Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806055395/ng2187sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806055395/ng2187Isup2.hkl |
CCDC reference: 636755
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CrystalMaker (CrystalMaker, 2005); software used to prepare material for publication: SHELXS97.
[Cu2(SCN)2(C13H14N2)] | F(000) = 1776 |
Mr = 883.00 | Dx = 1.734 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 23.296 (5) Å | Cell parameters from 21991 reflections |
b = 5.7045 (11) Å | θ = 1.3–28.3° |
c = 30.675 (6) Å | µ = 2.76 mm−1 |
β = 123.95 (3)° | T = 94 K |
V = 3381.4 (17) Å3 | Block, yellow |
Z = 4 | 0.30 × 0.24 × 0.20 mm |
Bruker P4 area-detector diffractometer | 8273 independent reflections |
Radiation source: fine-focus sealed tube | 4812 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.089 |
ω scans | θmax = 28.3°, θmin = 1.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −31→26 |
Tmin = 0.465, Tmax = 0.575 | k = −7→7 |
21991 measured reflections | l = −39→40 |
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)] = 0.056 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.127 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0481P)2] where P = (Fo2 + 2Fc2)/3 |
8273 reflections | (Δ/σ)max < 0.001 |
391 parameters | Δρmax = 0.70 e Å−3 |
0 restraints | Δρmin = −0.66 e Å−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 | 0.39051 (4) | 0.64606 (11) | 0.30046 (3) | 0.01809 (18) | |
Cu2 | 0.32806 (4) | 0.44795 (11) | 0.34942 (3) | 0.01749 (18) | |
Cu3 | 0.08931 (4) | 0.66330 (11) | 0.38820 (3) | 0.01785 (18) | |
Cu4 | 0.16365 (4) | 0.85323 (11) | 0.49132 (3) | 0.01868 (18) | |
S1 | 0.45180 (8) | 0.4005 (2) | 0.37313 (5) | 0.0167 (3) | |
S2 | 0.27177 (8) | 0.7006 (2) | 0.27239 (5) | 0.0152 (3) | |
S3 | 0.21612 (8) | 0.6020 (2) | 0.46098 (5) | 0.0157 (3) | |
S4 | 0.03777 (7) | 0.9131 (2) | 0.42067 (5) | 0.0150 (3) | |
N1 | 0.3877 (2) | 0.5257 (8) | 0.23780 (17) | 0.0172 (11) | |
N2 | 0.3455 (3) | 0.8479 (8) | −0.09229 (17) | 0.0178 (11) | |
N3 | 0.4322 (2) | −0.0439 (8) | 0.32660 (18) | 0.0203 (11) | |
N4 | 0.2909 (2) | 1.1536 (8) | 0.31531 (17) | 0.0159 (10) | |
N5 | 0.0969 (2) | 0.8406 (7) | 0.33508 (16) | 0.0152 (10) | |
N6 | 0.1562 (2) | 0.8246 (7) | 0.04410 (17) | 0.0157 (10) | |
N7 | 0.2003 (2) | 0.1615 (7) | 0.49495 (17) | 0.0163 (10) | |
N8 | 0.0512 (2) | 1.3587 (8) | 0.38827 (16) | 0.0157 (10) | |
C1 | 0.4210 (3) | 0.6410 (10) | 0.2200 (2) | 0.0214 (13) | |
H1 | 0.4443 | 0.7786 | 0.2369 | 0.026* | |
C2 | 0.4224 (3) | 0.5651 (9) | 0.1777 (2) | 0.0176 (13) | |
H2 | 0.4455 | 0.6532 | 0.1665 | 0.021* | |
C3 | 0.3897 (3) | 0.3594 (9) | 0.15195 (19) | 0.0134 (12) | |
C4 | 0.3546 (3) | 0.2428 (10) | 0.1696 (2) | 0.0174 (13) | |
H4 | 0.3305 | 0.1061 | 0.1529 | 0.021* | |
C5 | 0.3551 (3) | 0.3280 (9) | 0.2121 (2) | 0.0202 (13) | |
H5 | 0.3315 | 0.2438 | 0.2233 | 0.024* | |
C6 | 0.3930 (3) | 0.2621 (9) | 0.1078 (2) | 0.0163 (13) | |
H6A | 0.3585 | 0.1397 | 0.0903 | 0.020* | |
H6B | 0.4380 | 0.1904 | 0.1226 | 0.020* | |
C7 | 0.3814 (3) | 0.4421 (9) | 0.06669 (19) | 0.0156 (12) | |
H7A | 0.4137 | 0.5707 | 0.0839 | 0.019* | |
H7B | 0.3349 | 0.5049 | 0.0492 | 0.019* | |
C8 | 0.3913 (3) | 0.3311 (9) | 0.0257 (2) | 0.0196 (13) | |
H8A | 0.4385 | 0.2751 | 0.0429 | 0.024* | |
H8B | 0.3605 | 0.1977 | 0.0096 | 0.024* | |
C9 | 0.2987 (3) | 0.6921 (9) | −0.0986 (2) | 0.0152 (12) | |
H9 | 0.2544 | 0.7010 | −0.1291 | 0.018* | |
C10 | 0.3118 (3) | 0.5187 (10) | −0.0628 (2) | 0.0178 (13) | |
H10 | 0.2775 | 0.4115 | −0.0701 | 0.021* | |
C11 | 0.3765 (3) | 0.5050 (9) | −0.0160 (2) | 0.0155 (13) | |
C12 | 0.4251 (3) | 0.6683 (10) | −0.0089 (2) | 0.0238 (14) | |
H12 | 0.4694 | 0.6663 | 0.0218 | 0.029* | |
C13 | 0.4082 (3) | 0.8327 (10) | −0.0468 (2) | 0.0264 (15) | |
H13 | 0.4419 | 0.9400 | −0.0408 | 0.032* | |
C14 | 0.4405 (3) | 0.1393 (10) | 0.3458 (2) | 0.0147 (12) | |
C15 | 0.2827 (3) | 0.9684 (9) | 0.2976 (2) | 0.0143 (12) | |
C16 | 0.0707 (3) | 0.7622 (9) | 0.2858 (2) | 0.0136 (5) | |
H16 | 0.0480 | 0.6184 | 0.2758 | 0.016* | |
C17 | 0.0761 (3) | 0.8867 (9) | 0.2495 (2) | 0.0136 (5) | |
H17 | 0.0570 | 0.8255 | 0.2160 | 0.016* | |
C18 | 0.1094 (3) | 1.1012 (9) | 0.2624 (2) | 0.0136 (5) | |
C19 | 0.1377 (3) | 1.1803 (9) | 0.31378 (19) | 0.0136 (5) | |
H19 | 0.1614 | 1.3221 | 0.3248 | 0.016* | |
C20 | 0.1303 (3) | 1.0468 (9) | 0.3483 (2) | 0.0136 (5) | |
H20 | 0.1493 | 1.1032 | 0.3822 | 0.016* | |
C21 | 0.1163 (3) | 1.2471 (9) | 0.22448 (19) | 0.0138 (12) | |
H21A | 0.1576 | 1.3427 | 0.2444 | 0.017* | |
H21B | 0.0769 | 1.3521 | 0.2059 | 0.017* | |
C22 | 0.1204 (3) | 1.1021 (9) | 0.18349 (19) | 0.0135 (12) | |
H22A | 0.1488 | 0.9644 | 0.2004 | 0.016* | |
H22B | 0.0743 | 1.0495 | 0.1560 | 0.016* | |
C23 | 0.1508 (3) | 1.2443 (9) | 0.1590 (2) | 0.0156 (12) | |
H23A | 0.1228 | 1.3832 | 0.1424 | 0.019* | |
H23B | 0.1972 | 1.2946 | 0.1863 | 0.019* | |
C24 | 0.1977 (3) | 0.7780 (9) | 0.0957 (2) | 0.0187 (13) | |
H24 | 0.2277 | 0.6510 | 0.1066 | 0.022* | |
C25 | 0.1977 (3) | 0.9109 (9) | 0.1334 (2) | 0.0171 (12) | |
H25 | 0.2275 | 0.8722 | 0.1687 | 0.021* | |
C26 | 0.1534 (3) | 1.1027 (9) | 0.1188 (2) | 0.0161 (12) | |
C27 | 0.1106 (3) | 1.1487 (9) | 0.0654 (2) | 0.0167 (12) | |
H27 | 0.0796 | 1.2733 | 0.0534 | 0.020* | |
C28 | 0.1140 (3) | 1.0091 (9) | 0.0303 (2) | 0.0195 (13) | |
H28 | 0.0852 | 1.0456 | −0.0053 | 0.023* | |
C29 | 0.2065 (3) | 0.3428 (9) | 0.48130 (19) | 0.0136 (12) | |
C30 | 0.0457 (3) | 1.1773 (9) | 0.40196 (19) | 0.0123 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0290 (4) | 0.0112 (3) | 0.0190 (4) | 0.0008 (3) | 0.0164 (4) | −0.0012 (3) |
Cu2 | 0.0264 (4) | 0.0098 (3) | 0.0166 (4) | −0.0002 (3) | 0.0122 (4) | −0.0022 (3) |
Cu3 | 0.0269 (4) | 0.0117 (3) | 0.0188 (4) | 0.0003 (3) | 0.0152 (4) | 0.0038 (3) |
Cu4 | 0.0283 (4) | 0.0115 (3) | 0.0196 (4) | −0.0006 (3) | 0.0155 (4) | 0.0032 (3) |
S1 | 0.0181 (8) | 0.0113 (7) | 0.0171 (8) | −0.0010 (6) | 0.0076 (7) | −0.0013 (6) |
S2 | 0.0201 (8) | 0.0095 (7) | 0.0132 (7) | −0.0002 (6) | 0.0075 (7) | −0.0017 (5) |
S3 | 0.0192 (8) | 0.0105 (7) | 0.0204 (8) | −0.0001 (6) | 0.0129 (7) | 0.0026 (6) |
S4 | 0.0178 (8) | 0.0102 (7) | 0.0187 (8) | −0.0014 (6) | 0.0112 (7) | 0.0009 (6) |
N1 | 0.022 (3) | 0.016 (2) | 0.015 (3) | −0.001 (2) | 0.010 (2) | −0.001 (2) |
N2 | 0.025 (3) | 0.014 (2) | 0.017 (3) | 0.000 (2) | 0.013 (2) | −0.002 (2) |
N3 | 0.018 (3) | 0.016 (3) | 0.028 (3) | −0.002 (2) | 0.013 (3) | 0.001 (2) |
N4 | 0.017 (3) | 0.012 (2) | 0.021 (3) | 0.000 (2) | 0.012 (2) | −0.001 (2) |
N5 | 0.016 (3) | 0.014 (2) | 0.014 (2) | 0.002 (2) | 0.008 (2) | 0.0049 (19) |
N6 | 0.019 (3) | 0.016 (2) | 0.017 (3) | 0.000 (2) | 0.013 (2) | −0.001 (2) |
N7 | 0.019 (3) | 0.008 (2) | 0.020 (3) | 0.000 (2) | 0.010 (2) | 0.002 (2) |
N8 | 0.024 (3) | 0.014 (2) | 0.010 (2) | 0.003 (2) | 0.011 (2) | 0.0039 (19) |
C1 | 0.028 (4) | 0.013 (3) | 0.027 (3) | −0.005 (3) | 0.018 (3) | 0.000 (3) |
C2 | 0.024 (3) | 0.017 (3) | 0.017 (3) | −0.004 (3) | 0.014 (3) | −0.001 (2) |
C3 | 0.013 (3) | 0.015 (3) | 0.009 (3) | 0.008 (2) | 0.004 (2) | 0.005 (2) |
C4 | 0.021 (3) | 0.015 (3) | 0.021 (3) | −0.004 (3) | 0.014 (3) | −0.002 (2) |
C5 | 0.029 (4) | 0.016 (3) | 0.026 (3) | −0.007 (3) | 0.021 (3) | 0.001 (3) |
C6 | 0.021 (3) | 0.015 (3) | 0.016 (3) | 0.003 (3) | 0.013 (3) | −0.003 (2) |
C7 | 0.023 (3) | 0.014 (3) | 0.011 (3) | 0.001 (3) | 0.010 (3) | 0.002 (2) |
C8 | 0.024 (3) | 0.016 (3) | 0.020 (3) | 0.000 (3) | 0.013 (3) | −0.002 (2) |
C9 | 0.016 (3) | 0.017 (3) | 0.012 (3) | 0.005 (2) | 0.008 (3) | 0.004 (2) |
C10 | 0.021 (3) | 0.019 (3) | 0.020 (3) | 0.000 (3) | 0.015 (3) | 0.000 (2) |
C11 | 0.025 (3) | 0.014 (3) | 0.015 (3) | 0.005 (3) | 0.016 (3) | 0.001 (2) |
C12 | 0.029 (4) | 0.027 (3) | 0.008 (3) | −0.006 (3) | 0.005 (3) | 0.003 (3) |
C13 | 0.024 (4) | 0.030 (4) | 0.014 (3) | −0.011 (3) | 0.004 (3) | −0.005 (3) |
C14 | 0.013 (3) | 0.014 (3) | 0.018 (3) | 0.003 (2) | 0.009 (3) | 0.004 (2) |
C15 | 0.016 (3) | 0.013 (3) | 0.013 (3) | 0.003 (2) | 0.008 (3) | 0.006 (2) |
C16 | 0.0136 (13) | 0.0133 (13) | 0.0144 (13) | 0.0036 (11) | 0.0081 (12) | 0.0009 (10) |
C17 | 0.0136 (13) | 0.0133 (13) | 0.0144 (13) | 0.0036 (11) | 0.0081 (12) | 0.0009 (10) |
C18 | 0.0136 (13) | 0.0133 (13) | 0.0144 (13) | 0.0036 (11) | 0.0081 (12) | 0.0009 (10) |
C19 | 0.0136 (13) | 0.0133 (13) | 0.0144 (13) | 0.0036 (11) | 0.0081 (12) | 0.0009 (10) |
C20 | 0.0136 (13) | 0.0133 (13) | 0.0144 (13) | 0.0036 (11) | 0.0081 (12) | 0.0009 (10) |
C21 | 0.015 (3) | 0.013 (3) | 0.013 (3) | −0.005 (2) | 0.007 (3) | −0.002 (2) |
C22 | 0.015 (3) | 0.011 (3) | 0.014 (3) | −0.001 (2) | 0.008 (3) | −0.001 (2) |
C23 | 0.023 (3) | 0.013 (3) | 0.016 (3) | −0.005 (3) | 0.014 (3) | −0.004 (2) |
C24 | 0.030 (4) | 0.013 (3) | 0.020 (3) | 0.002 (3) | 0.018 (3) | 0.001 (2) |
C25 | 0.015 (3) | 0.020 (3) | 0.013 (3) | 0.000 (3) | 0.006 (3) | 0.004 (2) |
C26 | 0.021 (3) | 0.015 (3) | 0.019 (3) | −0.006 (3) | 0.015 (3) | 0.000 (2) |
C27 | 0.021 (3) | 0.012 (3) | 0.016 (3) | 0.001 (3) | 0.010 (3) | 0.005 (2) |
C28 | 0.022 (3) | 0.021 (3) | 0.014 (3) | 0.000 (3) | 0.010 (3) | 0.000 (2) |
C29 | 0.011 (3) | 0.016 (3) | 0.009 (3) | 0.000 (2) | 0.002 (2) | −0.003 (2) |
C30 | 0.014 (3) | 0.012 (3) | 0.009 (3) | 0.002 (2) | 0.005 (2) | −0.001 (2) |
Cu1—N3i | 1.961 (5) | C6—C7 | 1.528 (7) |
Cu1—N1 | 2.008 (4) | C6—H6A | 0.9700 |
Cu1—S1 | 2.3272 (17) | C6—H6B | 0.9700 |
Cu1—S2 | 2.4142 (18) | C7—C8 | 1.537 (7) |
Cu1—Cu2 | 2.8441 (11) | C7—H7A | 0.9700 |
Cu2—N4ii | 1.911 (5) | C7—H7B | 0.9700 |
Cu2—N2iii | 1.977 (4) | C8—C11 | 1.498 (7) |
Cu2—S2 | 2.4329 (16) | C8—H8A | 0.9700 |
Cu2—S1 | 2.5630 (18) | C8—H8B | 0.9700 |
Cu3—N8ii | 1.952 (5) | C9—C10 | 1.379 (7) |
Cu3—N5 | 2.008 (4) | C9—H9 | 0.9300 |
Cu3—S4 | 2.4080 (16) | C10—C11 | 1.386 (7) |
Cu3—S3 | 2.543 (2) | C10—H10 | 0.9300 |
Cu3—Cu4 | 2.8390 (13) | C11—C12 | 1.387 (8) |
Cu4—N7i | 1.931 (4) | C12—C13 | 1.370 (7) |
Cu4—N6iii | 1.999 (4) | C12—H12 | 0.9300 |
Cu4—S3 | 2.3844 (16) | C13—H13 | 0.9300 |
Cu4—S4 | 2.513 (2) | C16—C17 | 1.384 (7) |
S1—C14 | 1.657 (6) | C16—H16 | 0.9300 |
S2—C15 | 1.666 (6) | C17—C18 | 1.383 (7) |
S3—C29 | 1.668 (6) | C17—H17 | 0.9300 |
S4—C30 | 1.660 (5) | C18—C19 | 1.400 (7) |
N1—C5 | 1.343 (7) | C18—C21 | 1.510 (7) |
N1—C1 | 1.344 (7) | C19—C20 | 1.391 (7) |
N2—C9 | 1.333 (7) | C19—H19 | 0.9300 |
N2—C13 | 1.345 (7) | C20—H20 | 0.9300 |
N3—C14 | 1.162 (6) | C21—C22 | 1.552 (7) |
N4—C15 | 1.154 (6) | C21—H21A | 0.9700 |
N5—C20 | 1.341 (6) | C21—H21B | 0.9700 |
N5—C16 | 1.352 (6) | C22—C23 | 1.524 (7) |
N6—C28 | 1.338 (7) | C22—H22A | 0.9700 |
N6—C24 | 1.342 (6) | C22—H22B | 0.9700 |
N7—C29 | 1.155 (6) | C23—C26 | 1.502 (7) |
N8—C30 | 1.150 (6) | C23—H23A | 0.9700 |
C1—C2 | 1.386 (7) | C23—H23B | 0.9700 |
C1—H1 | 0.9300 | C24—C25 | 1.382 (7) |
C2—C3 | 1.382 (7) | C24—H24 | 0.9300 |
C2—H2 | 0.9300 | C25—C26 | 1.395 (7) |
C3—C4 | 1.378 (7) | C25—H25 | 0.9300 |
C3—C6 | 1.506 (7) | C26—C27 | 1.385 (7) |
C4—C5 | 1.385 (7) | C27—C28 | 1.378 (7) |
C4—H4 | 0.9300 | C27—H27 | 0.9300 |
C5—H5 | 0.9300 | C28—H28 | 0.9300 |
N3i—Cu1—N1 | 116.35 (19) | C3—C6—H6A | 108.6 |
N3i—Cu1—S1 | 104.63 (14) | C7—C6—H6A | 108.6 |
N1—Cu1—S1 | 112.68 (14) | C3—C6—H6B | 108.6 |
N3i—Cu1—S2 | 103.68 (14) | C7—C6—H6B | 108.6 |
N1—Cu1—S2 | 106.55 (15) | H6A—C6—H6B | 107.5 |
S1—Cu1—S2 | 112.77 (6) | C6—C7—C8 | 111.1 (4) |
N3i—Cu1—Cu2 | 115.15 (14) | C6—C7—H7A | 109.4 |
N1—Cu1—Cu2 | 128.11 (14) | C8—C7—H7A | 109.4 |
S1—Cu1—Cu2 | 58.40 (4) | C6—C7—H7B | 109.4 |
S2—Cu1—Cu2 | 54.38 (4) | C8—C7—H7B | 109.4 |
N4ii—Cu2—N2iii | 144.51 (19) | H7A—C7—H7B | 108.0 |
N4ii—Cu2—S2 | 98.93 (14) | C11—C8—C7 | 110.9 (4) |
N2iii—Cu2—S2 | 104.87 (14) | C11—C8—H8A | 109.5 |
N4ii—Cu2—S1 | 98.99 (14) | C7—C8—H8A | 109.5 |
N2iii—Cu2—S1 | 100.10 (15) | C11—C8—H8B | 109.5 |
S2—Cu2—S1 | 104.42 (6) | C7—C8—H8B | 109.5 |
N4ii—Cu2—Cu1 | 105.60 (13) | H8A—C8—H8B | 108.0 |
N2iii—Cu2—Cu1 | 109.66 (13) | N2—C9—C10 | 124.2 (5) |
S2—Cu2—Cu1 | 53.77 (4) | N2—C9—H9 | 117.9 |
S1—Cu2—Cu1 | 50.66 (4) | C10—C9—H9 | 117.9 |
N8ii—Cu3—N5 | 134.07 (18) | C9—C10—C11 | 119.7 (5) |
N8ii—Cu3—S4 | 101.20 (13) | C9—C10—H10 | 120.2 |
N5—Cu3—S4 | 109.15 (13) | C11—C10—H10 | 120.2 |
N8ii—Cu3—S3 | 100.54 (14) | C10—C11—C12 | 116.4 (5) |
N5—Cu3—S3 | 101.28 (14) | C10—C11—C8 | 121.4 (5) |
S4—Cu3—S3 | 108.75 (5) | C12—C11—C8 | 122.1 (5) |
N8ii—Cu3—Cu4 | 109.48 (12) | C13—C12—C11 | 120.2 (6) |
N5—Cu3—Cu4 | 115.88 (13) | C13—C12—H12 | 119.9 |
S4—Cu3—Cu4 | 56.51 (4) | C11—C12—H12 | 119.9 |
S3—Cu3—Cu4 | 52.24 (4) | N2—C13—C12 | 123.8 (6) |
N7i—Cu4—N6iii | 130.64 (18) | N2—C13—H13 | 118.1 |
N7i—Cu4—S3 | 105.26 (14) | C12—C13—H13 | 118.1 |
N6iii—Cu4—S3 | 107.87 (13) | N3—C14—S1 | 179.6 (5) |
N7i—Cu4—S4 | 101.04 (14) | N4—C15—S2 | 179.4 (7) |
N6iii—Cu4—S4 | 100.37 (14) | N5—C16—C17 | 122.8 (5) |
S3—Cu4—S4 | 110.53 (5) | N5—C16—H16 | 118.6 |
N7i—Cu4—Cu3 | 112.75 (13) | C17—C16—H16 | 118.6 |
N6iii—Cu4—Cu3 | 115.72 (14) | C18—C17—C16 | 120.8 (5) |
S3—Cu4—Cu3 | 57.48 (4) | C18—C17—H17 | 119.6 |
S4—Cu4—Cu3 | 53.06 (4) | C16—C17—H17 | 119.6 |
C14—S1—Cu1 | 102.55 (19) | C17—C18—C19 | 116.3 (5) |
C14—S1—Cu2 | 96.6 (2) | C17—C18—C21 | 123.4 (5) |
Cu1—S1—Cu2 | 70.94 (5) | C19—C18—C21 | 120.3 (5) |
C15—S2—Cu1 | 96.0 (2) | C20—C19—C18 | 120.0 (5) |
C15—S2—Cu2 | 103.48 (18) | C20—C19—H19 | 120.0 |
Cu1—S2—Cu2 | 71.85 (5) | C18—C19—H19 | 120.0 |
C29—S3—Cu4 | 100.47 (19) | N5—C20—C19 | 123.1 (5) |
C29—S3—Cu3 | 96.73 (19) | N5—C20—H20 | 118.4 |
Cu4—S3—Cu3 | 70.28 (5) | C19—C20—H20 | 118.4 |
C30—S4—Cu3 | 102.50 (19) | C18—C21—C22 | 114.3 (4) |
C30—S4—Cu4 | 96.9 (2) | C18—C21—H21A | 108.7 |
Cu3—S4—Cu4 | 70.43 (5) | C22—C21—H21A | 108.7 |
C5—N1—C1 | 116.0 (5) | C18—C21—H21B | 108.7 |
C5—N1—Cu1 | 123.7 (4) | C22—C21—H21B | 108.7 |
C1—N1—Cu1 | 120.3 (4) | H21A—C21—H21B | 107.6 |
C9—N2—C13 | 115.7 (5) | C23—C22—C21 | 111.9 (4) |
C9—N2—Cu2iv | 121.5 (4) | C23—C22—H22A | 109.2 |
C13—N2—Cu2iv | 122.1 (4) | C21—C22—H22A | 109.2 |
C14—N3—Cu1ii | 157.4 (5) | C23—C22—H22B | 109.2 |
C15—N4—Cu2i | 165.3 (5) | C21—C22—H22B | 109.2 |
C20—N5—C16 | 116.9 (4) | H22A—C22—H22B | 107.9 |
C20—N5—Cu3 | 119.6 (3) | C26—C23—C22 | 111.2 (4) |
C16—N5—Cu3 | 123.4 (4) | C26—C23—H23A | 109.4 |
C28—N6—C24 | 116.6 (4) | C22—C23—H23A | 109.4 |
C28—N6—Cu4iv | 121.6 (4) | C26—C23—H23B | 109.4 |
C24—N6—Cu4iv | 121.6 (4) | C22—C23—H23B | 109.4 |
C29—N7—Cu4ii | 159.3 (4) | H23A—C23—H23B | 108.0 |
C30—N8—Cu3i | 160.8 (5) | N6—C24—C25 | 122.8 (5) |
N1—C1—C2 | 123.3 (5) | N6—C24—H24 | 118.6 |
N1—C1—H1 | 118.3 | C25—C24—H24 | 118.6 |
C2—C1—H1 | 118.3 | C24—C25—C26 | 120.5 (5) |
C3—C2—C1 | 120.4 (5) | C24—C25—H25 | 119.8 |
C3—C2—H2 | 119.8 | C26—C25—H25 | 119.8 |
C1—C2—H2 | 119.8 | C27—C26—C25 | 116.3 (5) |
C4—C3—C2 | 116.4 (5) | C27—C26—C23 | 122.4 (5) |
C4—C3—C6 | 121.0 (5) | C25—C26—C23 | 121.3 (5) |
C2—C3—C6 | 122.5 (5) | C28—C27—C26 | 119.8 (5) |
C3—C4—C5 | 120.4 (5) | C28—C27—H27 | 120.1 |
C3—C4—H4 | 119.8 | C26—C27—H27 | 120.1 |
C5—C4—H4 | 119.8 | N6—C28—C27 | 124.1 (5) |
N1—C5—C4 | 123.5 (5) | N6—C28—H28 | 118.0 |
N1—C5—H5 | 118.3 | C27—C28—H28 | 118.0 |
C4—C5—H5 | 118.3 | N7—C29—S3 | 178.8 (5) |
C3—C6—C7 | 114.8 (4) | N8—C30—S4 | 178.8 (5) |
N3i—Cu1—Cu2—N4ii | 178.9 (2) | S3—Cu3—S4—Cu4 | 0.75 (5) |
N1—Cu1—Cu2—N4ii | 6.4 (2) | N7i—Cu4—S4—C30 | 9.4 (2) |
S1—Cu1—Cu2—N4ii | −88.90 (15) | N6iii—Cu4—S4—C30 | 144.6 (2) |
S2—Cu1—Cu2—N4ii | 89.73 (15) | S3—Cu4—S4—C30 | −101.67 (18) |
N3i—Cu1—Cu2—N2iii | −5.2 (2) | Cu3—Cu4—S4—C30 | −100.87 (18) |
N1—Cu1—Cu2—N2iii | −177.7 (2) | N7i—Cu4—S4—Cu3 | 110.26 (14) |
S1—Cu1—Cu2—N2iii | 87.01 (16) | N6iii—Cu4—S4—Cu3 | −114.48 (13) |
S2—Cu1—Cu2—N2iii | −94.36 (16) | S3—Cu4—S4—Cu3 | −0.80 (5) |
N3i—Cu1—Cu2—S2 | 89.15 (16) | N3i—Cu1—N1—C5 | −173.2 (4) |
N1—Cu1—Cu2—S2 | −83.30 (18) | S1—Cu1—N1—C5 | 65.9 (5) |
S1—Cu1—Cu2—S2 | −178.63 (6) | S2—Cu1—N1—C5 | −58.2 (5) |
N3i—Cu1—Cu2—S1 | −92.23 (16) | Cu2—Cu1—N1—C5 | −0.9 (5) |
N1—Cu1—Cu2—S1 | 95.33 (18) | N3i—Cu1—N1—C1 | 8.3 (5) |
S2—Cu1—Cu2—S1 | 178.63 (6) | S1—Cu1—N1—C1 | −112.5 (4) |
N8ii—Cu3—Cu4—N7i | −177.6 (2) | S2—Cu1—N1—C1 | 123.3 (4) |
N5—Cu3—Cu4—N7i | 9.9 (2) | Cu2—Cu1—N1—C1 | −179.3 (4) |
S4—Cu3—Cu4—N7i | −86.81 (16) | N8ii—Cu3—N5—C20 | −176.3 (4) |
S3—Cu3—Cu4—N7i | 94.08 (16) | S4—Cu3—N5—C20 | 55.2 (4) |
N8ii—Cu3—Cu4—N6iii | −7.2 (2) | S3—Cu3—N5—C20 | −59.4 (4) |
N5—Cu3—Cu4—N6iii | −179.8 (2) | Cu4—Cu3—N5—C20 | −6.1 (4) |
S4—Cu3—Cu4—N6iii | 83.55 (15) | N8ii—Cu3—N5—C16 | 2.9 (6) |
S3—Cu3—Cu4—N6iii | −95.56 (15) | S4—Cu3—N5—C16 | −125.6 (4) |
N8ii—Cu3—Cu4—S3 | 88.36 (15) | S3—Cu3—N5—C16 | 119.8 (4) |
N5—Cu3—Cu4—S3 | −84.22 (15) | Cu4—Cu3—N5—C16 | 173.1 (4) |
S4—Cu3—Cu4—S3 | 179.11 (6) | C5—N1—C1—C2 | 0.1 (9) |
N8ii—Cu3—Cu4—S4 | −90.75 (15) | Cu1—N1—C1—C2 | 178.6 (4) |
N5—Cu3—Cu4—S4 | 96.68 (15) | N1—C1—C2—C3 | −1.2 (9) |
S3—Cu3—Cu4—S4 | −179.11 (6) | C1—C2—C3—C4 | 2.1 (8) |
N3i—Cu1—S1—C14 | −156.4 (2) | C1—C2—C3—C6 | −176.5 (5) |
N1—Cu1—S1—C14 | −29.1 (3) | C2—C3—C4—C5 | −2.0 (8) |
S2—Cu1—S1—C14 | 91.5 (2) | C6—C3—C4—C5 | 176.6 (5) |
Cu2—Cu1—S1—C14 | 92.8 (2) | C1—N1—C5—C4 | 0.0 (9) |
N3i—Cu1—S1—Cu2 | 110.80 (15) | Cu1—N1—C5—C4 | −178.5 (4) |
N1—Cu1—S1—Cu2 | −121.89 (15) | C3—C4—C5—N1 | 1.0 (9) |
S2—Cu1—S1—Cu2 | −1.21 (5) | C4—C3—C6—C7 | 136.2 (5) |
N4ii—Cu2—S1—C14 | 1.8 (2) | C2—C3—C6—C7 | −45.3 (8) |
N2iii—Cu2—S1—C14 | 151.8 (2) | C3—C6—C7—C8 | 175.6 (5) |
S2—Cu2—S1—C14 | −99.89 (19) | C6—C7—C8—C11 | 177.2 (5) |
Cu1—Cu2—S1—C14 | −101.03 (19) | C13—N2—C9—C10 | −2.0 (8) |
N4ii—Cu2—S1—Cu1 | 102.85 (14) | Cu2iv—N2—C9—C10 | 168.5 (4) |
N2iii—Cu2—S1—Cu1 | −107.21 (13) | N2—C9—C10—C11 | 2.4 (8) |
S2—Cu2—S1—Cu1 | 1.14 (5) | C9—C10—C11—C12 | −1.4 (8) |
N3i—Cu1—S2—C15 | −9.1 (2) | C9—C10—C11—C8 | 175.4 (5) |
N1—Cu1—S2—C15 | −132.4 (2) | C7—C8—C11—C10 | −94.8 (6) |
S1—Cu1—S2—C15 | 103.52 (18) | C7—C8—C11—C12 | 81.8 (7) |
Cu2—Cu1—S2—C15 | 102.25 (18) | C10—C11—C12—C13 | 0.4 (8) |
N3i—Cu1—S2—Cu2 | −111.32 (14) | C8—C11—C12—C13 | −176.3 (5) |
N1—Cu1—S2—Cu2 | 125.39 (14) | C9—N2—C13—C12 | 0.9 (8) |
S1—Cu1—S2—Cu2 | 1.27 (6) | Cu2iv—N2—C13—C12 | −169.6 (5) |
N4ii—Cu2—S2—C15 | 165.2 (2) | C11—C12—C13—N2 | −0.1 (9) |
N2iii—Cu2—S2—C15 | 11.7 (3) | C20—N5—C16—C17 | −1.1 (8) |
S1—Cu2—S2—C15 | −93.1 (2) | Cu3—N5—C16—C17 | 179.7 (4) |
Cu1—Cu2—S2—C15 | −92.0 (2) | N5—C16—C17—C18 | 0.2 (8) |
N4ii—Cu2—S2—Cu1 | −102.85 (14) | C16—C17—C18—C19 | 0.9 (8) |
N2iii—Cu2—S2—Cu1 | 103.71 (15) | C16—C17—C18—C21 | −179.2 (5) |
S1—Cu2—S2—Cu1 | −1.10 (5) | C17—C18—C19—C20 | −1.1 (8) |
N7i—Cu4—S3—C29 | 159.0 (2) | C21—C18—C19—C20 | 179.0 (5) |
N6iii—Cu4—S3—C29 | 16.1 (2) | C16—N5—C20—C19 | 0.9 (8) |
S4—Cu4—S3—C29 | −92.70 (19) | Cu3—N5—C20—C19 | −179.9 (4) |
Cu3—Cu4—S3—C29 | −93.46 (19) | C18—C19—C20—N5 | 0.2 (8) |
N7i—Cu4—S3—Cu3 | −107.55 (14) | C17—C18—C21—C22 | −31.1 (7) |
N6iii—Cu4—S3—Cu3 | 109.58 (15) | C19—C18—C21—C22 | 148.7 (5) |
S4—Cu4—S3—Cu3 | 0.76 (5) | C18—C21—C22—C23 | −160.9 (5) |
N8ii—Cu3—S3—C29 | −7.8 (2) | C21—C22—C23—C26 | −179.1 (5) |
N5—Cu3—S3—C29 | −147.1 (2) | C28—N6—C24—C25 | 0.2 (8) |
S4—Cu3—S3—C29 | 97.96 (18) | Cu4iv—N6—C24—C25 | 174.3 (4) |
Cu4—Cu3—S3—C29 | 98.75 (18) | N6—C24—C25—C26 | 0.1 (9) |
N8ii—Cu3—S3—Cu4 | −106.56 (13) | C24—C25—C26—C27 | 0.1 (8) |
N5—Cu3—S3—Cu4 | 114.11 (13) | C24—C25—C26—C23 | 177.8 (5) |
S4—Cu3—S3—Cu4 | −0.79 (5) | C22—C23—C26—C27 | 109.6 (6) |
N8ii—Cu3—S4—C30 | −161.0 (2) | C22—C23—C26—C25 | −68.0 (7) |
N5—Cu3—S4—C30 | −16.0 (2) | C25—C26—C27—C28 | −0.7 (8) |
S3—Cu3—S4—C30 | 93.7 (2) | C23—C26—C27—C28 | −178.3 (5) |
Cu4—Cu3—S4—C30 | 92.9 (2) | C24—N6—C28—C27 | −0.7 (8) |
N8ii—Cu3—S4—Cu4 | 106.06 (13) | Cu4iv—N6—C28—C27 | −174.9 (4) |
N5—Cu3—S4—Cu4 | −108.92 (14) | C26—C27—C28—N6 | 1.0 (9) |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z; (iii) x, −y+3/2, z+1/2; (iv) x, −y+3/2, z−1/2. |