Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805020878/hb6230sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805020878/hb6230Isup2.hkl |
CCDC reference: 282361
Data collection: COLLECT (Nonius, 2003); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXTL/PC (Sheldrick, 2001); program(s) used to refine structure: SHELXTL/PC; molecular graphics: SHELXTL/PC; software used to prepare material for publication: SHELXTL/PC.
[Cu(ClO4)2(C13H14N2)2] | F(000) = 2034 |
Mr = 658.96 | Dx = 1.483 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 27195 reflections |
a = 15.0179 (5) Å | θ = 2.6–27.5° |
b = 16.2881 (5) Å | µ = 0.98 mm−1 |
c = 18.5719 (7) Å | T = 150 K |
β = 102.9642 (13)° | Block, violet |
V = 4427.2 (3) Å3 | 0.10 × 0.08 × 0.06 mm |
Z = 6 |
Bruker–Nonius KappaCCD diffractometer | 7778 independent reflections |
Radiation source: fine-focus sealed tube | 5253 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.097 |
Detector resolution: 9 pixels mm-1 | θmax = 25.0°, θmin = 2.6° |
φ scans and ω scans with κ offsets | h = −17→16 |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | k = −18→19 |
Tmin = 0.689, Tmax = 0.952 | l = −21→22 |
27195 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.057 | H-atom parameters constrained |
wR(F2) = 0.159 | w = 1/[σ2(Fo2) + (0.0775P)2 + 2.2199P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max < 0.001 |
7778 reflections | Δρmax = 0.46 e Å−3 |
557 parameters | Δρmin = −0.68 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0013 (3) |
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 | ||
Cu1 | 0.5000 | 0.5000 | 0.5000 | 0.0314 (2) | |
N1 | 0.4540 (2) | 0.0473 (2) | 0.8983 (2) | 0.0321 (8) | |
N2 | 0.4481 (2) | 0.3978 (2) | 0.5369 (2) | 0.0324 (8) | |
C1 | 0.4701 (3) | 0.3228 (3) | 0.5153 (3) | 0.0403 (11) | |
H1A | 0.5220 | 0.3181 | 0.4942 | 0.048* | |
C2 | 0.4217 (3) | 0.2533 (3) | 0.5221 (2) | 0.0379 (11) | |
H2A | 0.4400 | 0.2021 | 0.5057 | 0.046* | |
C3 | 0.3459 (3) | 0.2578 (3) | 0.5530 (2) | 0.0316 (10) | |
C4 | 0.3244 (3) | 0.3343 (3) | 0.5782 (2) | 0.0371 (11) | |
H4A | 0.2745 | 0.3400 | 0.6015 | 0.045* | |
C5 | 0.3766 (3) | 0.4013 (3) | 0.5689 (2) | 0.0370 (11) | |
H5A | 0.3610 | 0.4531 | 0.5862 | 0.044* | |
C6 | 0.2912 (3) | 0.1824 (3) | 0.5625 (2) | 0.0372 (11) | |
H6A | 0.2872 | 0.1456 | 0.5194 | 0.045* | |
H6B | 0.2284 | 0.1988 | 0.5647 | 0.045* | |
C7 | 0.3358 (3) | 0.1361 (3) | 0.6335 (2) | 0.0364 (11) | |
H7A | 0.2991 | 0.0866 | 0.6380 | 0.044* | |
H7B | 0.3976 | 0.1178 | 0.6301 | 0.044* | |
C8 | 0.3433 (3) | 0.1893 (3) | 0.7025 (3) | 0.0387 (11) | |
H8A | 0.3830 | 0.2372 | 0.6997 | 0.046* | |
H8B | 0.2821 | 0.2099 | 0.7049 | 0.046* | |
C10 | 0.3824 (3) | 0.1408 (3) | 0.7704 (3) | 0.0362 (11) | |
C11 | 0.4751 (3) | 0.1266 (3) | 0.7947 (3) | 0.0397 (11) | |
H11A | 0.5166 | 0.1489 | 0.7680 | 0.048* | |
C12 | 0.5080 (3) | 0.0803 (3) | 0.8574 (3) | 0.0411 (12) | |
H12A | 0.5720 | 0.0715 | 0.8723 | 0.049* | |
C13 | 0.3634 (3) | 0.0606 (3) | 0.8745 (2) | 0.0360 (10) | |
H13A | 0.3235 | 0.0380 | 0.9025 | 0.043* | |
C14 | 0.3260 (3) | 0.1045 (3) | 0.8128 (2) | 0.0374 (11) | |
H14A | 0.2616 | 0.1108 | 0.7982 | 0.045* | |
Cl1 | 0.25978 (7) | 0.59447 (7) | 0.48949 (6) | 0.0355 (3) | |
O1 | 0.3538 (2) | 0.5841 (2) | 0.48385 (19) | 0.0439 (8) | |
O2 | 0.2196 (2) | 0.6604 (2) | 0.4430 (2) | 0.0538 (10) | |
O3 | 0.2588 (2) | 0.6122 (2) | 0.56544 (19) | 0.0487 (9) | |
O4 | 0.2109 (2) | 0.5195 (2) | 0.46686 (19) | 0.0438 (8) | |
Cu2 | 0.16100 (4) | −0.04187 (3) | 0.34533 (3) | 0.03170 (18) | |
N3 | 0.2218 (2) | −0.0767 (2) | 0.4487 (2) | 0.0321 (8) | |
N4 | 0.1974 (2) | −0.3496 (2) | 0.8087 (2) | 0.0340 (9) | |
N5 | 0.1296 (2) | 0.0692 (2) | 0.3828 (2) | 0.0354 (9) | |
N6 | 0.1042 (2) | 0.5043 (2) | 0.74131 (19) | 0.0323 (8) | |
C15 | 0.1983 (3) | −0.1458 (3) | 0.4798 (3) | 0.0374 (11) | |
H15A | 0.1465 | −0.1757 | 0.4542 | 0.045* | |
C16 | 0.2462 (3) | −0.1753 (3) | 0.5473 (3) | 0.0374 (11) | |
H16A | 0.2264 | −0.2238 | 0.5675 | 0.045* | |
C17 | 0.3231 (3) | −0.1340 (3) | 0.5854 (2) | 0.0348 (10) | |
C18 | 0.3477 (3) | −0.0626 (3) | 0.5529 (3) | 0.0388 (11) | |
H18A | 0.4000 | −0.0323 | 0.5769 | 0.047* | |
C19 | 0.2959 (3) | −0.0364 (3) | 0.4863 (3) | 0.0360 (11) | |
H19A | 0.3134 | 0.0129 | 0.4658 | 0.043* | |
C20 | 0.3792 (3) | −0.1640 (3) | 0.6581 (3) | 0.0423 (12) | |
H20A | 0.4441 | −0.1668 | 0.6552 | 0.051* | |
H20B | 0.3593 | −0.2202 | 0.6674 | 0.051* | |
C21 | 0.3707 (3) | −0.1088 (3) | 0.7226 (3) | 0.0460 (13) | |
H21A | 0.4177 | −0.1252 | 0.7667 | 0.055* | |
H21B | 0.3837 | −0.0515 | 0.7105 | 0.055* | |
C22 | 0.2773 (4) | −0.1117 (3) | 0.7417 (3) | 0.0454 (12) | |
H22A | 0.2771 | −0.0725 | 0.7825 | 0.054* | |
H22B | 0.2307 | −0.0930 | 0.6983 | 0.054* | |
C23 | 0.2502 (3) | −0.1956 (3) | 0.7646 (3) | 0.0370 (11) | |
C24 | 0.3124 (3) | −0.2475 (3) | 0.8085 (3) | 0.0424 (12) | |
H24A | 0.3746 | −0.2315 | 0.8243 | 0.051* | |
C25 | 0.2840 (3) | −0.3227 (3) | 0.8294 (3) | 0.0378 (11) | |
H25A | 0.3278 | −0.3572 | 0.8599 | 0.045* | |
C26 | 0.1369 (3) | −0.2993 (3) | 0.7663 (2) | 0.0363 (11) | |
H26A | 0.0750 | −0.3166 | 0.7515 | 0.044* | |
C27 | 0.1604 (3) | −0.2237 (3) | 0.7430 (3) | 0.0399 (11) | |
H27A | 0.1154 | −0.1905 | 0.7122 | 0.048* | |
C28 | 0.1515 (3) | 0.1382 (3) | 0.3524 (3) | 0.0405 (11) | |
H28A | 0.1919 | 0.1357 | 0.3198 | 0.049* | |
C29 | 0.1164 (3) | 0.2140 (3) | 0.3671 (3) | 0.0443 (12) | |
H29A | 0.1344 | 0.2624 | 0.3456 | 0.053* | |
C30 | 0.0557 (3) | 0.2194 (3) | 0.4130 (3) | 0.0439 (13) | |
C31 | 0.0371 (4) | 0.1471 (3) | 0.4466 (3) | 0.0524 (14) | |
H31A | −0.0014 | 0.1480 | 0.4807 | 0.063* | |
C32 | 0.0745 (3) | 0.0744 (3) | 0.4305 (3) | 0.0424 (12) | |
H32A | 0.0609 | 0.0257 | 0.4540 | 0.051* | |
C33 | 0.0127 (4) | 0.2993 (3) | 0.4273 (3) | 0.0607 (17) | |
H33A | −0.0536 | 0.2909 | 0.4226 | 0.073* | |
H33B | 0.0206 | 0.3399 | 0.3896 | 0.073* | |
C34 | 0.0547 (4) | 0.3337 (4) | 0.5044 (4) | 0.076 (2) | |
H34A | 0.0655 | 0.2877 | 0.5402 | 0.092* | |
H34B | 0.1147 | 0.3583 | 0.5037 | 0.092* | |
C35 | 0.0015 (5) | 0.3922 (6) | 0.5291 (4) | 0.096 (3) | |
H35A | −0.0580 | 0.3666 | 0.5298 | 0.116* | |
H35B | −0.0105 | 0.4368 | 0.4921 | 0.116* | |
C36 | 0.0377 (3) | 0.4305 (4) | 0.6033 (3) | 0.0546 (15) | |
C37 | −0.0107 (3) | 0.4279 (3) | 0.6587 (3) | 0.0478 (13) | |
H37A | −0.0680 | 0.4006 | 0.6501 | 0.057* | |
C38 | 0.0235 (3) | 0.4643 (3) | 0.7255 (3) | 0.0373 (11) | |
H38A | −0.0111 | 0.4614 | 0.7624 | 0.045* | |
C39 | 0.1512 (3) | 0.5085 (3) | 0.6879 (3) | 0.0387 (11) | |
H39A | 0.2074 | 0.5376 | 0.6973 | 0.046* | |
C40 | 0.1209 (3) | 0.4721 (4) | 0.6198 (3) | 0.0491 (13) | |
H40A | 0.1569 | 0.4754 | 0.5839 | 0.059* | |
Cl2 | 0.38975 (8) | 0.04822 (8) | 0.32392 (8) | 0.0498 (3) | |
O5 | 0.3017 (2) | 0.0153 (2) | 0.3222 (2) | 0.0535 (9) | |
O6 | 0.3941 (4) | 0.0843 (5) | 0.2583 (3) | 0.137 (3) | |
O7 | 0.4100 (3) | 0.1062 (3) | 0.3843 (3) | 0.0965 (17) | |
O8 | 0.4554 (3) | −0.0152 (3) | 0.3424 (3) | 0.0933 (17) | |
Cl3 | −0.07474 (8) | −0.11524 (8) | 0.33164 (7) | 0.0444 (3) | |
O9 | 0.0212 (2) | −0.1050 (2) | 0.36641 (18) | 0.0463 (9) | |
O10 | −0.0841 (3) | −0.1231 (3) | 0.2539 (2) | 0.0620 (11) | |
O11 | −0.1078 (3) | −0.1867 (3) | 0.3599 (3) | 0.0850 (15) | |
O12 | −0.1233 (3) | −0.0451 (3) | 0.3464 (3) | 0.0893 (16) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0341 (4) | 0.0340 (4) | 0.0265 (4) | −0.0067 (3) | 0.0076 (3) | −0.0030 (3) |
N1 | 0.031 (2) | 0.036 (2) | 0.0291 (19) | 0.0044 (16) | 0.0052 (16) | 0.0042 (16) |
N2 | 0.033 (2) | 0.035 (2) | 0.030 (2) | −0.0023 (16) | 0.0089 (16) | −0.0049 (16) |
C1 | 0.041 (3) | 0.042 (3) | 0.042 (3) | −0.004 (2) | 0.018 (2) | −0.004 (2) |
C2 | 0.046 (3) | 0.034 (3) | 0.036 (3) | −0.005 (2) | 0.014 (2) | −0.003 (2) |
C3 | 0.032 (2) | 0.036 (3) | 0.024 (2) | −0.0032 (19) | 0.0010 (18) | 0.0062 (19) |
C4 | 0.036 (3) | 0.045 (3) | 0.032 (2) | 0.000 (2) | 0.012 (2) | 0.007 (2) |
C5 | 0.044 (3) | 0.036 (3) | 0.031 (2) | 0.003 (2) | 0.010 (2) | 0.001 (2) |
C6 | 0.036 (3) | 0.043 (3) | 0.030 (2) | −0.006 (2) | 0.000 (2) | 0.006 (2) |
C7 | 0.034 (2) | 0.039 (3) | 0.036 (3) | −0.003 (2) | 0.007 (2) | 0.001 (2) |
C8 | 0.041 (3) | 0.037 (3) | 0.035 (3) | 0.001 (2) | 0.003 (2) | 0.004 (2) |
C10 | 0.041 (3) | 0.031 (2) | 0.034 (3) | −0.002 (2) | 0.002 (2) | 0.0003 (19) |
C11 | 0.042 (3) | 0.045 (3) | 0.033 (3) | 0.001 (2) | 0.010 (2) | 0.010 (2) |
C12 | 0.027 (2) | 0.057 (3) | 0.039 (3) | 0.004 (2) | 0.009 (2) | 0.009 (2) |
C13 | 0.035 (2) | 0.041 (3) | 0.033 (2) | −0.002 (2) | 0.008 (2) | 0.004 (2) |
C14 | 0.033 (2) | 0.045 (3) | 0.032 (3) | −0.002 (2) | 0.003 (2) | 0.006 (2) |
Cl1 | 0.0309 (6) | 0.0382 (6) | 0.0377 (6) | 0.0011 (4) | 0.0081 (5) | −0.0017 (5) |
O1 | 0.0283 (17) | 0.048 (2) | 0.057 (2) | −0.0030 (14) | 0.0131 (15) | −0.0086 (17) |
O2 | 0.054 (2) | 0.046 (2) | 0.058 (2) | 0.0109 (17) | 0.0033 (18) | 0.0079 (18) |
O3 | 0.055 (2) | 0.053 (2) | 0.040 (2) | 0.0009 (17) | 0.0126 (17) | −0.0081 (16) |
O4 | 0.0359 (18) | 0.0423 (19) | 0.054 (2) | −0.0090 (14) | 0.0115 (16) | −0.0110 (16) |
Cu2 | 0.0323 (3) | 0.0343 (3) | 0.0278 (3) | 0.0025 (2) | 0.0053 (2) | −0.0010 (2) |
N3 | 0.0312 (19) | 0.031 (2) | 0.034 (2) | −0.0008 (15) | 0.0052 (16) | −0.0016 (16) |
N4 | 0.030 (2) | 0.038 (2) | 0.032 (2) | −0.0007 (16) | 0.0031 (16) | 0.0012 (16) |
N5 | 0.036 (2) | 0.041 (2) | 0.029 (2) | 0.0025 (17) | 0.0051 (17) | −0.0003 (17) |
N6 | 0.035 (2) | 0.035 (2) | 0.0260 (19) | 0.0003 (16) | 0.0044 (16) | 0.0007 (16) |
C15 | 0.033 (2) | 0.042 (3) | 0.035 (3) | −0.003 (2) | 0.002 (2) | −0.001 (2) |
C16 | 0.041 (3) | 0.035 (3) | 0.037 (3) | −0.006 (2) | 0.012 (2) | 0.001 (2) |
C17 | 0.030 (2) | 0.042 (3) | 0.032 (3) | −0.0007 (19) | 0.0074 (19) | 0.002 (2) |
C18 | 0.036 (3) | 0.039 (3) | 0.038 (3) | −0.005 (2) | 0.001 (2) | −0.001 (2) |
C19 | 0.041 (3) | 0.029 (2) | 0.036 (2) | −0.0070 (19) | 0.002 (2) | −0.0021 (19) |
C20 | 0.039 (3) | 0.045 (3) | 0.041 (3) | −0.004 (2) | 0.003 (2) | 0.010 (2) |
C21 | 0.053 (3) | 0.040 (3) | 0.041 (3) | −0.014 (2) | 0.001 (2) | 0.004 (2) |
C22 | 0.064 (3) | 0.036 (3) | 0.036 (3) | −0.005 (2) | 0.011 (2) | −0.001 (2) |
C23 | 0.044 (3) | 0.033 (2) | 0.032 (2) | −0.004 (2) | 0.006 (2) | −0.0019 (19) |
C24 | 0.035 (3) | 0.047 (3) | 0.042 (3) | −0.004 (2) | 0.002 (2) | 0.004 (2) |
C25 | 0.033 (3) | 0.039 (3) | 0.040 (3) | 0.000 (2) | 0.006 (2) | 0.001 (2) |
C26 | 0.032 (2) | 0.045 (3) | 0.031 (2) | −0.002 (2) | 0.005 (2) | 0.001 (2) |
C27 | 0.041 (3) | 0.042 (3) | 0.037 (3) | 0.007 (2) | 0.010 (2) | 0.000 (2) |
C28 | 0.044 (3) | 0.040 (3) | 0.038 (3) | 0.005 (2) | 0.011 (2) | 0.003 (2) |
C29 | 0.054 (3) | 0.040 (3) | 0.036 (3) | 0.006 (2) | 0.002 (2) | −0.002 (2) |
C30 | 0.041 (3) | 0.048 (3) | 0.035 (3) | 0.010 (2) | −0.008 (2) | −0.011 (2) |
C31 | 0.052 (3) | 0.064 (4) | 0.045 (3) | 0.004 (3) | 0.017 (3) | −0.019 (3) |
C32 | 0.047 (3) | 0.046 (3) | 0.037 (3) | 0.000 (2) | 0.015 (2) | −0.002 (2) |
C33 | 0.053 (3) | 0.058 (4) | 0.062 (4) | 0.020 (3) | −0.006 (3) | −0.027 (3) |
C34 | 0.057 (4) | 0.086 (5) | 0.071 (4) | 0.028 (3) | −0.017 (3) | −0.047 (4) |
C35 | 0.058 (4) | 0.164 (8) | 0.058 (4) | 0.021 (4) | −0.005 (3) | −0.057 (5) |
C36 | 0.041 (3) | 0.081 (4) | 0.039 (3) | 0.010 (3) | 0.004 (2) | −0.019 (3) |
C37 | 0.036 (3) | 0.060 (3) | 0.044 (3) | −0.003 (2) | 0.002 (2) | −0.011 (3) |
C38 | 0.028 (2) | 0.048 (3) | 0.036 (3) | −0.002 (2) | 0.0062 (19) | 0.001 (2) |
C39 | 0.032 (2) | 0.050 (3) | 0.036 (3) | 0.003 (2) | 0.012 (2) | 0.006 (2) |
C40 | 0.042 (3) | 0.079 (4) | 0.027 (2) | 0.008 (3) | 0.010 (2) | −0.002 (2) |
Cl2 | 0.0356 (7) | 0.0594 (8) | 0.0562 (8) | −0.0075 (6) | 0.0143 (6) | −0.0006 (6) |
O5 | 0.0296 (18) | 0.066 (2) | 0.067 (2) | −0.0088 (16) | 0.0155 (17) | 0.001 (2) |
O6 | 0.117 (5) | 0.202 (7) | 0.094 (4) | −0.046 (5) | 0.030 (4) | 0.063 (5) |
O7 | 0.086 (3) | 0.092 (4) | 0.115 (4) | −0.026 (3) | 0.028 (3) | −0.059 (3) |
O8 | 0.043 (2) | 0.093 (3) | 0.130 (5) | 0.018 (2) | −0.009 (3) | −0.036 (3) |
Cl3 | 0.0284 (6) | 0.0581 (8) | 0.0457 (7) | −0.0030 (5) | 0.0060 (5) | 0.0029 (6) |
O9 | 0.0294 (17) | 0.065 (2) | 0.0411 (19) | −0.0048 (15) | 0.0014 (14) | −0.0009 (17) |
O10 | 0.052 (2) | 0.088 (3) | 0.043 (2) | −0.011 (2) | 0.0045 (18) | −0.009 (2) |
O11 | 0.069 (3) | 0.093 (3) | 0.096 (4) | −0.030 (2) | 0.026 (3) | 0.032 (3) |
O12 | 0.054 (3) | 0.099 (4) | 0.112 (4) | 0.030 (2) | 0.013 (3) | −0.026 (3) |
Cu1—N1i | 2.014 (3) | C16—C17 | 1.386 (6) |
Cu1—N1ii | 2.014 (3) | C16—H16A | 0.9500 |
Cu1—N2iii | 2.022 (4) | C17—C18 | 1.396 (6) |
Cu1—N2 | 2.022 (4) | C17—C20 | 1.504 (6) |
Cu1—O1 | 2.548 (3) | C18—C19 | 1.373 (6) |
Cu1—O1iii | 2.548 (3) | C18—H18A | 0.9500 |
N1—C12 | 1.341 (6) | C19—H19A | 0.9500 |
N1—C13 | 1.351 (5) | C20—C21 | 1.525 (7) |
N1—Cu1iv | 2.014 (3) | C20—H20A | 0.9900 |
N2—C5 | 1.341 (6) | C20—H20B | 0.9900 |
N2—C1 | 1.349 (6) | C21—C22 | 1.523 (7) |
C1—C2 | 1.365 (6) | C21—H21A | 0.9900 |
C1—H1A | 0.9500 | C21—H21B | 0.9900 |
C2—C3 | 1.387 (6) | C22—C23 | 1.514 (7) |
C2—H2A | 0.9500 | C22—H22A | 0.9900 |
C3—C4 | 1.395 (6) | C22—H22B | 0.9900 |
C3—C6 | 1.510 (6) | C23—C24 | 1.382 (6) |
C4—C5 | 1.378 (6) | C23—C27 | 1.394 (6) |
C4—H4A | 0.9500 | C24—C25 | 1.382 (7) |
C5—H5A | 0.9500 | C24—H24A | 0.9500 |
C6—C7 | 1.535 (6) | C25—H25A | 0.9500 |
C6—H6A | 0.9900 | C26—C27 | 1.378 (7) |
C6—H6B | 0.9900 | C26—H26A | 0.9500 |
C7—C8 | 1.530 (7) | C27—H27A | 0.9500 |
C7—H7A | 0.9900 | C28—C29 | 1.393 (7) |
C7—H7B | 0.9900 | C28—H28A | 0.9500 |
C8—C10 | 1.493 (6) | C29—C30 | 1.383 (7) |
C8—H8A | 0.9900 | C29—H29A | 0.9500 |
C8—H8B | 0.9900 | C30—C31 | 1.391 (8) |
C10—C11 | 1.383 (6) | C30—C33 | 1.502 (7) |
C10—C14 | 1.408 (7) | C31—C32 | 1.371 (7) |
C11—C12 | 1.383 (6) | C31—H31A | 0.9500 |
C11—H11A | 0.9500 | C32—H32A | 0.9500 |
C12—H12A | 0.9500 | C33—C34 | 1.535 (7) |
C13—C14 | 1.361 (6) | C33—H33A | 0.9900 |
C13—H13A | 0.9500 | C33—H33B | 0.9900 |
C14—H14A | 0.9500 | C34—C35 | 1.385 (8) |
Cl1—O2 | 1.424 (3) | C34—H34A | 0.9900 |
Cl1—O4 | 1.438 (3) | C34—H34B | 0.9900 |
Cl1—O3 | 1.443 (4) | C35—C36 | 1.499 (8) |
Cl1—O1 | 1.449 (3) | C35—H35A | 0.9900 |
Cu2—N4v | 2.014 (4) | C35—H35B | 0.9900 |
Cu2—N3 | 2.014 (4) | C36—C37 | 1.387 (8) |
Cu2—N6ii | 2.023 (3) | C36—C40 | 1.394 (8) |
Cu2—N5 | 2.031 (4) | C37—C38 | 1.368 (7) |
Cu2—O5 | 2.434 (3) | C37—H37A | 0.9500 |
Cu2—O9 | 2.447 (3) | C38—H38A | 0.9500 |
N3—C19 | 1.345 (5) | C39—C40 | 1.378 (7) |
N3—C15 | 1.348 (6) | C39—H39A | 0.9500 |
N4—C26 | 1.341 (6) | C40—H40A | 0.9500 |
N4—C25 | 1.343 (6) | Cl2—O6 | 1.368 (5) |
N4—Cu2vi | 2.014 (4) | Cl2—O8 | 1.415 (4) |
N5—C28 | 1.332 (6) | Cl2—O5 | 1.420 (3) |
N5—C32 | 1.343 (6) | Cl2—O7 | 1.445 (5) |
N6—C39 | 1.343 (6) | Cl3—O11 | 1.412 (4) |
N6—C38 | 1.348 (6) | Cl3—O12 | 1.415 (4) |
N6—Cu2vii | 2.023 (3) | Cl3—O10 | 1.426 (4) |
C15—C16 | 1.384 (6) | Cl3—O9 | 1.450 (3) |
C15—H15A | 0.9500 | ||
N1i—Cu1—N1ii | 180 | C16—C17—C18 | 117.0 (4) |
N1i—Cu1—N2iii | 85.74 (14) | C16—C17—C20 | 122.4 (4) |
N1ii—Cu1—N2iii | 94.26 (14) | C18—C17—C20 | 120.6 (4) |
N1i—Cu1—N2 | 94.26 (14) | C19—C18—C17 | 119.8 (4) |
N1ii—Cu1—N2 | 85.74 (14) | C19—C18—H18A | 120.1 |
N2iii—Cu1—N2 | 180 | C17—C18—H18A | 120.1 |
N1i—Cu1—O1 | 90.56 (13) | N3—C19—C18 | 123.4 (4) |
N1ii—Cu1—O1 | 89.44 (13) | N3—C19—H19A | 118.3 |
N2iii—Cu1—O1 | 84.55 (13) | C18—C19—H19A | 118.3 |
N2—Cu1—O1 | 95.45 (13) | C17—C20—C21 | 112.7 (4) |
O1—Cu1—O1iii | 180 | C17—C20—H20A | 109.1 |
C12—N1—C13 | 116.3 (4) | C21—C20—H20A | 109.1 |
C12—N1—Cu1iv | 124.1 (3) | C17—C20—H20B | 109.1 |
C13—N1—Cu1iv | 118.4 (3) | C21—C20—H20B | 109.1 |
C5—N2—C1 | 116.4 (4) | H20A—C20—H20B | 107.8 |
C5—N2—Cu1 | 121.5 (3) | C22—C21—C20 | 114.1 (4) |
C1—N2—Cu1 | 120.4 (3) | C22—C21—H21A | 108.7 |
N2—C1—C2 | 123.5 (5) | C20—C21—H21A | 108.7 |
N2—C1—H1A | 118.3 | C22—C21—H21B | 108.7 |
C2—C1—H1A | 118.3 | C20—C21—H21B | 108.7 |
C1—C2—C3 | 119.9 (4) | H21A—C21—H21B | 107.6 |
C1—C2—H2A | 120.1 | C23—C22—C21 | 114.4 (4) |
C3—C2—H2A | 120.1 | C23—C22—H22A | 108.7 |
C2—C3—C4 | 117.4 (4) | C21—C22—H22A | 108.7 |
C2—C3—C6 | 121.6 (4) | C23—C22—H22B | 108.7 |
C4—C3—C6 | 120.9 (4) | C21—C22—H22B | 108.7 |
C5—C4—C3 | 119.0 (4) | H22A—C22—H22B | 107.6 |
C5—C4—H4A | 120.5 | C24—C23—C27 | 116.8 (4) |
C3—C4—H4A | 120.5 | C24—C23—C22 | 121.9 (4) |
N2—C5—C4 | 123.8 (4) | C27—C23—C22 | 121.3 (4) |
N2—C5—H5A | 118.1 | C25—C24—C23 | 119.8 (4) |
C4—C5—H5A | 118.1 | C25—C24—H24A | 120.1 |
C3—C6—C7 | 110.9 (4) | C23—C24—H24A | 120.1 |
C3—C6—H6A | 109.5 | N4—C25—C24 | 123.3 (4) |
C7—C6—H6A | 109.5 | N4—C25—H25A | 118.4 |
C3—C6—H6B | 109.5 | C24—C25—H25A | 118.4 |
C7—C6—H6B | 109.5 | N4—C26—C27 | 122.8 (4) |
H6A—C6—H6B | 108.0 | N4—C26—H26A | 118.6 |
C8—C7—C6 | 112.2 (4) | C27—C26—H26A | 118.6 |
C8—C7—H7A | 109.2 | C26—C27—C23 | 120.2 (4) |
C6—C7—H7A | 109.2 | C26—C27—H27A | 119.9 |
C8—C7—H7B | 109.2 | C23—C27—H27A | 119.9 |
C6—C7—H7B | 109.2 | N5—C28—C29 | 121.6 (5) |
H7A—C7—H7B | 107.9 | N5—C28—H28A | 119.2 |
C10—C8—C7 | 110.5 (4) | C29—C28—H28A | 119.2 |
C10—C8—H8A | 109.6 | C30—C29—C28 | 120.5 (5) |
C7—C8—H8A | 109.6 | C30—C29—H29A | 119.7 |
C10—C8—H8B | 109.6 | C28—C29—H29A | 119.7 |
C7—C8—H8B | 109.6 | C29—C30—C31 | 116.7 (4) |
H8A—C8—H8B | 108.1 | C29—C30—C33 | 122.2 (5) |
C11—C10—C14 | 115.8 (4) | C31—C30—C33 | 121.1 (5) |
C11—C10—C8 | 122.6 (4) | C32—C31—C30 | 120.0 (5) |
C14—C10—C8 | 121.5 (4) | C32—C31—H31A | 120.0 |
C12—C11—C10 | 120.5 (5) | C30—C31—H31A | 120.0 |
C12—C11—H11A | 119.7 | N5—C32—C31 | 122.8 (5) |
C10—C11—H11A | 119.7 | N5—C32—H32A | 118.6 |
N1—C12—C11 | 123.3 (4) | C31—C32—H32A | 118.6 |
N1—C12—H12A | 118.4 | C30—C33—C34 | 112.3 (4) |
C11—C12—H12A | 118.4 | C30—C33—H33A | 109.1 |
N1—C13—C14 | 123.6 (4) | C34—C33—H33A | 109.1 |
N1—C13—H13A | 118.2 | C30—C33—H33B | 109.1 |
C14—C13—H13A | 118.2 | C34—C33—H33B | 109.1 |
C13—C14—C10 | 120.4 (4) | H33A—C33—H33B | 107.9 |
C13—C14—H14A | 119.8 | C35—C34—C33 | 114.4 (5) |
C10—C14—H14A | 119.8 | C35—C34—H34A | 108.7 |
O2—Cl1—O4 | 110.1 (2) | C33—C34—H34A | 108.7 |
O2—Cl1—O3 | 110.2 (2) | C35—C34—H34B | 108.7 |
O4—Cl1—O3 | 109.9 (2) | C33—C34—H34B | 108.7 |
O2—Cl1—O1 | 109.4 (2) | H34A—C34—H34B | 107.6 |
O4—Cl1—O1 | 108.8 (2) | C34—C35—C36 | 118.3 (5) |
O3—Cl1—O1 | 108.5 (2) | C34—C35—H35A | 107.7 |
Cl1—O1—Cu1 | 151.9 (2) | C36—C35—H35A | 107.7 |
N4v—Cu2—N3 | 88.58 (15) | C34—C35—H35B | 107.7 |
N4v—Cu2—N6ii | 91.80 (15) | C36—C35—H35B | 107.7 |
N3—Cu2—N6ii | 177.79 (15) | H35A—C35—H35B | 107.1 |
N4v—Cu2—N5 | 177.66 (15) | C37—C36—C40 | 116.4 (5) |
N3—Cu2—N5 | 90.81 (14) | C37—C36—C35 | 121.8 (5) |
N6ii—Cu2—N5 | 88.72 (15) | C40—C36—C35 | 121.8 (5) |
N4v—Cu2—O5 | 87.92 (14) | C38—C37—C36 | 120.5 (5) |
N3—Cu2—O5 | 92.85 (14) | C38—C37—H37A | 119.8 |
N6ii—Cu2—O5 | 84.99 (14) | C36—C37—H37A | 119.8 |
N5—Cu2—O5 | 89.85 (14) | N6—C38—C37 | 122.9 (5) |
N4v—Cu2—O9 | 89.59 (14) | N6—C38—H38A | 118.6 |
N3—Cu2—O9 | 87.21 (13) | C37—C38—H38A | 118.6 |
N6ii—Cu2—O9 | 94.97 (13) | N6—C39—C40 | 122.4 (5) |
N5—Cu2—O9 | 92.63 (14) | N6—C39—H39A | 118.8 |
O5—Cu2—O9 | 177.51 (13) | C40—C39—H39A | 118.8 |
C19—N3—C15 | 116.8 (4) | C39—C40—C36 | 120.5 (5) |
C19—N3—Cu2 | 120.2 (3) | C39—C40—H40A | 119.8 |
C15—N3—Cu2 | 122.5 (3) | C36—C40—H40A | 119.8 |
C26—N4—C25 | 117.1 (4) | O6—Cl2—O8 | 111.1 (4) |
C26—N4—Cu2vi | 122.3 (3) | O6—Cl2—O5 | 111.9 (3) |
C25—N4—Cu2vi | 120.5 (3) | O8—Cl2—O5 | 108.9 (3) |
C28—N5—C32 | 118.2 (4) | O6—Cl2—O7 | 111.5 (4) |
C28—N5—Cu2 | 120.5 (3) | O8—Cl2—O7 | 105.9 (3) |
C32—N5—Cu2 | 120.5 (3) | O5—Cl2—O7 | 107.3 (3) |
C39—N6—C38 | 117.4 (4) | Cl2—O5—Cu2 | 168.8 (3) |
C39—N6—Cu2vii | 120.8 (3) | O11—Cl3—O12 | 110.8 (3) |
C38—N6—Cu2vii | 121.3 (3) | O11—Cl3—O10 | 109.8 (3) |
N3—C15—C16 | 123.0 (4) | O12—Cl3—O10 | 109.3 (3) |
N3—C15—H15A | 118.5 | O11—Cl3—O9 | 109.1 (2) |
C16—C15—H15A | 118.5 | O12—Cl3—O9 | 108.9 (3) |
C15—C16—C17 | 119.9 (4) | O10—Cl3—O9 | 108.9 (2) |
C15—C16—H16A | 120.1 | Cl3—O9—Cu2 | 141.2 (2) |
C17—C16—H16A | 120.1 |
Symmetry codes: (i) −x+1, y+1/2, −z+3/2; (ii) x, −y+1/2, z−1/2; (iii) −x+1, −y+1, −z+1; (iv) −x+1, y−1/2, −z+3/2; (v) x, −y−1/2, z−1/2; (vi) x, −y−1/2, z+1/2; (vii) x, −y+1/2, z+1/2. |