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
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.007 Å
- R factor = 0.057
- wR factor = 0.159
- Data-to-parameter ratio = 14.0
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C35 PLAT411_ALERT_2_B Short Inter H...H Contact H35B .. H35B .. 2.09 Ang.
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.689 0.952 Tmin(prime) and Tmax expected: 0.905 0.943 RR(prime) = 0.754 Please check that your absorption correction is appropriate. PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.75 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.78 Ratio PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.96 Ratio PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C34 - C35 ... 1.39 Ang.
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
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. |