.3011 (3)0.9366 (4)0.1750 (3)0.0344 (13)
C230.2916 (4)0.9928 (5)0.1173 (3)0.0493 (16)
H230.30721.06200.11920.059*
C240.2598 (4)0.9472 (7)0.0578 (3)0.067 (2)
H240.25440.98550.01980.080*
C250.2360 (4)0.8462 (7)0.0540 (4)0.072 (2)
H250.21350.81630.01340.086*
C260.2451 (4)0.7885 (6)0.1094 (4)0.064 (2)
H260.22950.71940.10670.077*
C270.2780 (3)0.8341 (5)0.1701 (3)0.0414 (15)
H270.28440.79490.20780.050*
C280.4436 (3)1.0447 (4)0.2473 (2)0.0316 (13)
C290.5061 (4)0.9717 (5)0.2491 (3)0.0546 (17)
H290.49330.90270.25380.065*
C300.5879 (4)0.9987 (6)0.2440 (3)0.0558 (18)
H300.62930.94800.24570.067*
C310.6076 (4)1.0982 (6)0.2364 (3)0.0517 (17)
H310.66221.11680.23250.062*
C320.5462 (4)1.1703 (6)0.2348 (3)0.064 (2)
H320.55991.23920.23030.076*
C330.4644 (4)1.1457 (5)0.2394 (3)0.0538 (17)
H330.42341.19710.23720.065*
C340.2046 (3)1.1279 (4)0.3465 (2)0.0335 (13)
H34A0.15551.10340.36150.040*
H34B0.20851.20160.35400.040*
C350.3880 (3)1.1605 (4)0.3966 (3)0.0332 (13)
C360.3729 (4)1.2654 (4)0.3852 (3)0.0403 (14)
H360.31731.29120.37820.048*
C370.4399 (4)1.3305 (5)0.3841 (3)0.0455 (15)
H370.42901.40030.37620.055*
C380.5223 (4)1.2952 (5)0.3945 (3)0.0510 (17)
H380.56691.34040.39350.061*
C390.5388 (4)1.1913 (5)0.4064 (3)0.0519 (17)
H390.59471.16650.41370.062*
C400.4717 (4)1.1246 (5)0.4075 (3)0.0442 (15)
H400.48291.05500.41550.053*
C410.2857 (3)1.0908 (4)0.4797 (3)0.0364 (13)
C420.3190 (4)1.0208 (5)0.5277 (3)0.0594 (19)
H420.34610.96190.51740.071*
C430.3128 (5)1.0363 (7)0.5912 (3)0.080 (2)
H430.33540.98800.62320.096*
C440.2734 (5)1.1224 (7)0.6069 (3)0.070 (2)
H440.26941.13300.64960.084*
C450.2402 (4)1.1926 (6)0.5599 (4)0.063 (2)
H450.21341.25130.57070.076*
C460.2459 (4)1.1776 (5)0.4964 (3)0.0528 (17)
H460.22281.22610.46460.063*
B10.1798 (6)0.4621 (7)0.3609 (5)0.065 (2)
F10.1845 (3)0.5558 (4)0.3909 (2)0.1057 (16)
F20.2378 (3)0.4595 (5)0.3235 (3)0.132 (2)
F30.1016 (4)0.4554 (6)0.3221 (3)0.154 (3)
F40.1938 (4)0.3884 (4)0.4065 (3)0.143 (2)
C470.0280 (17)0.0044 (19)0.0277 (9)0.166 (10)0.50
Cl10.0391 (4)0.0809 (4)0.0425 (3)0.240 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0312 (4)0.0349 (4)0.0332 (4)0.0035 (3)0.0088 (3)0.0049 (3)
P10.0281 (7)0.0353 (8)0.0294 (8)0.0010 (6)0.0095 (6)0.0026 (6)
P20.0312 (7)0.0346 (8)0.0290 (8)0.0014 (6)0.0116 (6)0.0017 (6)
P30.0315 (8)0.0365 (8)0.0291 (8)0.0030 (7)0.0105 (6)0.0005 (6)
N10.030 (3)0.037 (3)0.032 (3)0.002 (2)0.009 (2)0.001 (2)
N20.038 (3)0.030 (3)0.041 (3)0.003 (2)0.002 (2)0.007 (2)
C10.029 (3)0.042 (4)0.042 (4)0.002 (3)0.005 (3)0.005 (3)
C20.037 (3)0.031 (3)0.039 (4)0.000 (3)0.005 (3)0.007 (3)
C30.036 (3)0.033 (3)0.029 (3)0.004 (3)0.006 (3)0.001 (2)
C40.025 (3)0.040 (3)0.048 (4)0.001 (3)0.002 (3)0.008 (3)
C50.038 (3)0.034 (3)0.054 (4)0.004 (3)0.010 (3)0.008 (3)
C60.034 (3)0.030 (3)0.029 (3)0.002 (2)0.011 (2)0.001 (2)
C70.042 (3)0.068 (5)0.037 (4)0.002 (3)0.009 (3)0.007 (3)
C80.066 (5)0.096 (6)0.035 (4)0.007 (4)0.015 (3)0.013 (4)
C90.061 (5)0.065 (5)0.054 (5)0.003 (4)0.033 (4)0.006 (4)
C100.037 (3)0.062 (4)0.054 (5)0.005 (3)0.021 (3)0.006 (3)
C110.036 (3)0.049 (4)0.035 (3)0.007 (3)0.009 (3)0.007 (3)
C120.028 (3)0.041 (3)0.028 (3)0.002 (3)0.015 (2)0.003 (3)
C130.039 (3)0.046 (4)0.034 (4)0.003 (3)0.003 (3)0.002 (3)
C140.053 (4)0.060 (4)0.036 (4)0.002 (3)0.004 (3)0.002 (3)
C150.064 (4)0.055 (4)0.048 (5)0.011 (4)0.008 (4)0.008 (4)
C160.074 (5)0.036 (4)0.058 (5)0.003 (3)0.012 (4)0.006 (3)
C170.047 (4)0.045 (4)0.033 (4)0.002 (3)0.002 (3)0.003 (3)
C180.026 (3)0.046 (3)0.027 (3)0.003 (3)0.004 (2)0.006 (3)
C190.033 (3)0.036 (3)0.024 (3)0.003 (2)0.007 (2)0.006 (2)
C200.050 (4)0.047 (4)0.053 (4)0.016 (3)0.010 (3)0.014 (3)
C210.047 (3)0.034 (3)0.029 (3)0.001 (3)0.013 (3)0.004 (3)
C220.029 (3)0.040 (3)0.036 (3)0.004 (3)0.010 (2)0.004 (3)
C230.057 (4)0.058 (4)0.035 (4)0.009 (3)0.015 (3)0.003 (3)
C240.067 (5)0.096 (6)0.035 (4)0.017 (5)0.008 (3)0.005 (4)
C250.054 (5)0.109 (7)0.052 (5)0.004 (5)0.012 (4)0.036 (5)
C260.050 (4)0.068 (5)0.081 (6)0.013 (4)0.026 (4)0.032 (5)
C270.031 (3)0.051 (4)0.047 (4)0.005 (3)0.017 (3)0.008 (3)
C280.031 (3)0.040 (3)0.027 (3)0.004 (3)0.013 (2)0.000 (3)
C290.037 (4)0.047 (4)0.080 (5)0.004 (3)0.014 (3)0.007 (4)
C300.042 (4)0.069 (5)0.056 (4)0.009 (4)0.011 (3)0.007 (4)
C310.044 (4)0.074 (5)0.040 (4)0.010 (4)0.018 (3)0.004 (4)
C320.062 (5)0.053 (4)0.083 (6)0.014 (4)0.033 (4)0.007 (4)
C330.049 (4)0.045 (4)0.075 (5)0.001 (3)0.032 (4)0.008 (3)
C340.029 (3)0.035 (3)0.038 (3)0.005 (2)0.012 (3)0.003 (3)
C350.031 (3)0.044 (3)0.026 (3)0.002 (3)0.008 (2)0.003 (3)
C360.040 (3)0.038 (3)0.041 (4)0.001 (3)0.007 (3)0.001 (3)
C370.054 (4)0.041 (4)0.041 (4)0.011 (3)0.012 (3)0.004 (3)
C380.048 (4)0.066 (5)0.041 (4)0.019 (4)0.015 (3)0.000 (3)
C390.034 (3)0.068 (5)0.055 (4)0.003 (3)0.012 (3)0.005 (4)
C400.039 (3)0.047 (4)0.047 (4)0.001 (3)0.012 (3)0.000 (3)
C410.036 (3)0.049 (4)0.027 (3)0.006 (3)0.013 (2)0.006 (3)
C420.079 (5)0.065 (5)0.033 (4)0.021 (4)0.011 (3)0.004 (3)
C430.106 (6)0.100 (6)0.033 (4)0.022 (5)0.015 (4)0.013 (4)
C440.073 (5)0.107 (7)0.033 (4)0.010 (5)0.021 (4)0.011 (4)
C450.065 (5)0.073 (5)0.056 (5)0.008 (4)0.023 (4)0.015 (4)
C460.066 (4)0.059 (4)0.038 (4)0.006 (4)0.021 (3)0.005 (3)
B10.058 (6)0.053 (5)0.085 (7)0.001 (5)0.020 (5)0.005 (5)
F10.135 (4)0.069 (3)0.104 (4)0.017 (3)0.010 (3)0.003 (3)
F20.110 (4)0.169 (5)0.139 (5)0.041 (4)0.073 (4)0.050 (4)
F30.096 (4)0.221 (7)0.127 (5)0.085 (4)0.008 (3)0.004 (5)
F40.235 (7)0.084 (4)0.135 (5)0.064 (4)0.095 (5)0.058 (3)
C470.166 (10)0.166 (10)0.166 (10)0.0004 (10)0.040 (3)0.0001 (10)
Cl10.241 (2)0.240 (2)0.240 (2)0.0006 (10)0.0574 (11)0.0037 (10)
Geometric parameters (Å, º) top
Cu1—N12.072 (4)C21—H21A0.9700
Cu1—P22.3145 (19)C21—H21B0.9700
Cu1—P32.330 (2)C22—C271.378 (8)
Cu1—P12.337 (2)C22—C231.397 (8)
P1—C121.832 (6)C23—C241.372 (9)
P1—C181.836 (5)C23—H230.9300
P1—C61.837 (5)C24—C251.363 (10)
P2—C221.824 (6)C24—H240.9300
P2—C281.838 (5)C25—C261.367 (10)
P2—C211.853 (5)C25—H250.9300
P3—C411.837 (5)C26—C271.397 (9)
P3—C351.838 (6)C26—H260.9300
P3—C341.838 (5)C27—H270.9300
N1—C51.338 (6)C28—C291.373 (7)
N1—C11.350 (7)C28—C331.373 (8)
N2—N2i1.247 (8)C29—C301.385 (8)
N2—C31.442 (6)C29—H290.9300
C1—C21.377 (7)C30—C311.348 (9)
C1—H10.9300C30—H300.9300
C2—C31.378 (7)C31—C321.353 (9)
C2—H20.9300C31—H310.9300
C3—C41.378 (7)C32—C331.377 (8)
C4—C51.375 (7)C32—H320.9300
C4—H40.9300C33—H330.9300
C5—H50.9300C34—H34A0.9700
C6—C71.371 (8)C34—H34B0.9700
C6—C111.384 (7)C35—C401.387 (7)
C7—C81.387 (8)C35—C361.394 (7)
C7—H70.9300C36—C371.372 (7)
C8—C91.360 (9)C36—H360.9300
C8—H80.9300C37—C381.365 (8)
C9—C101.367 (8)C37—H370.9300
C9—H90.9300C38—C391.386 (8)
C10—C111.379 (8)C38—H380.9300
C10—H100.9300C39—C401.385 (8)
C11—H110.9300C39—H390.9300
C12—C131.381 (7)C40—H400.9300
C12—C171.388 (7)C41—C421.372 (8)
C13—C141.373 (8)C41—C461.381 (8)
C13—H130.9300C42—C431.381 (9)
C14—C151.359 (8)C42—H420.9300
C14—H140.9300C43—C441.362 (10)
C15—C161.395 (9)C43—H430.9300
C15—H150.9300C44—C451.359 (9)
C16—C171.373 (8)C44—H440.9300
C16—H160.9300C45—C461.379 (8)
C17—H170.9300C45—H450.9300
C18—C191.542 (7)C46—H460.9300
C18—H18A0.9700B1—F31.327 (10)
C18—H18B0.9700B1—F41.337 (9)
C19—C201.536 (7)B1—F21.356 (9)
C19—C341.546 (7)B1—F11.366 (10)
C19—C211.554 (7)C47—Cl1ii1.52 (2)
C20—H20A0.9600C47—C47ii1.64 (4)
C20—H20B0.9600C47—Cl11.757 (10)
C20—H20C0.9600Cl1—C47ii1.52 (2)
N1—Cu1—P2127.11 (13)H20B—C20—H20C109.5
N1—Cu1—P3121.46 (13)C19—C21—P2118.6 (4)
P2—Cu1—P391.80 (7)C19—C21—H21A107.7
N1—Cu1—P1118.74 (13)P2—C21—H21A107.7
P2—Cu1—P193.25 (6)C19—C21—H21B107.7
P3—Cu1—P196.85 (6)P2—C21—H21B107.7
C12—P1—C18101.0 (2)H21A—C21—H21B107.1
C12—P1—C6102.2 (2)C27—C22—C23118.0 (5)
C18—P1—C6104.8 (2)C27—C22—P2120.6 (5)
C12—P1—Cu1127.83 (17)C23—C22—P2121.4 (4)
C18—P1—Cu1104.41 (17)C24—C23—C22120.7 (7)
C6—P1—Cu1113.99 (18)C24—C23—H23119.6
C22—P2—C2899.9 (2)C22—C23—H23119.6
C22—P2—C21102.0 (2)C25—C24—C23120.5 (7)
C28—P2—C21104.9 (2)C25—C24—H24119.7
C22—P2—Cu1118.28 (19)C23—C24—H24119.7
C28—P2—Cu1124.41 (18)C24—C25—C26120.3 (7)
C21—P2—Cu1104.63 (17)C24—C25—H25119.8
C41—P3—C35100.2 (2)C26—C25—H25119.8
C41—P3—C34101.4 (2)C25—C26—C27119.6 (7)
C35—P3—C34104.6 (3)C25—C26—H26120.2
C41—P3—Cu1129.4 (2)C27—C26—H26120.2
C35—P3—Cu1114.20 (18)C22—C27—C26120.9 (6)
C34—P3—Cu1104.21 (18)C22—C27—H27119.6
C5—N1—C1115.8 (5)C26—C27—H27119.6
C5—N1—Cu1124.5 (4)C29—C28—C33117.8 (5)
C1—N1—Cu1119.7 (4)C29—C28—P2116.5 (4)
N2i—N2—C3114.1 (5)C33—C28—P2125.7 (4)
N1—C1—C2123.9 (5)C28—C29—C30121.4 (6)
N1—C1—H1118.0C28—C29—H29119.3
C2—C1—H1118.0C30—C29—H29119.3
C1—C2—C3118.9 (5)C31—C30—C29120.3 (6)
C1—C2—H2120.6C31—C30—H30119.8
C3—C2—H2120.6C29—C30—H30119.8
C4—C3—C2118.3 (5)C30—C31—C32118.5 (6)
C4—C3—N2117.5 (5)C30—C31—H31120.8
C2—C3—N2124.2 (5)C32—C31—H31120.8
C5—C4—C3119.2 (5)C31—C32—C33122.5 (6)
C5—C4—H4120.4C31—C32—H32118.8
C3—C4—H4120.4C33—C32—H32118.8
N1—C5—C4124.0 (5)C28—C33—C32119.6 (6)
N1—C5—H5118.0C28—C33—H33120.2
C4—C5—H5118.0C32—C33—H33120.2
C7—C6—C11118.0 (5)C19—C34—P3117.2 (3)
C7—C6—P1119.9 (4)C19—C34—H34A108.0
C11—C6—P1122.1 (4)P3—C34—H34A108.0
C6—C7—C8121.4 (6)C19—C34—H34B108.0
C6—C7—H7119.3P3—C34—H34B108.0
C8—C7—H7119.3H34A—C34—H34B107.2
C9—C8—C7119.9 (6)C40—C35—C36118.6 (5)
C9—C8—H8120.0C40—C35—P3118.8 (4)
C7—C8—H8120.0C36—C35—P3122.6 (4)
C8—C9—C10119.4 (6)C37—C36—C35120.0 (5)
C8—C9—H9120.3C37—C36—H36120.0
C10—C9—H9120.3C35—C36—H36120.0
C9—C10—C11121.0 (6)C38—C37—C36121.4 (6)
C9—C10—H10119.5C38—C37—H37119.3
C11—C10—H10119.5C36—C37—H37119.3
C10—C11—C6120.2 (6)C37—C38—C39119.4 (6)
C10—C11—H11119.9C37—C38—H38120.3
C6—C11—H11119.9C39—C38—H38120.3
C13—C12—C17117.5 (5)C40—C39—C38119.8 (6)
C13—C12—P1123.9 (4)C40—C39—H39120.1
C17—C12—P1118.6 (4)C38—C39—H39120.1
C14—C13—C12121.4 (6)C39—C40—C35120.8 (6)
C14—C13—H13119.3C39—C40—H40119.6
C12—C13—H13119.3C35—C40—H40119.6
C15—C14—C13120.8 (6)C42—C41—C46118.3 (6)
C15—C14—H14119.6C42—C41—P3118.4 (5)
C13—C14—H14119.6C46—C41—P3123.2 (5)
C14—C15—C16119.1 (6)C41—C42—C43121.0 (7)
C14—C15—H15120.5C41—C42—H42119.5
C16—C15—H15120.5C43—C42—H42119.5
C17—C16—C15119.9 (6)C44—C43—C42120.0 (7)
C17—C16—H16120.1C44—C43—H43120.0
C15—C16—H16120.1C42—C43—H43120.0
C16—C17—C12121.3 (5)C45—C44—C43119.8 (7)
C16—C17—H17119.3C45—C44—H44120.1
C12—C17—H17119.3C43—C44—H44120.1
C19—C18—P1120.0 (3)C44—C45—C46120.6 (7)
C19—C18—H18A107.3C44—C45—H45119.7
P1—C18—H18A107.3C46—C45—H45119.7
C19—C18—H18B107.3C45—C46—C41120.3 (6)
P1—C18—H18B107.3C45—C46—H46119.9
H18A—C18—H18B106.9C41—C46—H46119.9
C20—C19—C18107.0 (4)F3—B1—F4111.7 (8)
C20—C19—C34107.0 (4)F3—B1—F2108.5 (8)
C18—C19—C34111.6 (4)F4—B1—F2112.3 (7)
C20—C19—C21106.2 (4)F3—B1—F1106.5 (7)
C18—C19—C21112.2 (4)F4—B1—F1108.8 (8)
C34—C19—C21112.4 (4)F2—B1—F1108.8 (7)
C19—C20—H20A109.5Cl1ii—C47—C47ii67.4 (16)
C19—C20—H20B109.5Cl1ii—C47—Cl1120.6 (15)
H20A—C20—H20B109.5C47ii—C47—Cl153.2 (7)
C19—C20—H20C109.5C47ii—Cl1—C4759.4 (15)
H20A—C20—H20C109.5
N1—Cu1—P1—C1256.9 (3)C6—P1—C18—C1995.6 (4)
P2—Cu1—P1—C1279.1 (2)Cu1—P1—C18—C1924.5 (4)
P3—Cu1—P1—C12171.3 (2)P1—C18—C19—C20163.6 (4)
N1—Cu1—P1—C18173.6 (2)P1—C18—C19—C3446.9 (5)
P2—Cu1—P1—C1837.49 (18)P1—C18—C19—C2180.3 (5)
P3—Cu1—P1—C1854.71 (19)C20—C19—C21—P2161.6 (4)
N1—Cu1—P1—C672.7 (2)C18—C19—C21—P245.0 (6)
P2—Cu1—P1—C6151.23 (19)C34—C19—C21—P281.8 (5)
P3—Cu1—P1—C659.03 (19)C22—P2—C21—C1996.0 (4)
N1—Cu1—P2—C2278.9 (2)C28—P2—C21—C19160.1 (4)
P3—Cu1—P2—C22148.38 (19)Cu1—P2—C21—C1927.8 (4)
P1—Cu1—P2—C2251.41 (19)C28—P2—C22—C27123.2 (4)
N1—Cu1—P2—C2848.4 (3)C21—P2—C22—C27129.0 (4)
P3—Cu1—P2—C2884.3 (2)Cu1—P2—C22—C2715.0 (5)
P1—Cu1—P2—C28178.7 (2)C28—P2—C22—C2359.4 (5)
N1—Cu1—P2—C21168.5 (2)C21—P2—C22—C2348.3 (5)
P3—Cu1—P2—C2135.80 (19)Cu1—P2—C22—C23162.3 (4)
P1—Cu1—P2—C2161.17 (19)C27—C22—C23—C240.5 (8)
N1—Cu1—P3—C4140.1 (3)P2—C22—C23—C24176.9 (5)
P2—Cu1—P3—C41176.7 (2)C22—C23—C24—C250.5 (10)
P1—Cu1—P3—C4189.8 (2)C23—C24—C25—C261.2 (11)
N1—Cu1—P3—C3588.2 (2)C24—C25—C26—C270.8 (10)
P2—Cu1—P3—C3548.4 (2)C23—C22—C27—C260.8 (8)
P1—Cu1—P3—C35141.9 (2)P2—C22—C27—C26176.6 (4)
N1—Cu1—P3—C34158.3 (2)C25—C26—C27—C220.2 (9)
P2—Cu1—P3—C3465.10 (19)C22—P2—C28—C2971.9 (5)
P1—Cu1—P3—C3428.39 (19)C21—P2—C28—C29177.3 (4)
P2—Cu1—N1—C547.6 (5)Cu1—P2—C28—C2962.8 (5)
P3—Cu1—N1—C573.0 (5)C22—P2—C28—C33107.2 (6)
P1—Cu1—N1—C5167.3 (4)C21—P2—C28—C331.8 (6)
P2—Cu1—N1—C1129.6 (4)Cu1—P2—C28—C33118.2 (5)
P3—Cu1—N1—C1109.8 (4)C33—C28—C29—C300.8 (9)
P1—Cu1—N1—C19.9 (4)P2—C28—C29—C30180.0 (5)
C5—N1—C1—C20.2 (8)C28—C29—C30—C310.6 (10)
Cu1—N1—C1—C2177.6 (4)C29—C30—C31—C320.7 (10)
N1—C1—C2—C30.0 (9)C30—C31—C32—C331.0 (11)
C1—C2—C3—C40.5 (8)C29—C28—C33—C321.1 (9)
C1—C2—C3—N2179.5 (5)P2—C28—C33—C32179.8 (5)
N2i—N2—C3—C4164.1 (6)C31—C32—C33—C281.3 (11)
N2i—N2—C3—C216.9 (9)C20—C19—C34—P3156.3 (4)
C2—C3—C4—C50.7 (8)C18—C19—C34—P387.0 (5)
N2—C3—C4—C5179.8 (5)C21—C19—C34—P340.2 (6)
C1—N1—C5—C40.0 (8)C41—P3—C34—C19170.3 (4)
Cu1—N1—C5—C4177.2 (4)C35—P3—C34—C1985.8 (4)
C3—C4—C5—N10.5 (9)Cu1—P3—C34—C1934.4 (4)
C12—P1—C6—C7134.5 (5)C41—P3—C35—C40100.6 (5)
C18—P1—C6—C7120.6 (5)C34—P3—C35—C40154.6 (4)
Cu1—P1—C6—C77.0 (5)Cu1—P3—C35—C4041.4 (5)
C12—P1—C6—C1145.1 (5)C41—P3—C35—C3679.8 (5)
C18—P1—C6—C1159.8 (5)C34—P3—C35—C3624.9 (5)
Cu1—P1—C6—C11173.4 (4)Cu1—P3—C35—C36138.2 (4)
C11—C6—C7—C81.3 (9)C40—C35—C36—C370.6 (8)
P1—C6—C7—C8179.0 (5)P3—C35—C36—C37178.9 (4)
C6—C7—C8—C91.8 (10)C35—C36—C37—C380.3 (9)
C7—C8—C9—C101.0 (11)C36—C37—C38—C390.1 (9)
C8—C9—C10—C110.2 (10)C37—C38—C39—C400.2 (9)
C9—C10—C11—C60.7 (9)C38—C39—C40—C350.0 (9)
C7—C6—C11—C100.1 (8)C36—C35—C40—C390.5 (8)
P1—C6—C11—C10179.7 (4)P3—C35—C40—C39179.1 (5)
C18—P1—C12—C1313.3 (5)C35—P3—C41—C42103.0 (5)
C6—P1—C12—C1394.7 (5)C34—P3—C41—C42149.7 (5)
Cu1—P1—C12—C13131.4 (4)Cu1—P3—C41—C4230.3 (6)
C18—P1—C12—C17165.9 (4)C35—P3—C41—C4673.6 (5)
C6—P1—C12—C1786.2 (4)C34—P3—C41—C4633.7 (6)
Cu1—P1—C12—C1747.8 (5)Cu1—P3—C41—C46153.0 (4)
C17—C12—C13—C141.5 (8)C46—C41—C42—C430.1 (10)
P1—C12—C13—C14177.7 (4)P3—C41—C42—C43176.9 (6)
C12—C13—C14—C150.3 (10)C41—C42—C43—C440.2 (12)
C13—C14—C15—C161.0 (10)C42—C43—C44—C450.2 (12)
C14—C15—C16—C171.1 (10)C43—C44—C45—C460.0 (11)
C15—C16—C17—C120.1 (10)C44—C45—C46—C410.1 (10)
C13—C12—C17—C161.4 (8)C42—C41—C46—C450.1 (9)
P1—C12—C17—C16177.8 (5)P3—C41—C46—C45176.5 (5)
C12—P1—C18—C19158.5 (4)Cl1ii—C47—Cl1—C47ii0.000 (2)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y, z.
 

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