Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804031903/fl6133sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804031903/fl6133Isup2.hkl |
CCDC reference: 262253
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.
[Cu2(C10H4N4)(C41H39P3)2](BF4)2·CH2Cl2 | F(000) = 1876 |
Mr = 1819.09 | Dx = 1.416 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 16.029 (11) Å | Cell parameters from 933 reflections |
b = 12.985 (9) Å | θ = 3.4–23.2° |
c = 21.106 (14) Å | µ = 0.74 mm−1 |
β = 103.768 (12)° | T = 293 K |
V = 4267 (5) Å3 | Block, brown |
Z = 2 | 0.22 × 0.20 × 0.16 mm |
Bruker CCD area-detector diffractometer | 8715 independent reflections |
Radiation source: fine-focus sealed tube | 4513 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.100 |
φ and ω scans | θmax = 26.4°, θmin = 1.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −18→19 |
Tmin = 0.834, Tmax = 0.883 | k = −14→16 |
23889 measured reflections | l = −26→26 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.146 | H-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 parameters | Δρmax = 0.75 e Å−3 |
13 restraints | Δρmin = −0.58 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cu1 | 0.31419 (4) | 0.91277 (5) | 0.34514 (3) | 0.0329 (2) | |
P1 | 0.16792 (8) | 0.88993 (11) | 0.29806 (7) | 0.0305 (3) | |
P2 | 0.33827 (9) | 0.99731 (11) | 0.25460 (7) | 0.0309 (3) | |
P3 | 0.30151 (9) | 1.06800 (11) | 0.39745 (7) | 0.0318 (4) | |
N1 | 0.3836 (3) | 0.7904 (3) | 0.3945 (2) | 0.0328 (11) | |
N2 | 0.5210 (3) | 0.5320 (3) | 0.4881 (2) | 0.0380 (11) | |
C1 | 0.3420 (3) | 0.7055 (4) | 0.4073 (3) | 0.0384 (14) | |
H1 | 0.2823 | 0.7053 | 0.3948 | 0.046* | |
C2 | 0.3826 (3) | 0.6190 (4) | 0.4376 (3) | 0.0361 (14) | |
H2 | 0.3508 | 0.5623 | 0.4453 | 0.043* | |
C3 | 0.4710 (3) | 0.6179 (4) | 0.4565 (3) | 0.0331 (13) | |
C4 | 0.5149 (3) | 0.7035 (4) | 0.4435 (3) | 0.0390 (14) | |
H4 | 0.5746 | 0.7049 | 0.4552 | 0.047* | |
C5 | 0.4694 (3) | 0.7868 (4) | 0.4132 (3) | 0.0422 (15) | |
H5 | 0.5001 | 0.8441 | 0.4052 | 0.051* | |
C6 | 0.1008 (3) | 0.8840 (4) | 0.3574 (3) | 0.0306 (12) | |
C7 | 0.1386 (4) | 0.8817 (5) | 0.4229 (3) | 0.0489 (16) | |
H7 | 0.1982 | 0.8820 | 0.4366 | 0.059* | |
C8 | 0.0899 (5) | 0.8787 (6) | 0.4691 (3) | 0.065 (2) | |
H8 | 0.1168 | 0.8791 | 0.5133 | 0.078* | |
C9 | 0.0027 (4) | 0.8753 (5) | 0.4496 (3) | 0.0567 (18) | |
H9 | −0.0302 | 0.8722 | 0.4804 | 0.068* | |
C10 | −0.0360 (4) | 0.8763 (5) | 0.3845 (3) | 0.0491 (17) | |
H10 | −0.0956 | 0.8737 | 0.3711 | 0.059* | |
C11 | 0.0120 (3) | 0.8812 (4) | 0.3383 (3) | 0.0399 (14) | |
H11 | −0.0154 | 0.8827 | 0.2942 | 0.048* | |
C12 | 0.1176 (3) | 0.7931 (4) | 0.2379 (3) | 0.0309 (13) | |
C13 | 0.0563 (3) | 0.8156 (5) | 0.1816 (3) | 0.0409 (14) | |
H13 | 0.0372 | 0.8830 | 0.1737 | 0.049* | |
C14 | 0.0229 (4) | 0.7403 (5) | 0.1371 (3) | 0.0509 (17) | |
H14 | −0.0181 | 0.7577 | 0.0994 | 0.061* | |
C15 | 0.0490 (4) | 0.6409 (5) | 0.1473 (3) | 0.0566 (18) | |
H15 | 0.0268 | 0.5904 | 0.1166 | 0.068* | |
C16 | 0.1095 (4) | 0.6156 (5) | 0.2043 (3) | 0.0566 (18) | |
H16 | 0.1273 | 0.5476 | 0.2124 | 0.068* | |
C17 | 0.1428 (4) | 0.6911 (5) | 0.2487 (3) | 0.0431 (15) | |
H17 | 0.1831 | 0.6735 | 0.2867 | 0.052* | |
C18 | 0.1352 (3) | 1.0092 (4) | 0.2521 (2) | 0.0332 (13) | |
H18A | 0.1352 | 0.9956 | 0.2070 | 0.040* | |
H18B | 0.0762 | 1.0229 | 0.2535 | 0.040* | |
C19 | 0.1865 (3) | 1.1093 (4) | 0.2721 (2) | 0.0311 (13) | |
C20 | 0.1297 (4) | 1.1986 (5) | 0.2390 (3) | 0.0506 (17) | |
H20A | 0.1128 | 1.1867 | 0.1928 | 0.076* | |
H20B | 0.1613 | 1.2620 | 0.2474 | 0.076* | |
H20C | 0.0794 | 1.2030 | 0.2562 | 0.076* | |
C21 | 0.2694 (3) | 1.1135 (4) | 0.2462 (3) | 0.0361 (13) | |
H21A | 0.3045 | 1.1697 | 0.2683 | 0.043* | |
H21B | 0.2527 | 1.1311 | 0.2003 | 0.043* | |
C22 | 0.3011 (3) | 0.9366 (4) | 0.1750 (3) | 0.0344 (13) | |
C23 | 0.2916 (4) | 0.9928 (5) | 0.1173 (3) | 0.0493 (16) | |
H23 | 0.3072 | 1.0620 | 0.1192 | 0.059* | |
C24 | 0.2598 (4) | 0.9472 (7) | 0.0578 (3) | 0.067 (2) | |
H24 | 0.2544 | 0.9855 | 0.0198 | 0.080* | |
C25 | 0.2360 (4) | 0.8462 (7) | 0.0540 (4) | 0.072 (2) | |
H25 | 0.2135 | 0.8163 | 0.0134 | 0.086* | |
C26 | 0.2451 (4) | 0.7885 (6) | 0.1094 (4) | 0.064 (2) | |
H26 | 0.2295 | 0.7194 | 0.1067 | 0.077* | |
C27 | 0.2780 (3) | 0.8341 (5) | 0.1701 (3) | 0.0414 (15) | |
H27 | 0.2844 | 0.7949 | 0.2078 | 0.050* | |
C28 | 0.4436 (3) | 1.0447 (4) | 0.2473 (2) | 0.0316 (13) | |
C29 | 0.5061 (4) | 0.9717 (5) | 0.2491 (3) | 0.0546 (17) | |
H29 | 0.4933 | 0.9027 | 0.2538 | 0.065* | |
C30 | 0.5879 (4) | 0.9987 (6) | 0.2440 (3) | 0.0558 (18) | |
H30 | 0.6293 | 0.9480 | 0.2457 | 0.067* | |
C31 | 0.6076 (4) | 1.0982 (6) | 0.2364 (3) | 0.0517 (17) | |
H31 | 0.6622 | 1.1168 | 0.2325 | 0.062* | |
C32 | 0.5462 (4) | 1.1703 (6) | 0.2348 (3) | 0.064 (2) | |
H32 | 0.5599 | 1.2392 | 0.2303 | 0.076* | |
C33 | 0.4644 (4) | 1.1457 (5) | 0.2394 (3) | 0.0538 (17) | |
H33 | 0.4234 | 1.1971 | 0.2372 | 0.065* | |
C34 | 0.2046 (3) | 1.1279 (4) | 0.3465 (2) | 0.0335 (13) | |
H34A | 0.1555 | 1.1034 | 0.3615 | 0.040* | |
H34B | 0.2085 | 1.2016 | 0.3540 | 0.040* | |
C35 | 0.3880 (3) | 1.1605 (4) | 0.3966 (3) | 0.0332 (13) | |
C36 | 0.3729 (4) | 1.2654 (4) | 0.3852 (3) | 0.0403 (14) | |
H36 | 0.3173 | 1.2912 | 0.3782 | 0.048* | |
C37 | 0.4399 (4) | 1.3305 (5) | 0.3841 (3) | 0.0455 (15) | |
H37 | 0.4290 | 1.4003 | 0.3762 | 0.055* | |
C38 | 0.5223 (4) | 1.2952 (5) | 0.3945 (3) | 0.0510 (17) | |
H38 | 0.5669 | 1.3404 | 0.3935 | 0.061* | |
C39 | 0.5388 (4) | 1.1913 (5) | 0.4064 (3) | 0.0519 (17) | |
H39 | 0.5947 | 1.1665 | 0.4137 | 0.062* | |
C40 | 0.4717 (4) | 1.1246 (5) | 0.4075 (3) | 0.0442 (15) | |
H40 | 0.4829 | 1.0550 | 0.4155 | 0.053* | |
C41 | 0.2857 (3) | 1.0908 (4) | 0.4797 (3) | 0.0364 (13) | |
C42 | 0.3190 (4) | 1.0208 (5) | 0.5277 (3) | 0.0594 (19) | |
H42 | 0.3461 | 0.9619 | 0.5174 | 0.071* | |
C43 | 0.3128 (5) | 1.0363 (7) | 0.5912 (3) | 0.080 (2) | |
H43 | 0.3354 | 0.9880 | 0.6232 | 0.096* | |
C44 | 0.2734 (5) | 1.1224 (7) | 0.6069 (3) | 0.070 (2) | |
H44 | 0.2694 | 1.1330 | 0.6496 | 0.084* | |
C45 | 0.2402 (4) | 1.1926 (6) | 0.5599 (4) | 0.063 (2) | |
H45 | 0.2134 | 1.2513 | 0.5707 | 0.076* | |
C46 | 0.2459 (4) | 1.1776 (5) | 0.4964 (3) | 0.0528 (17) | |
H46 | 0.2228 | 1.2261 | 0.4646 | 0.063* | |
B1 | 0.1798 (6) | 0.4621 (7) | 0.3609 (5) | 0.065 (2) | |
F1 | 0.1845 (3) | 0.5558 (4) | 0.3909 (2) | 0.1057 (16) | |
F2 | 0.2378 (3) | 0.4595 (5) | 0.3235 (3) | 0.132 (2) | |
F3 | 0.1016 (4) | 0.4554 (6) | 0.3221 (3) | 0.154 (3) | |
F4 | 0.1938 (4) | 0.3884 (4) | 0.4065 (3) | 0.143 (2) | |
C47 | 0.0280 (17) | 0.0044 (19) | −0.0277 (9) | 0.166 (10) | 0.50 |
Cl1 | 0.0391 (4) | 0.0809 (4) | 0.0425 (3) | 0.240 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0312 (4) | 0.0349 (4) | 0.0332 (4) | 0.0035 (3) | 0.0088 (3) | 0.0049 (3) |
P1 | 0.0281 (7) | 0.0353 (8) | 0.0294 (8) | 0.0010 (6) | 0.0095 (6) | 0.0026 (6) |
P2 | 0.0312 (7) | 0.0346 (8) | 0.0290 (8) | 0.0014 (6) | 0.0116 (6) | 0.0017 (6) |
P3 | 0.0315 (8) | 0.0365 (8) | 0.0291 (8) | 0.0030 (7) | 0.0105 (6) | 0.0005 (6) |
N1 | 0.030 (3) | 0.037 (3) | 0.032 (3) | −0.002 (2) | 0.009 (2) | 0.001 (2) |
N2 | 0.038 (3) | 0.030 (3) | 0.041 (3) | 0.003 (2) | 0.002 (2) | 0.007 (2) |
C1 | 0.029 (3) | 0.042 (4) | 0.042 (4) | 0.002 (3) | 0.005 (3) | 0.005 (3) |
C2 | 0.037 (3) | 0.031 (3) | 0.039 (4) | 0.000 (3) | 0.005 (3) | 0.007 (3) |
C3 | 0.036 (3) | 0.033 (3) | 0.029 (3) | 0.004 (3) | 0.006 (3) | 0.001 (2) |
C4 | 0.025 (3) | 0.040 (3) | 0.048 (4) | 0.001 (3) | 0.002 (3) | 0.008 (3) |
C5 | 0.038 (3) | 0.034 (3) | 0.054 (4) | −0.004 (3) | 0.010 (3) | 0.008 (3) |
C6 | 0.034 (3) | 0.030 (3) | 0.029 (3) | −0.002 (2) | 0.011 (2) | 0.001 (2) |
C7 | 0.042 (3) | 0.068 (5) | 0.037 (4) | 0.002 (3) | 0.009 (3) | 0.007 (3) |
C8 | 0.066 (5) | 0.096 (6) | 0.035 (4) | 0.007 (4) | 0.015 (3) | 0.013 (4) |
C9 | 0.061 (5) | 0.065 (5) | 0.054 (5) | −0.003 (4) | 0.033 (4) | 0.006 (4) |
C10 | 0.037 (3) | 0.062 (4) | 0.054 (5) | −0.005 (3) | 0.021 (3) | −0.006 (3) |
C11 | 0.036 (3) | 0.049 (4) | 0.035 (3) | −0.007 (3) | 0.009 (3) | −0.007 (3) |
C12 | 0.028 (3) | 0.041 (3) | 0.028 (3) | 0.002 (3) | 0.015 (2) | 0.003 (3) |
C13 | 0.039 (3) | 0.046 (4) | 0.034 (4) | 0.003 (3) | 0.003 (3) | −0.002 (3) |
C14 | 0.053 (4) | 0.060 (4) | 0.036 (4) | −0.002 (3) | 0.004 (3) | −0.002 (3) |
C15 | 0.064 (4) | 0.055 (4) | 0.048 (5) | −0.011 (4) | 0.008 (4) | −0.008 (4) |
C16 | 0.074 (5) | 0.036 (4) | 0.058 (5) | 0.003 (3) | 0.012 (4) | −0.006 (3) |
C17 | 0.047 (4) | 0.045 (4) | 0.033 (4) | 0.002 (3) | 0.002 (3) | 0.003 (3) |
C18 | 0.026 (3) | 0.046 (3) | 0.027 (3) | 0.003 (3) | 0.004 (2) | 0.006 (3) |
C19 | 0.033 (3) | 0.036 (3) | 0.024 (3) | 0.003 (2) | 0.007 (2) | 0.006 (2) |
C20 | 0.050 (4) | 0.047 (4) | 0.053 (4) | 0.016 (3) | 0.010 (3) | 0.014 (3) |
C21 | 0.047 (3) | 0.034 (3) | 0.029 (3) | −0.001 (3) | 0.013 (3) | 0.004 (3) |
C22 | 0.029 (3) | 0.040 (3) | 0.036 (3) | 0.004 (3) | 0.010 (2) | −0.004 (3) |
C23 | 0.057 (4) | 0.058 (4) | 0.035 (4) | 0.009 (3) | 0.015 (3) | −0.003 (3) |
C24 | 0.067 (5) | 0.096 (6) | 0.035 (4) | 0.017 (5) | 0.008 (3) | −0.005 (4) |
C25 | 0.054 (5) | 0.109 (7) | 0.052 (5) | −0.004 (5) | 0.012 (4) | −0.036 (5) |
C26 | 0.050 (4) | 0.068 (5) | 0.081 (6) | −0.013 (4) | 0.026 (4) | −0.032 (5) |
C27 | 0.031 (3) | 0.051 (4) | 0.047 (4) | −0.005 (3) | 0.017 (3) | −0.008 (3) |
C28 | 0.031 (3) | 0.040 (3) | 0.027 (3) | −0.004 (3) | 0.013 (2) | 0.000 (3) |
C29 | 0.037 (4) | 0.047 (4) | 0.080 (5) | −0.004 (3) | 0.014 (3) | −0.007 (4) |
C30 | 0.042 (4) | 0.069 (5) | 0.056 (4) | 0.009 (4) | 0.011 (3) | −0.007 (4) |
C31 | 0.044 (4) | 0.074 (5) | 0.040 (4) | −0.010 (4) | 0.018 (3) | −0.004 (4) |
C32 | 0.062 (5) | 0.053 (4) | 0.083 (6) | −0.014 (4) | 0.033 (4) | 0.007 (4) |
C33 | 0.049 (4) | 0.045 (4) | 0.075 (5) | 0.001 (3) | 0.032 (4) | 0.008 (3) |
C34 | 0.029 (3) | 0.035 (3) | 0.038 (3) | 0.005 (2) | 0.012 (3) | −0.003 (3) |
C35 | 0.031 (3) | 0.044 (3) | 0.026 (3) | −0.002 (3) | 0.008 (2) | −0.003 (3) |
C36 | 0.040 (3) | 0.038 (3) | 0.041 (4) | −0.001 (3) | 0.007 (3) | −0.001 (3) |
C37 | 0.054 (4) | 0.041 (4) | 0.041 (4) | −0.011 (3) | 0.012 (3) | −0.004 (3) |
C38 | 0.048 (4) | 0.066 (5) | 0.041 (4) | −0.019 (4) | 0.015 (3) | 0.000 (3) |
C39 | 0.034 (3) | 0.068 (5) | 0.055 (4) | −0.003 (3) | 0.012 (3) | 0.005 (4) |
C40 | 0.039 (3) | 0.047 (4) | 0.047 (4) | −0.001 (3) | 0.012 (3) | 0.000 (3) |
C41 | 0.036 (3) | 0.049 (4) | 0.027 (3) | −0.006 (3) | 0.013 (2) | −0.006 (3) |
C42 | 0.079 (5) | 0.065 (5) | 0.033 (4) | 0.021 (4) | 0.011 (3) | 0.004 (3) |
C43 | 0.106 (6) | 0.100 (6) | 0.033 (4) | 0.022 (5) | 0.015 (4) | 0.013 (4) |
C44 | 0.073 (5) | 0.107 (7) | 0.033 (4) | 0.010 (5) | 0.021 (4) | −0.011 (4) |
C45 | 0.065 (5) | 0.073 (5) | 0.056 (5) | 0.008 (4) | 0.023 (4) | −0.015 (4) |
C46 | 0.066 (4) | 0.059 (4) | 0.038 (4) | 0.006 (4) | 0.021 (3) | −0.005 (3) |
B1 | 0.058 (6) | 0.053 (5) | 0.085 (7) | −0.001 (5) | 0.020 (5) | 0.005 (5) |
F1 | 0.135 (4) | 0.069 (3) | 0.104 (4) | −0.017 (3) | 0.010 (3) | −0.003 (3) |
F2 | 0.110 (4) | 0.169 (5) | 0.139 (5) | 0.041 (4) | 0.073 (4) | 0.050 (4) |
F3 | 0.096 (4) | 0.221 (7) | 0.127 (5) | −0.085 (4) | −0.008 (3) | 0.004 (5) |
F4 | 0.235 (7) | 0.084 (4) | 0.135 (5) | 0.064 (4) | 0.095 (5) | 0.058 (3) |
C47 | 0.166 (10) | 0.166 (10) | 0.166 (10) | −0.0004 (10) | 0.040 (3) | −0.0001 (10) |
Cl1 | 0.241 (2) | 0.240 (2) | 0.240 (2) | −0.0006 (10) | 0.0574 (11) | −0.0037 (10) |
Cu1—N1 | 2.072 (4) | C21—H21A | 0.9700 |
Cu1—P2 | 2.3145 (19) | C21—H21B | 0.9700 |
Cu1—P3 | 2.330 (2) | C22—C27 | 1.378 (8) |
Cu1—P1 | 2.337 (2) | C22—C23 | 1.397 (8) |
P1—C12 | 1.832 (6) | C23—C24 | 1.372 (9) |
P1—C18 | 1.836 (5) | C23—H23 | 0.9300 |
P1—C6 | 1.837 (5) | C24—C25 | 1.363 (10) |
P2—C22 | 1.824 (6) | C24—H24 | 0.9300 |
P2—C28 | 1.838 (5) | C25—C26 | 1.367 (10) |
P2—C21 | 1.853 (5) | C25—H25 | 0.9300 |
P3—C41 | 1.837 (5) | C26—C27 | 1.397 (9) |
P3—C35 | 1.838 (6) | C26—H26 | 0.9300 |
P3—C34 | 1.838 (5) | C27—H27 | 0.9300 |
N1—C5 | 1.338 (6) | C28—C29 | 1.373 (7) |
N1—C1 | 1.350 (7) | C28—C33 | 1.373 (8) |
N2—N2i | 1.247 (8) | C29—C30 | 1.385 (8) |
N2—C3 | 1.442 (6) | C29—H29 | 0.9300 |
C1—C2 | 1.377 (7) | C30—C31 | 1.348 (9) |
C1—H1 | 0.9300 | C30—H30 | 0.9300 |
C2—C3 | 1.378 (7) | C31—C32 | 1.353 (9) |
C2—H2 | 0.9300 | C31—H31 | 0.9300 |
C3—C4 | 1.378 (7) | C32—C33 | 1.377 (8) |
C4—C5 | 1.375 (7) | C32—H32 | 0.9300 |
C4—H4 | 0.9300 | C33—H33 | 0.9300 |
C5—H5 | 0.9300 | C34—H34A | 0.9700 |
C6—C7 | 1.371 (8) | C34—H34B | 0.9700 |
C6—C11 | 1.384 (7) | C35—C40 | 1.387 (7) |
C7—C8 | 1.387 (8) | C35—C36 | 1.394 (7) |
C7—H7 | 0.9300 | C36—C37 | 1.372 (7) |
C8—C9 | 1.360 (9) | C36—H36 | 0.9300 |
C8—H8 | 0.9300 | C37—C38 | 1.365 (8) |
C9—C10 | 1.367 (8) | C37—H37 | 0.9300 |
C9—H9 | 0.9300 | C38—C39 | 1.386 (8) |
C10—C11 | 1.379 (8) | C38—H38 | 0.9300 |
C10—H10 | 0.9300 | C39—C40 | 1.385 (8) |
C11—H11 | 0.9300 | C39—H39 | 0.9300 |
C12—C13 | 1.381 (7) | C40—H40 | 0.9300 |
C12—C17 | 1.388 (7) | C41—C42 | 1.372 (8) |
C13—C14 | 1.373 (8) | C41—C46 | 1.381 (8) |
C13—H13 | 0.9300 | C42—C43 | 1.381 (9) |
C14—C15 | 1.359 (8) | C42—H42 | 0.9300 |
C14—H14 | 0.9300 | C43—C44 | 1.362 (10) |
C15—C16 | 1.395 (9) | C43—H43 | 0.9300 |
C15—H15 | 0.9300 | C44—C45 | 1.359 (9) |
C16—C17 | 1.373 (8) | C44—H44 | 0.9300 |
C16—H16 | 0.9300 | C45—C46 | 1.379 (8) |
C17—H17 | 0.9300 | C45—H45 | 0.9300 |
C18—C19 | 1.542 (7) | C46—H46 | 0.9300 |
C18—H18A | 0.9700 | B1—F3 | 1.327 (10) |
C18—H18B | 0.9700 | B1—F4 | 1.337 (9) |
C19—C20 | 1.536 (7) | B1—F2 | 1.356 (9) |
C19—C34 | 1.546 (7) | B1—F1 | 1.366 (10) |
C19—C21 | 1.554 (7) | C47—Cl1ii | 1.52 (2) |
C20—H20A | 0.9600 | C47—C47ii | 1.64 (4) |
C20—H20B | 0.9600 | C47—Cl1 | 1.757 (10) |
C20—H20C | 0.9600 | Cl1—C47ii | 1.52 (2) |
N1—Cu1—P2 | 127.11 (13) | H20B—C20—H20C | 109.5 |
N1—Cu1—P3 | 121.46 (13) | C19—C21—P2 | 118.6 (4) |
P2—Cu1—P3 | 91.80 (7) | C19—C21—H21A | 107.7 |
N1—Cu1—P1 | 118.74 (13) | P2—C21—H21A | 107.7 |
P2—Cu1—P1 | 93.25 (6) | C19—C21—H21B | 107.7 |
P3—Cu1—P1 | 96.85 (6) | P2—C21—H21B | 107.7 |
C12—P1—C18 | 101.0 (2) | H21A—C21—H21B | 107.1 |
C12—P1—C6 | 102.2 (2) | C27—C22—C23 | 118.0 (5) |
C18—P1—C6 | 104.8 (2) | C27—C22—P2 | 120.6 (5) |
C12—P1—Cu1 | 127.83 (17) | C23—C22—P2 | 121.4 (4) |
C18—P1—Cu1 | 104.41 (17) | C24—C23—C22 | 120.7 (7) |
C6—P1—Cu1 | 113.99 (18) | C24—C23—H23 | 119.6 |
C22—P2—C28 | 99.9 (2) | C22—C23—H23 | 119.6 |
C22—P2—C21 | 102.0 (2) | C25—C24—C23 | 120.5 (7) |
C28—P2—C21 | 104.9 (2) | C25—C24—H24 | 119.7 |
C22—P2—Cu1 | 118.28 (19) | C23—C24—H24 | 119.7 |
C28—P2—Cu1 | 124.41 (18) | C24—C25—C26 | 120.3 (7) |
C21—P2—Cu1 | 104.63 (17) | C24—C25—H25 | 119.8 |
C41—P3—C35 | 100.2 (2) | C26—C25—H25 | 119.8 |
C41—P3—C34 | 101.4 (2) | C25—C26—C27 | 119.6 (7) |
C35—P3—C34 | 104.6 (3) | C25—C26—H26 | 120.2 |
C41—P3—Cu1 | 129.4 (2) | C27—C26—H26 | 120.2 |
C35—P3—Cu1 | 114.20 (18) | C22—C27—C26 | 120.9 (6) |
C34—P3—Cu1 | 104.21 (18) | C22—C27—H27 | 119.6 |
C5—N1—C1 | 115.8 (5) | C26—C27—H27 | 119.6 |
C5—N1—Cu1 | 124.5 (4) | C29—C28—C33 | 117.8 (5) |
C1—N1—Cu1 | 119.7 (4) | C29—C28—P2 | 116.5 (4) |
N2i—N2—C3 | 114.1 (5) | C33—C28—P2 | 125.7 (4) |
N1—C1—C2 | 123.9 (5) | C28—C29—C30 | 121.4 (6) |
N1—C1—H1 | 118.0 | C28—C29—H29 | 119.3 |
C2—C1—H1 | 118.0 | C30—C29—H29 | 119.3 |
C1—C2—C3 | 118.9 (5) | C31—C30—C29 | 120.3 (6) |
C1—C2—H2 | 120.6 | C31—C30—H30 | 119.8 |
C3—C2—H2 | 120.6 | C29—C30—H30 | 119.8 |
C4—C3—C2 | 118.3 (5) | C30—C31—C32 | 118.5 (6) |
C4—C3—N2 | 117.5 (5) | C30—C31—H31 | 120.8 |
C2—C3—N2 | 124.2 (5) | C32—C31—H31 | 120.8 |
C5—C4—C3 | 119.2 (5) | C31—C32—C33 | 122.5 (6) |
C5—C4—H4 | 120.4 | C31—C32—H32 | 118.8 |
C3—C4—H4 | 120.4 | C33—C32—H32 | 118.8 |
N1—C5—C4 | 124.0 (5) | C28—C33—C32 | 119.6 (6) |
N1—C5—H5 | 118.0 | C28—C33—H33 | 120.2 |
C4—C5—H5 | 118.0 | C32—C33—H33 | 120.2 |
C7—C6—C11 | 118.0 (5) | C19—C34—P3 | 117.2 (3) |
C7—C6—P1 | 119.9 (4) | C19—C34—H34A | 108.0 |
C11—C6—P1 | 122.1 (4) | P3—C34—H34A | 108.0 |
C6—C7—C8 | 121.4 (6) | C19—C34—H34B | 108.0 |
C6—C7—H7 | 119.3 | P3—C34—H34B | 108.0 |
C8—C7—H7 | 119.3 | H34A—C34—H34B | 107.2 |
C9—C8—C7 | 119.9 (6) | C40—C35—C36 | 118.6 (5) |
C9—C8—H8 | 120.0 | C40—C35—P3 | 118.8 (4) |
C7—C8—H8 | 120.0 | C36—C35—P3 | 122.6 (4) |
C8—C9—C10 | 119.4 (6) | C37—C36—C35 | 120.0 (5) |
C8—C9—H9 | 120.3 | C37—C36—H36 | 120.0 |
C10—C9—H9 | 120.3 | C35—C36—H36 | 120.0 |
C9—C10—C11 | 121.0 (6) | C38—C37—C36 | 121.4 (6) |
C9—C10—H10 | 119.5 | C38—C37—H37 | 119.3 |
C11—C10—H10 | 119.5 | C36—C37—H37 | 119.3 |
C10—C11—C6 | 120.2 (6) | C37—C38—C39 | 119.4 (6) |
C10—C11—H11 | 119.9 | C37—C38—H38 | 120.3 |
C6—C11—H11 | 119.9 | C39—C38—H38 | 120.3 |
C13—C12—C17 | 117.5 (5) | C40—C39—C38 | 119.8 (6) |
C13—C12—P1 | 123.9 (4) | C40—C39—H39 | 120.1 |
C17—C12—P1 | 118.6 (4) | C38—C39—H39 | 120.1 |
C14—C13—C12 | 121.4 (6) | C39—C40—C35 | 120.8 (6) |
C14—C13—H13 | 119.3 | C39—C40—H40 | 119.6 |
C12—C13—H13 | 119.3 | C35—C40—H40 | 119.6 |
C15—C14—C13 | 120.8 (6) | C42—C41—C46 | 118.3 (6) |
C15—C14—H14 | 119.6 | C42—C41—P3 | 118.4 (5) |
C13—C14—H14 | 119.6 | C46—C41—P3 | 123.2 (5) |
C14—C15—C16 | 119.1 (6) | C41—C42—C43 | 121.0 (7) |
C14—C15—H15 | 120.5 | C41—C42—H42 | 119.5 |
C16—C15—H15 | 120.5 | C43—C42—H42 | 119.5 |
C17—C16—C15 | 119.9 (6) | C44—C43—C42 | 120.0 (7) |
C17—C16—H16 | 120.1 | C44—C43—H43 | 120.0 |
C15—C16—H16 | 120.1 | C42—C43—H43 | 120.0 |
C16—C17—C12 | 121.3 (5) | C45—C44—C43 | 119.8 (7) |
C16—C17—H17 | 119.3 | C45—C44—H44 | 120.1 |
C12—C17—H17 | 119.3 | C43—C44—H44 | 120.1 |
C19—C18—P1 | 120.0 (3) | C44—C45—C46 | 120.6 (7) |
C19—C18—H18A | 107.3 | C44—C45—H45 | 119.7 |
P1—C18—H18A | 107.3 | C46—C45—H45 | 119.7 |
C19—C18—H18B | 107.3 | C45—C46—C41 | 120.3 (6) |
P1—C18—H18B | 107.3 | C45—C46—H46 | 119.9 |
H18A—C18—H18B | 106.9 | C41—C46—H46 | 119.9 |
C20—C19—C18 | 107.0 (4) | F3—B1—F4 | 111.7 (8) |
C20—C19—C34 | 107.0 (4) | F3—B1—F2 | 108.5 (8) |
C18—C19—C34 | 111.6 (4) | F4—B1—F2 | 112.3 (7) |
C20—C19—C21 | 106.2 (4) | F3—B1—F1 | 106.5 (7) |
C18—C19—C21 | 112.2 (4) | F4—B1—F1 | 108.8 (8) |
C34—C19—C21 | 112.4 (4) | F2—B1—F1 | 108.8 (7) |
C19—C20—H20A | 109.5 | Cl1ii—C47—C47ii | 67.4 (16) |
C19—C20—H20B | 109.5 | Cl1ii—C47—Cl1 | 120.6 (15) |
H20A—C20—H20B | 109.5 | C47ii—C47—Cl1 | 53.2 (7) |
C19—C20—H20C | 109.5 | C47ii—Cl1—C47 | 59.4 (15) |
H20A—C20—H20C | 109.5 | ||
N1—Cu1—P1—C12 | −56.9 (3) | C6—P1—C18—C19 | 95.6 (4) |
P2—Cu1—P1—C12 | 79.1 (2) | Cu1—P1—C18—C19 | −24.5 (4) |
P3—Cu1—P1—C12 | 171.3 (2) | P1—C18—C19—C20 | −163.6 (4) |
N1—Cu1—P1—C18 | −173.6 (2) | P1—C18—C19—C34 | −46.9 (5) |
P2—Cu1—P1—C18 | −37.49 (18) | P1—C18—C19—C21 | 80.3 (5) |
P3—Cu1—P1—C18 | 54.71 (19) | C20—C19—C21—P2 | −161.6 (4) |
N1—Cu1—P1—C6 | 72.7 (2) | C18—C19—C21—P2 | −45.0 (6) |
P2—Cu1—P1—C6 | −151.23 (19) | C34—C19—C21—P2 | 81.8 (5) |
P3—Cu1—P1—C6 | −59.03 (19) | C22—P2—C21—C19 | 96.0 (4) |
N1—Cu1—P2—C22 | 78.9 (2) | C28—P2—C21—C19 | −160.1 (4) |
P3—Cu1—P2—C22 | −148.38 (19) | Cu1—P2—C21—C19 | −27.8 (4) |
P1—Cu1—P2—C22 | −51.41 (19) | C28—P2—C22—C27 | 123.2 (4) |
N1—Cu1—P2—C28 | −48.4 (3) | C21—P2—C22—C27 | −129.0 (4) |
P3—Cu1—P2—C28 | 84.3 (2) | Cu1—P2—C22—C27 | −15.0 (5) |
P1—Cu1—P2—C28 | −178.7 (2) | C28—P2—C22—C23 | −59.4 (5) |
N1—Cu1—P2—C21 | −168.5 (2) | C21—P2—C22—C23 | 48.3 (5) |
P3—Cu1—P2—C21 | −35.80 (19) | Cu1—P2—C22—C23 | 162.3 (4) |
P1—Cu1—P2—C21 | 61.17 (19) | C27—C22—C23—C24 | 0.5 (8) |
N1—Cu1—P3—C41 | −40.1 (3) | P2—C22—C23—C24 | −176.9 (5) |
P2—Cu1—P3—C41 | −176.7 (2) | C22—C23—C24—C25 | 0.5 (10) |
P1—Cu1—P3—C41 | 89.8 (2) | C23—C24—C25—C26 | −1.2 (11) |
N1—Cu1—P3—C35 | 88.2 (2) | C24—C25—C26—C27 | 0.8 (10) |
P2—Cu1—P3—C35 | −48.4 (2) | C23—C22—C27—C26 | −0.8 (8) |
P1—Cu1—P3—C35 | −141.9 (2) | P2—C22—C27—C26 | 176.6 (4) |
N1—Cu1—P3—C34 | −158.3 (2) | C25—C26—C27—C22 | 0.2 (9) |
P2—Cu1—P3—C34 | 65.10 (19) | C22—P2—C28—C29 | −71.9 (5) |
P1—Cu1—P3—C34 | −28.39 (19) | C21—P2—C28—C29 | −177.3 (4) |
P2—Cu1—N1—C5 | 47.6 (5) | Cu1—P2—C28—C29 | 62.8 (5) |
P3—Cu1—N1—C5 | −73.0 (5) | C22—P2—C28—C33 | 107.2 (6) |
P1—Cu1—N1—C5 | 167.3 (4) | C21—P2—C28—C33 | 1.8 (6) |
P2—Cu1—N1—C1 | −129.6 (4) | Cu1—P2—C28—C33 | −118.2 (5) |
P3—Cu1—N1—C1 | 109.8 (4) | C33—C28—C29—C30 | 0.8 (9) |
P1—Cu1—N1—C1 | −9.9 (4) | P2—C28—C29—C30 | 180.0 (5) |
C5—N1—C1—C2 | 0.2 (8) | C28—C29—C30—C31 | −0.6 (10) |
Cu1—N1—C1—C2 | 177.6 (4) | C29—C30—C31—C32 | 0.7 (10) |
N1—C1—C2—C3 | 0.0 (9) | C30—C31—C32—C33 | −1.0 (11) |
C1—C2—C3—C4 | −0.5 (8) | C29—C28—C33—C32 | −1.1 (9) |
C1—C2—C3—N2 | −179.5 (5) | P2—C28—C33—C32 | 179.8 (5) |
N2i—N2—C3—C4 | 164.1 (6) | C31—C32—C33—C28 | 1.3 (11) |
N2i—N2—C3—C2 | −16.9 (9) | C20—C19—C34—P3 | −156.3 (4) |
C2—C3—C4—C5 | 0.7 (8) | C18—C19—C34—P3 | 87.0 (5) |
N2—C3—C4—C5 | 179.8 (5) | C21—C19—C34—P3 | −40.2 (6) |
C1—N1—C5—C4 | 0.0 (8) | C41—P3—C34—C19 | −170.3 (4) |
Cu1—N1—C5—C4 | −177.2 (4) | C35—P3—C34—C19 | 85.8 (4) |
C3—C4—C5—N1 | −0.5 (9) | Cu1—P3—C34—C19 | −34.4 (4) |
C12—P1—C6—C7 | 134.5 (5) | C41—P3—C35—C40 | 100.6 (5) |
C18—P1—C6—C7 | −120.6 (5) | C34—P3—C35—C40 | −154.6 (4) |
Cu1—P1—C6—C7 | −7.0 (5) | Cu1—P3—C35—C40 | −41.4 (5) |
C12—P1—C6—C11 | −45.1 (5) | C41—P3—C35—C36 | −79.8 (5) |
C18—P1—C6—C11 | 59.8 (5) | C34—P3—C35—C36 | 24.9 (5) |
Cu1—P1—C6—C11 | 173.4 (4) | Cu1—P3—C35—C36 | 138.2 (4) |
C11—C6—C7—C8 | −1.3 (9) | C40—C35—C36—C37 | 0.6 (8) |
P1—C6—C7—C8 | 179.0 (5) | P3—C35—C36—C37 | −178.9 (4) |
C6—C7—C8—C9 | 1.8 (10) | C35—C36—C37—C38 | −0.3 (9) |
C7—C8—C9—C10 | −1.0 (11) | C36—C37—C38—C39 | −0.1 (9) |
C8—C9—C10—C11 | −0.2 (10) | C37—C38—C39—C40 | 0.2 (9) |
C9—C10—C11—C6 | 0.7 (9) | C38—C39—C40—C35 | 0.0 (9) |
C7—C6—C11—C10 | 0.1 (8) | C36—C35—C40—C39 | −0.5 (8) |
P1—C6—C11—C10 | 179.7 (4) | P3—C35—C40—C39 | 179.1 (5) |
C18—P1—C12—C13 | −13.3 (5) | C35—P3—C41—C42 | −103.0 (5) |
C6—P1—C12—C13 | 94.7 (5) | C34—P3—C41—C42 | 149.7 (5) |
Cu1—P1—C12—C13 | −131.4 (4) | Cu1—P3—C41—C42 | 30.3 (6) |
C18—P1—C12—C17 | 165.9 (4) | C35—P3—C41—C46 | 73.6 (5) |
C6—P1—C12—C17 | −86.2 (4) | C34—P3—C41—C46 | −33.7 (6) |
Cu1—P1—C12—C17 | 47.8 (5) | Cu1—P3—C41—C46 | −153.0 (4) |
C17—C12—C13—C14 | −1.5 (8) | C46—C41—C42—C43 | 0.1 (10) |
P1—C12—C13—C14 | 177.7 (4) | P3—C41—C42—C43 | 176.9 (6) |
C12—C13—C14—C15 | 0.3 (10) | C41—C42—C43—C44 | −0.2 (12) |
C13—C14—C15—C16 | 1.0 (10) | C42—C43—C44—C45 | 0.2 (12) |
C14—C15—C16—C17 | −1.1 (10) | C43—C44—C45—C46 | 0.0 (11) |
C15—C16—C17—C12 | −0.1 (10) | C44—C45—C46—C41 | −0.1 (10) |
C13—C12—C17—C16 | 1.4 (8) | C42—C41—C46—C45 | 0.1 (9) |
P1—C12—C17—C16 | −177.8 (5) | P3—C41—C46—C45 | −176.5 (5) |
C12—P1—C18—C19 | −158.5 (4) | Cl1ii—C47—Cl1—C47ii | 0.000 (2) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y, −z. |