Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229615011298/yo3008sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229615011298/yo3008Isup2.hkl | |
Microsoft Word (DOC) file https://doi.org/10.1107/S2053229615011298/yo3008Isup3.doc | |
Microsoft Word (DOC) file https://doi.org/10.1107/S2053229615011298/yo3008sup1.doc |
CCDC reference: 1405920
Data collection: CrystalClear (Rigaku, 2005); cell refinement: CrystalClear (Rigaku, 2005); data reduction: CrystalClear (Rigaku, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).
(C9H13N2O2)[Cd(NCS)3][Cd(NCS)2(C9H12N2O2)] | F(000) = 1736 |
Mr = 876.62 | Dx = 1.798 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 7320 reflections |
a = 10.040 (2) Å | θ = 3.2–27.5° |
b = 29.500 (6) Å | µ = 1.68 mm−1 |
c = 10.966 (2) Å | T = 293 K |
β = 94.58 (3)° | Block, colourless |
V = 3237.9 (11) Å3 | 0.20 × 0.20 × 0.20 mm |
Z = 4 |
Rigaku SCXmini diffractometer | 3882 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.105 |
Graphite monochromator | θmax = 27.5°, θmin = 3.2° |
ω scans | h = −12→13 |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005) | k = −38→31 |
Tmin = 0.730, Tmax = 0.730 | l = −14→14 |
20257 measured reflections | 3 standard reflections every 180 reflections |
7320 independent reflections | intensity decay: none |
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)] = 0.071 | H-atom parameters constrained |
wR(F2) = 0.111 | w = 1/[σ2(Fo2) + (0.0208P)2 + 1.2625P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max < 0.001 |
7320 reflections | Δρmax = 0.59 e Å−3 |
393 parameters | Δρmin = −0.64 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 2008) |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0819 (12) |
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 | ||
Cd1 | 0.51914 (5) | 0.041738 (18) | 0.75495 (4) | 0.04176 (17) | |
Cd2 | 0.94922 (6) | 0.255263 (17) | 0.56172 (4) | 0.04225 (17) | |
S5 | 1.1785 (2) | 0.28037 (7) | 0.46280 (18) | 0.0567 (6) | |
S3 | 0.7662 (2) | 0.30422 (7) | 0.41403 (16) | 0.0532 (6) | |
S1 | 0.7043 (2) | −0.01086 (7) | 0.67081 (17) | 0.0544 (6) | |
S4 | 0.9538 (2) | 0.33571 (7) | 0.68868 (17) | 0.0556 (6) | |
S2 | 0.6891 (2) | 0.06062 (7) | 0.95530 (18) | 0.0582 (6) | |
C11 | 0.6415 (7) | 0.0243 (3) | 1.0555 (7) | 0.047 (2) | |
C10 | 0.6493 (7) | −0.0218 (2) | 0.5270 (7) | 0.0409 (19) | |
O3 | 0.9978 (5) | 0.02235 (16) | 0.8686 (4) | 0.0461 (13) | |
N5 | 1.0248 (6) | 0.09758 (18) | 0.7348 (5) | 0.0400 (15) | |
O1 | 0.5522 (5) | 0.11346 (17) | 0.6792 (5) | 0.0615 (15) | |
N6 | 0.8406 (6) | 0.07528 (19) | 0.3917 (5) | 0.0427 (15) | |
N3 | 0.3829 (6) | 0.0295 (2) | 0.5737 (6) | 0.0550 (19) | |
N1 | 0.4138 (6) | 0.18172 (19) | 0.5431 (5) | 0.0423 (15) | |
C23 | 1.1212 (7) | 0.2791 (2) | 0.3182 (7) | 0.0422 (19) | |
N7 | 0.9259 (7) | 0.19719 (19) | 0.4235 (6) | 0.058 (2) | |
C21 | 0.7736 (7) | 0.2815 (2) | 0.2773 (6) | 0.0391 (18) | |
C14 | 0.9012 (7) | 0.0841 (2) | 0.5000 (6) | 0.0329 (16) | |
C5 | 0.3119 (7) | 0.1592 (3) | 0.4806 (7) | 0.055 (2) | |
H5 | 0.2407 | 0.1491 | 0.5225 | 0.066* | |
C18 | 1.0495 (7) | 0.0544 (2) | 0.9219 (6) | 0.0372 (17) | |
O2 | 0.3833 (5) | 0.11245 (18) | 0.7918 (4) | 0.0594 (15) | |
N2 | 0.4255 (6) | 0.1540 (2) | 0.1749 (6) | 0.0503 (17) | |
N8 | 0.7729 (6) | 0.2325 (2) | 0.6798 (5) | 0.0499 (17) | |
C22 | 0.9376 (7) | 0.3155 (2) | 0.8274 (7) | 0.0418 (19) | |
N4 | 0.3894 (7) | 0.0003 (2) | 0.8721 (6) | 0.067 (2) | |
C13 | 1.0352 (6) | 0.0712 (2) | 0.5340 (6) | 0.0360 (17) | |
H13 | 1.0860 | 0.0582 | 0.4759 | 0.043* | |
C2 | 0.5148 (7) | 0.1921 (2) | 0.3589 (7) | 0.0459 (19) | |
H2 | 0.5812 | 0.2059 | 0.3173 | 0.055* | |
C3 | 0.4159 (7) | 0.1656 (2) | 0.2934 (7) | 0.0392 (18) | |
C12 | 1.0906 (7) | 0.0775 (2) | 0.6498 (6) | 0.0407 (18) | |
H12 | 1.1773 | 0.0675 | 0.6700 | 0.049* | |
C15 | 0.8366 (7) | 0.1062 (2) | 0.5929 (7) | 0.0447 (19) | |
H15 | 0.7501 | 0.1170 | 0.5756 | 0.054* | |
O4 | 1.0872 (6) | 0.05409 (16) | 1.0398 (4) | 0.0576 (15) | |
H4 | 1.0718 | 0.0291 | 1.0684 | 0.086* | |
C17 | 1.0794 (8) | 0.0986 (2) | 0.8622 (6) | 0.049 (2) | |
H17A | 1.0396 | 0.1234 | 0.9049 | 0.059* | |
H17B | 1.1752 | 0.1035 | 0.8661 | 0.059* | |
C20 | 0.7022 (7) | 0.0894 (3) | 0.3592 (7) | 0.063 (2) | |
H20A | 0.6456 | 0.0775 | 0.4181 | 0.094* | |
H20B | 0.6733 | 0.0780 | 0.2795 | 0.094* | |
H20C | 0.6970 | 0.1219 | 0.3588 | 0.094* | |
N9 | 1.0867 (7) | 0.2201 (2) | 0.7154 (6) | 0.062 (2) | |
C16 | 0.8971 (8) | 0.1121 (2) | 0.7060 (6) | 0.044 (2) | |
H16 | 0.8510 | 0.1264 | 0.7654 | 0.053* | |
C7 | 0.4553 (7) | 0.1312 (3) | 0.7228 (6) | 0.0386 (18) | |
C6 | 0.4211 (8) | 0.1804 (2) | 0.6787 (6) | 0.051 (2) | |
H6A | 0.3361 | 0.1896 | 0.7071 | 0.061* | |
H6B | 0.4893 | 0.2012 | 0.7122 | 0.061* | |
C1 | 0.5142 (7) | 0.1977 (2) | 0.4827 (7) | 0.048 (2) | |
H1 | 0.5845 | 0.2129 | 0.5253 | 0.058* | |
C8 | 0.5284 (8) | 0.1722 (3) | 0.1015 (7) | 0.072 (3) | |
H8A | 0.4951 | 0.1731 | 0.0171 | 0.108* | |
H8B | 0.6063 | 0.1533 | 0.1107 | 0.108* | |
H8C | 0.5515 | 0.2024 | 0.1288 | 0.108* | |
C9 | 0.3330 (8) | 0.1209 (3) | 0.1148 (7) | 0.072 (3) | |
H9A | 0.3432 | 0.0922 | 0.1561 | 0.108* | |
H9B | 0.3523 | 0.1173 | 0.0310 | 0.108* | |
H9C | 0.2428 | 0.1314 | 0.1179 | 0.108* | |
C19 | 0.9057 (8) | 0.0497 (2) | 0.2990 (6) | 0.057 (2) | |
H19A | 0.9856 | 0.0651 | 0.2799 | 0.086* | |
H19B | 0.8461 | 0.0471 | 0.2264 | 0.086* | |
H19C | 0.9282 | 0.0199 | 0.3297 | 0.086* | |
C4 | 0.3113 (8) | 0.1513 (3) | 0.3615 (7) | 0.063 (2) | |
H4A | 0.2394 | 0.1359 | 0.3222 | 0.076* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0403 (3) | 0.0544 (4) | 0.0309 (3) | 0.0051 (3) | 0.0047 (2) | 0.0025 (3) |
Cd2 | 0.0531 (4) | 0.0447 (3) | 0.0301 (3) | −0.0018 (3) | 0.0104 (3) | 0.0000 (3) |
S5 | 0.0506 (14) | 0.0734 (15) | 0.0462 (12) | −0.0063 (12) | 0.0051 (11) | −0.0013 (11) |
S3 | 0.0717 (16) | 0.0585 (13) | 0.0316 (11) | 0.0129 (12) | 0.0177 (10) | 0.0005 (10) |
S1 | 0.0514 (13) | 0.0723 (15) | 0.0373 (11) | 0.0265 (12) | −0.0097 (10) | −0.0119 (11) |
S4 | 0.0853 (17) | 0.0441 (12) | 0.0388 (12) | −0.0061 (12) | 0.0135 (11) | 0.0010 (10) |
S2 | 0.0507 (14) | 0.0789 (16) | 0.0438 (12) | −0.0205 (12) | −0.0029 (10) | 0.0098 (11) |
C11 | 0.036 (5) | 0.069 (6) | 0.033 (5) | −0.008 (4) | −0.008 (4) | −0.013 (4) |
C10 | 0.030 (4) | 0.036 (4) | 0.057 (5) | 0.008 (3) | 0.005 (4) | −0.001 (4) |
O3 | 0.058 (4) | 0.046 (3) | 0.034 (3) | −0.009 (3) | 0.000 (3) | −0.007 (2) |
N5 | 0.051 (4) | 0.034 (3) | 0.037 (4) | −0.003 (3) | 0.017 (3) | −0.005 (3) |
O1 | 0.052 (4) | 0.061 (4) | 0.074 (4) | 0.018 (3) | 0.022 (3) | 0.012 (3) |
N6 | 0.038 (4) | 0.046 (4) | 0.045 (4) | 0.006 (3) | 0.005 (3) | −0.003 (3) |
N3 | 0.033 (4) | 0.084 (5) | 0.047 (4) | 0.008 (3) | 0.001 (3) | −0.012 (4) |
N1 | 0.044 (4) | 0.043 (4) | 0.041 (4) | 0.005 (3) | 0.008 (3) | 0.003 (3) |
C23 | 0.039 (5) | 0.041 (4) | 0.049 (5) | −0.012 (4) | 0.021 (4) | 0.000 (4) |
N7 | 0.094 (6) | 0.040 (4) | 0.040 (4) | −0.016 (4) | 0.010 (4) | −0.001 (3) |
C21 | 0.039 (5) | 0.037 (4) | 0.041 (4) | 0.001 (4) | 0.002 (4) | 0.013 (4) |
C14 | 0.037 (4) | 0.025 (4) | 0.038 (4) | 0.003 (3) | 0.010 (4) | 0.006 (3) |
C5 | 0.029 (5) | 0.087 (6) | 0.050 (5) | −0.010 (4) | 0.012 (4) | 0.009 (5) |
C18 | 0.034 (4) | 0.048 (5) | 0.030 (4) | −0.006 (4) | 0.010 (3) | −0.014 (4) |
O2 | 0.050 (4) | 0.074 (4) | 0.057 (4) | −0.006 (3) | 0.020 (3) | 0.006 (3) |
N2 | 0.049 (4) | 0.055 (4) | 0.046 (4) | −0.007 (3) | −0.002 (4) | 0.008 (3) |
N8 | 0.061 (5) | 0.066 (4) | 0.024 (3) | −0.004 (4) | 0.005 (3) | −0.001 (3) |
C22 | 0.044 (5) | 0.039 (4) | 0.043 (5) | 0.008 (4) | 0.004 (4) | −0.013 (4) |
N4 | 0.057 (5) | 0.099 (6) | 0.044 (4) | −0.029 (4) | 0.002 (4) | 0.012 (4) |
C13 | 0.031 (4) | 0.044 (4) | 0.035 (4) | 0.010 (3) | 0.015 (3) | 0.000 (4) |
C2 | 0.043 (5) | 0.051 (5) | 0.045 (5) | −0.006 (4) | 0.011 (4) | 0.006 (4) |
C3 | 0.032 (4) | 0.038 (4) | 0.046 (5) | −0.001 (4) | −0.005 (4) | 0.009 (4) |
C12 | 0.033 (5) | 0.049 (5) | 0.041 (5) | 0.003 (4) | 0.010 (4) | 0.000 (4) |
C15 | 0.036 (5) | 0.049 (5) | 0.051 (5) | 0.013 (4) | 0.020 (4) | 0.000 (4) |
O4 | 0.089 (4) | 0.051 (3) | 0.033 (3) | −0.024 (3) | 0.001 (3) | −0.004 (2) |
C17 | 0.064 (6) | 0.051 (5) | 0.033 (4) | −0.018 (4) | 0.006 (4) | −0.015 (4) |
C20 | 0.051 (6) | 0.066 (6) | 0.069 (6) | 0.007 (5) | −0.007 (5) | −0.002 (5) |
N9 | 0.061 (5) | 0.078 (5) | 0.046 (4) | 0.014 (4) | 0.005 (4) | 0.007 (4) |
C16 | 0.064 (6) | 0.034 (4) | 0.040 (5) | 0.014 (4) | 0.032 (4) | 0.001 (4) |
C7 | 0.021 (4) | 0.063 (5) | 0.032 (4) | −0.005 (4) | 0.002 (3) | −0.004 (4) |
C6 | 0.059 (6) | 0.054 (5) | 0.042 (5) | 0.008 (4) | 0.012 (4) | −0.014 (4) |
C1 | 0.037 (5) | 0.047 (5) | 0.060 (5) | −0.013 (4) | 0.001 (4) | 0.005 (4) |
C8 | 0.071 (6) | 0.085 (7) | 0.063 (6) | −0.012 (5) | 0.028 (5) | 0.008 (5) |
C9 | 0.082 (7) | 0.082 (6) | 0.050 (5) | −0.029 (6) | −0.012 (5) | 0.002 (5) |
C19 | 0.067 (6) | 0.067 (6) | 0.035 (4) | 0.011 (5) | −0.007 (4) | −0.019 (4) |
C4 | 0.048 (6) | 0.092 (7) | 0.050 (6) | −0.019 (5) | 0.006 (5) | 0.015 (5) |
Cd1—N4 | 2.260 (7) | C18—C17 | 1.502 (9) |
Cd1—O1 | 2.306 (5) | O2—C7 | 1.220 (8) |
Cd1—N3 | 2.349 (6) | N2—C3 | 1.354 (8) |
Cd1—O2 | 2.542 (5) | N2—C8 | 1.462 (9) |
Cd1—S1 | 2.643 (2) | N2—C9 | 1.468 (8) |
Cd1—S2 | 2.730 (2) | N8—C21iv | 1.146 (8) |
Cd2—N7 | 2.287 (6) | C22—N7iv | 1.133 (8) |
Cd2—N9 | 2.335 (6) | N4—C11i | 1.138 (8) |
Cd2—N8 | 2.372 (6) | C13—C12 | 1.357 (8) |
Cd2—S5 | 2.724 (2) | C13—H13 | 0.9300 |
Cd2—S4 | 2.750 (2) | C2—C1 | 1.369 (9) |
Cd2—S3 | 2.759 (2) | C2—C3 | 1.414 (9) |
S5—C23 | 1.643 (8) | C2—H2 | 0.9300 |
S3—C21 | 1.649 (7) | C3—C4 | 1.403 (9) |
S1—C10 | 1.661 (8) | C12—H12 | 0.9300 |
S4—C22 | 1.654 (8) | C15—C16 | 1.348 (9) |
S2—C11 | 1.633 (8) | C15—H15 | 0.9300 |
C11—N4i | 1.138 (8) | O4—H4 | 0.8200 |
C10—N3ii | 1.148 (8) | C17—H17A | 0.9700 |
O3—C18 | 1.206 (7) | C17—H17B | 0.9700 |
N5—C12 | 1.325 (8) | C20—H20A | 0.9600 |
N5—C16 | 1.365 (8) | C20—H20B | 0.9600 |
N5—C17 | 1.460 (7) | C20—H20C | 0.9600 |
O1—C7 | 1.234 (8) | N9—C23iv | 1.153 (8) |
N6—C14 | 1.316 (8) | C16—H16 | 0.9300 |
N6—C19 | 1.463 (8) | C7—C6 | 1.559 (9) |
N6—C20 | 1.467 (8) | C6—H6A | 0.9700 |
N3—C10ii | 1.148 (8) | C6—H6B | 0.9700 |
N1—C1 | 1.336 (8) | C1—H1 | 0.9300 |
N1—C5 | 1.359 (8) | C8—H8A | 0.9600 |
N1—C6 | 1.483 (8) | C8—H8B | 0.9600 |
C23—N9iii | 1.153 (8) | C8—H8C | 0.9600 |
N7—C22iii | 1.133 (8) | C9—H9A | 0.9600 |
C21—N8iii | 1.146 (8) | C9—H9B | 0.9600 |
C14—C15 | 1.410 (8) | C9—H9C | 0.9600 |
C14—C13 | 1.419 (8) | C19—H19A | 0.9600 |
C5—C4 | 1.326 (9) | C19—H19B | 0.9600 |
C5—H5 | 0.9300 | C19—H19C | 0.9600 |
C18—O4 | 1.318 (7) | C4—H4A | 0.9300 |
N4—Cd1—O1 | 143.7 (2) | C11i—N4—Cd1 | 160.7 (7) |
N4—Cd1—N3 | 94.3 (2) | C12—C13—C14 | 121.2 (6) |
O1—Cd1—N3 | 85.8 (2) | C12—C13—H13 | 119.4 |
N4—Cd1—O2 | 90.7 (2) | C14—C13—H13 | 119.4 |
O1—Cd1—O2 | 53.04 (16) | C1—C2—C3 | 120.8 (7) |
N3—Cd1—O2 | 88.68 (19) | C1—C2—H2 | 119.6 |
N4—Cd1—S1 | 109.5 (2) | C3—C2—H2 | 119.6 |
O1—Cd1—S1 | 106.72 (14) | N2—C3—C4 | 123.3 (7) |
N3—Cd1—S1 | 89.58 (15) | N2—C3—C2 | 121.8 (7) |
O2—Cd1—S1 | 159.76 (13) | C4—C3—C2 | 114.9 (7) |
N4—Cd1—S2 | 90.27 (16) | N5—C12—C13 | 122.0 (6) |
O1—Cd1—S2 | 90.23 (14) | N5—C12—H12 | 119.0 |
N3—Cd1—S2 | 175.42 (17) | C13—C12—H12 | 119.0 |
O2—Cd1—S2 | 90.78 (12) | C16—C15—C14 | 121.7 (7) |
S1—Cd1—S2 | 89.36 (7) | C16—C15—H15 | 119.2 |
N7—Cd2—N9 | 99.7 (2) | C14—C15—H15 | 119.2 |
N7—Cd2—N8 | 96.2 (2) | C18—O4—H4 | 109.5 |
N9—Cd2—N8 | 84.5 (2) | N5—C17—C18 | 109.0 (5) |
N7—Cd2—S5 | 89.13 (18) | N5—C17—H17A | 109.9 |
N9—Cd2—S5 | 86.47 (18) | C18—C17—H17A | 109.9 |
N8—Cd2—S5 | 170.17 (14) | N5—C17—H17B | 109.9 |
N7—Cd2—S4 | 168.13 (16) | C18—C17—H17B | 109.9 |
N9—Cd2—S4 | 91.89 (17) | H17A—C17—H17B | 108.3 |
N8—Cd2—S4 | 87.16 (15) | N6—C20—H20A | 109.5 |
S5—Cd2—S4 | 89.23 (7) | N6—C20—H20B | 109.5 |
N7—Cd2—S3 | 88.55 (17) | H20A—C20—H20B | 109.5 |
N9—Cd2—S3 | 169.80 (17) | N6—C20—H20C | 109.5 |
N8—Cd2—S3 | 88.70 (15) | H20A—C20—H20C | 109.5 |
S5—Cd2—S3 | 99.69 (6) | H20B—C20—H20C | 109.5 |
S4—Cd2—S3 | 80.14 (6) | C23iv—N9—Cd2 | 144.2 (6) |
C23—S5—Cd2 | 97.8 (3) | C15—C16—N5 | 121.2 (6) |
C21—S3—Cd2 | 104.2 (2) | C15—C16—H16 | 119.4 |
C10—S1—Cd1 | 104.9 (2) | N5—C16—H16 | 119.4 |
C22—S4—Cd2 | 98.9 (2) | O2—C7—O1 | 124.9 (8) |
C11—S2—Cd1 | 102.1 (2) | O2—C7—C6 | 119.2 (7) |
N4i—C11—S2 | 177.9 (7) | O1—C7—C6 | 115.8 (7) |
N3ii—C10—S1 | 177.0 (7) | N1—C6—C7 | 109.1 (5) |
C12—N5—C16 | 119.3 (6) | N1—C6—H6A | 109.9 |
C12—N5—C17 | 120.9 (6) | C7—C6—H6A | 109.9 |
C16—N5—C17 | 119.3 (6) | N1—C6—H6B | 109.9 |
C7—O1—Cd1 | 96.3 (5) | C7—C6—H6B | 109.9 |
C14—N6—C19 | 122.0 (6) | H6A—C6—H6B | 108.3 |
C14—N6—C20 | 121.6 (6) | N1—C1—C2 | 120.8 (7) |
C19—N6—C20 | 116.4 (6) | N1—C1—H1 | 119.6 |
C10ii—N3—Cd1 | 160.8 (6) | C2—C1—H1 | 119.6 |
C1—N1—C5 | 119.3 (6) | N2—C8—H8A | 109.5 |
C1—N1—C6 | 121.9 (6) | N2—C8—H8B | 109.5 |
C5—N1—C6 | 117.9 (6) | H8A—C8—H8B | 109.5 |
N9iii—C23—S5 | 176.1 (7) | N2—C8—H8C | 109.5 |
C22iii—N7—Cd2 | 148.3 (6) | H8A—C8—H8C | 109.5 |
N8iii—C21—S3 | 176.0 (7) | H8B—C8—H8C | 109.5 |
N6—C14—C15 | 122.5 (7) | N2—C9—H9A | 109.5 |
N6—C14—C13 | 123.0 (6) | N2—C9—H9B | 109.5 |
C15—C14—C13 | 114.5 (6) | H9A—C9—H9B | 109.5 |
C4—C5—N1 | 121.8 (7) | N2—C9—H9C | 109.5 |
C4—C5—H5 | 119.1 | H9A—C9—H9C | 109.5 |
N1—C5—H5 | 119.1 | H9B—C9—H9C | 109.5 |
O3—C18—O4 | 123.3 (7) | N6—C19—H19A | 109.5 |
O3—C18—C17 | 124.3 (6) | N6—C19—H19B | 109.5 |
O4—C18—C17 | 112.4 (6) | H19A—C19—H19B | 109.5 |
C7—O2—Cd1 | 85.5 (5) | N6—C19—H19C | 109.5 |
C3—N2—C8 | 122.8 (6) | H19A—C19—H19C | 109.5 |
C3—N2—C9 | 120.6 (6) | H19B—C19—H19C | 109.5 |
C8—N2—C9 | 116.6 (6) | C5—C4—C3 | 121.8 (8) |
C21iv—N8—Cd2 | 131.5 (6) | C5—C4—H4A | 119.1 |
N7iv—C22—S4 | 178.1 (7) | C3—C4—H4A | 119.1 |
N7—Cd2—S5—C23 | 47.9 (3) | S1—Cd1—O2—C7 | 2.3 (6) |
N9—Cd2—S5—C23 | 147.8 (3) | S2—Cd1—O2—C7 | 92.6 (4) |
N8—Cd2—S5—C23 | 171.3 (9) | N7—Cd2—N8—C21iv | 111.1 (7) |
S4—Cd2—S5—C23 | −120.3 (3) | N9—Cd2—N8—C21iv | 11.8 (7) |
S3—Cd2—S5—C23 | −40.4 (3) | S5—Cd2—N8—C21iv | −11.7 (15) |
N7—Cd2—S3—C21 | −23.2 (3) | S4—Cd2—N8—C21iv | −80.3 (7) |
N9—Cd2—S3—C21 | −167.8 (10) | S3—Cd2—N8—C21iv | −160.5 (7) |
N8—Cd2—S3—C21 | −119.5 (3) | Cd2—S4—C22—N7iv | −169 (23) |
S5—Cd2—S3—C21 | 65.7 (3) | O1—Cd1—N4—C11i | −132 (2) |
S4—Cd2—S3—C21 | 153.2 (3) | N3—Cd1—N4—C11i | 139 (2) |
N4—Cd1—S1—C10 | 101.8 (3) | O2—Cd1—N4—C11i | −132 (2) |
O1—Cd1—S1—C10 | −78.1 (3) | S1—Cd1—N4—C11i | 48 (2) |
N3—Cd1—S1—C10 | 7.4 (3) | S2—Cd1—N4—C11i | −41 (2) |
O2—Cd1—S1—C10 | −77.7 (4) | N6—C14—C13—C12 | −174.4 (6) |
S2—Cd1—S1—C10 | −168.2 (3) | C15—C14—C13—C12 | 4.1 (9) |
N7—Cd2—S4—C22 | 149.4 (9) | C8—N2—C3—C4 | 174.5 (7) |
N9—Cd2—S4—C22 | −42.0 (3) | C9—N2—C3—C4 | −7.2 (10) |
N8—Cd2—S4—C22 | 42.4 (3) | C8—N2—C3—C2 | −7.8 (10) |
S5—Cd2—S4—C22 | −128.5 (3) | C9—N2—C3—C2 | 170.5 (7) |
S3—Cd2—S4—C22 | 131.6 (3) | C1—C2—C3—N2 | −170.0 (7) |
N4—Cd1—S2—C11 | 13.5 (3) | C1—C2—C3—C4 | 7.9 (10) |
O1—Cd1—S2—C11 | 157.2 (3) | C16—N5—C12—C13 | 0.5 (10) |
N3—Cd1—S2—C11 | −173 (2) | C17—N5—C12—C13 | 171.8 (6) |
O2—Cd1—S2—C11 | 104.2 (3) | C14—C13—C12—N5 | −2.8 (10) |
S1—Cd1—S2—C11 | −96.1 (3) | N6—C14—C15—C16 | 175.2 (6) |
Cd1—S2—C11—N4i | −168 (24) | C13—C14—C15—C16 | −3.2 (10) |
Cd1—S1—C10—N3ii | 148 (13) | C12—N5—C17—C18 | −81.4 (8) |
N4—Cd1—O1—C7 | −2.9 (6) | C16—N5—C17—C18 | 89.9 (7) |
N3—Cd1—O1—C7 | 88.7 (4) | O3—C18—C17—N5 | 5.2 (10) |
O2—Cd1—O1—C7 | −2.8 (4) | O4—C18—C17—N5 | −175.2 (6) |
S1—Cd1—O1—C7 | 177.0 (4) | N7—Cd2—N9—C23iv | −157.5 (11) |
S2—Cd1—O1—C7 | −93.6 (4) | N8—Cd2—N9—C23iv | −62.1 (11) |
N4—Cd1—N3—C10ii | −136.8 (19) | S5—Cd2—N9—C23iv | 114.0 (11) |
O1—Cd1—N3—C10ii | 79.6 (19) | S4—Cd2—N9—C23iv | 24.9 (11) |
O2—Cd1—N3—C10ii | 132.6 (19) | S3—Cd2—N9—C23iv | −14 (2) |
S1—Cd1—N3—C10ii | −27.2 (19) | C14—C15—C16—N5 | 1.1 (11) |
S2—Cd1—N3—C10ii | 49 (3) | C12—N5—C16—C15 | 0.4 (10) |
Cd2—S5—C23—N9iii | 158 (12) | C17—N5—C16—C15 | −171.1 (6) |
N9—Cd2—N7—C22iii | −123.0 (13) | Cd1—O2—C7—O1 | −5.2 (7) |
N8—Cd2—N7—C22iii | 151.5 (13) | Cd1—O2—C7—C6 | 171.3 (6) |
S5—Cd2—N7—C22iii | −36.7 (13) | Cd1—O1—C7—O2 | 5.8 (8) |
S4—Cd2—N7—C22iii | 45.4 (19) | Cd1—O1—C7—C6 | −170.9 (5) |
S3—Cd2—N7—C22iii | 63.0 (13) | C1—N1—C6—C7 | −101.0 (8) |
Cd2—S3—C21—N8iii | 177 (100) | C5—N1—C6—C7 | 68.0 (8) |
C19—N6—C14—C15 | −175.8 (6) | O2—C7—C6—N1 | −126.4 (7) |
C20—N6—C14—C15 | 2.1 (10) | O1—C7—C6—N1 | 50.4 (8) |
C19—N6—C14—C13 | 2.5 (10) | C5—N1—C1—C2 | 0.6 (10) |
C20—N6—C14—C13 | −179.6 (6) | C6—N1—C1—C2 | 169.5 (6) |
C1—N1—C5—C4 | 2.3 (11) | C3—C2—C1—N1 | −5.9 (11) |
C6—N1—C5—C4 | −167.0 (7) | N1—C5—C4—C3 | 0.2 (13) |
N4—Cd1—O2—C7 | −177.2 (4) | N2—C3—C4—C5 | 172.7 (8) |
O1—Cd1—O2—C7 | 2.9 (4) | C2—C3—C4—C5 | −5.2 (11) |
N3—Cd1—O2—C7 | −82.9 (4) |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x+1, −y, −z+1; (iii) x, −y+1/2, z−1/2; (iv) x, −y+1/2, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H4···O3v | 0.82 | 1.83 | 2.638 (6) | 168 |
C16—H16···S3iv | 0.93 | 2.79 | 3.674 (7) | 159 |
C17—H17B···O2vi | 0.97 | 2.32 | 3.233 (9) | 157 |
C1—H1···N8 | 0.93 | 2.50 | 3.403 (9) | 163 |
C15—H15···O1 | 0.93 | 2.37 | 3.088 (9) | 134 |
Symmetry codes: (iv) x, −y+1/2, z+1/2; (v) −x+2, −y, −z+2; (vi) x+1, y, z. |