Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806042681/ng2122sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806042681/ng2122Isup2.hkl |
CCDC reference: 628017
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: PATTY in DIRDIF92 (Beurskens et al., 1992); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97.
[Ni(C11H17OS2)2(C10H8N2)]·2CHCl3 | F(000) = 1888 |
Mr = 912.36 | Dx = 1.447 Mg m−3 |
Monoclinic, C2 | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: C 2y | Cell parameters from 3355 reflections |
a = 32.739 (2) Å | θ = 2.5–27.2° |
b = 11.3308 (8) Å | µ = 1.08 mm−1 |
c = 11.9635 (9) Å | T = 223 K |
β = 109.297 (2)° | Block, green |
V = 4188.6 (5) Å3 | 0.36 × 0.13 × 0.02 mm |
Z = 4 |
Bruker SMART CCD diffractometer | 11449 independent reflections |
Radiation source: fine-focus sealed tube | 8532 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
φ and ω scans | θmax = 30.1°, θmin = 1.3° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −46→46 |
Tmin = 0.599, Tmax = 1 | k = −15→15 |
17757 measured reflections | l = −16→10 |
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)] = 0.059 | H-atom parameters constrained |
wR(F2) = 0.165 | w = 1/[σ2(Fo2) + (0.0949P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max < 0.001 |
11449 reflections | Δρmax = 0.80 e Å−3 |
447 parameters | Δρmin = −1.07 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 4996 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.020 (17) |
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 | ||
Ni1 | 0.0000 | −0.05582 (5) | −0.5000 | 0.01589 (17) | |
Ni2 | 0.0000 | −0.00247 (5) | 0.0000 | 0.01502 (16) | |
Cl1 | −0.09606 (7) | −0.27674 (19) | −0.2705 (2) | 0.0840 (6) | |
Cl2 | −0.13084 (9) | −0.4363 (5) | −0.4683 (2) | 0.1536 (17) | |
Cl3 | −0.09786 (9) | −0.5241 (2) | −0.2346 (3) | 0.1110 (9) | |
Cl4 | −0.37453 (9) | −0.1757 (3) | −0.0039 (2) | 0.1046 (9) | |
Cl5 | −0.41591 (6) | −0.2085 (2) | −0.25157 (17) | 0.0768 (6) | |
Cl6 | −0.32472 (7) | −0.2504 (2) | −0.1492 (3) | 0.1122 (9) | |
S1 | 0.04419 (3) | −0.06210 (11) | −0.29225 (9) | 0.0217 (2) | |
S2 | 0.07460 (3) | −0.06511 (11) | −0.49637 (9) | 0.0222 (2) | |
S3 | 0.07324 (3) | 0.00694 (11) | −0.00683 (9) | 0.0200 (2) | |
S4 | 0.04856 (3) | 0.00182 (11) | 0.20710 (9) | 0.0206 (2) | |
O1 | 0.12583 (11) | −0.1014 (4) | −0.2848 (3) | 0.0414 (11) | |
O2 | 0.12867 (9) | 0.0334 (3) | 0.1996 (3) | 0.0277 (8) | |
N1 | 0.0000 | −0.2432 (5) | −0.5000 | 0.0191 (11) | |
N2 | 0.0000 | −0.8703 (5) | −0.5000 | 0.0214 (12) | |
N3 | 0.0000 | −0.1879 (4) | 0.0000 | 0.0177 (11) | |
N4 | 0.0000 | −0.8150 (5) | 0.0000 | 0.0193 (11) | |
C1 | 0.08526 (14) | −0.0785 (4) | −0.3478 (4) | 0.0220 (9) | |
C2 | 0.13753 (14) | −0.1497 (5) | −0.1670 (4) | 0.0281 (10) | |
H2 | 0.1124 | −0.1491 | −0.1386 | 0.034* | |
C3 | 0.15454 (15) | −0.2760 (5) | −0.1671 (4) | 0.0326 (10) | |
C4 | 0.18946 (16) | −0.2733 (6) | −0.2253 (5) | 0.0436 (13) | |
H4A | 0.1983 | −0.3535 | −0.2379 | 0.052* | |
H4B | 0.1791 | −0.2324 | −0.3017 | 0.052* | |
C5 | 0.22774 (17) | −0.2049 (5) | −0.1361 (5) | 0.0445 (13) | |
H5A | 0.2538 | −0.2540 | −0.1083 | 0.053* | |
H5B | 0.2344 | −0.1325 | −0.1714 | 0.053* | |
C6 | 0.20980 (16) | −0.1774 (5) | −0.0356 (5) | 0.0368 (12) | |
H6 | 0.2322 | −0.1589 | 0.0411 | 0.044* | |
C7 | 0.17577 (16) | −0.0818 (5) | −0.0807 (5) | 0.0369 (11) | |
H7A | 0.1860 | −0.0193 | −0.1215 | 0.044* | |
H7B | 0.1678 | −0.0470 | −0.0158 | 0.044* | |
C8 | 0.1187 (2) | −0.3650 (6) | −0.2212 (6) | 0.0547 (16) | |
H8A | 0.1313 | −0.4427 | −0.2206 | 0.082* | |
H8B | 0.1028 | −0.3424 | −0.3022 | 0.082* | |
H8C | 0.0992 | −0.3668 | −0.1755 | 0.082* | |
C9 | 0.18216 (16) | −0.2898 (5) | −0.0330 (4) | 0.0345 (11) | |
C10 | 0.15686 (19) | −0.2793 (6) | 0.0508 (5) | 0.0495 (14) | |
H10A | 0.1761 | −0.2900 | 0.1314 | 0.074* | |
H10B | 0.1345 | −0.3393 | 0.0322 | 0.074* | |
H10C | 0.1436 | −0.2018 | 0.0428 | 0.074* | |
C11 | 0.2082 (2) | −0.4029 (6) | −0.0028 (6) | 0.0587 (17) | |
H11A | 0.2243 | −0.4135 | −0.0570 | 0.088* | |
H11B | 0.1887 | −0.4692 | −0.0098 | 0.088* | |
H11C | 0.2281 | −0.3984 | 0.0777 | 0.088* | |
C12 | 0.08656 (13) | 0.0160 (4) | 0.1410 (4) | 0.0191 (9) | |
C13 | 0.14544 (13) | 0.0455 (4) | 0.3289 (4) | 0.0240 (9) | |
H13 | 0.1323 | −0.0150 | 0.3662 | 0.029* | |
C14 | 0.19461 (14) | 0.0304 (4) | 0.3702 (4) | 0.0331 (10) | |
C15 | 0.21177 (16) | 0.1153 (6) | 0.2980 (5) | 0.0498 (16) | |
H15A | 0.1954 | 0.1080 | 0.2133 | 0.060* | |
H15B | 0.2424 | 0.1000 | 0.3102 | 0.060* | |
C16 | 0.2056 (2) | 0.2391 (6) | 0.3443 (6) | 0.0555 (17) | |
H16A | 0.2334 | 0.2800 | 0.3780 | 0.067* | |
H16B | 0.1862 | 0.2878 | 0.2813 | 0.067* | |
C17 | 0.18589 (17) | 0.2104 (5) | 0.4380 (5) | 0.0400 (13) | |
H17 | 0.1884 | 0.2742 | 0.4964 | 0.048* | |
C18 | 0.13843 (17) | 0.1690 (5) | 0.3722 (5) | 0.0390 (12) | |
H18A | 0.1215 | 0.1654 | 0.4261 | 0.047* | |
H18B | 0.1238 | 0.2212 | 0.3057 | 0.047* | |
C19 | 0.2089 (2) | −0.0956 (5) | 0.3674 (7) | 0.0631 (19) | |
H19A | 0.1975 | −0.1438 | 0.4171 | 0.095* | |
H19B | 0.2403 | −0.0993 | 0.3965 | 0.095* | |
H19C | 0.1982 | −0.1248 | 0.2867 | 0.095* | |
C20 | 0.20766 (16) | 0.0937 (5) | 0.4919 (4) | 0.0352 (12) | |
C21 | 0.1907 (2) | 0.0376 (7) | 0.5819 (5) | 0.0594 (18) | |
H21A | 0.1595 | 0.0301 | 0.5488 | 0.089* | |
H21B | 0.1982 | 0.0866 | 0.6523 | 0.089* | |
H21C | 0.2035 | −0.0399 | 0.6025 | 0.089* | |
C22 | 0.25620 (17) | 0.1038 (6) | 0.5525 (5) | 0.0529 (16) | |
H22A | 0.2621 | 0.1439 | 0.6278 | 0.079* | |
H22B | 0.2687 | 0.1484 | 0.5026 | 0.079* | |
H22C | 0.2689 | 0.0255 | 0.5658 | 0.079* | |
C23 | −0.01073 (15) | −0.3056 (5) | −0.4186 (4) | 0.0248 (11) | |
H23 | −0.0183 | −0.2638 | −0.3605 | 0.030* | |
C24 | −0.01138 (16) | −0.4264 (4) | −0.4148 (4) | 0.0256 (10) | |
H24 | −0.0193 | −0.4657 | −0.3558 | 0.031* | |
C25 | 0.0000 | −0.4902 (6) | −0.5000 | 0.0221 (13) | |
C26 | 0.0000 | −0.6225 (6) | −0.5000 | 0.0212 (14) | |
C27 | −0.02289 (16) | −0.6863 (4) | −0.4412 (4) | 0.0251 (11) | |
H27 | −0.0392 | −0.6469 | −0.4012 | 0.030* | |
C28 | −0.02141 (15) | −0.8101 (4) | −0.4420 (4) | 0.0220 (10) | |
H28 | −0.0362 | −0.8522 | −0.3995 | 0.026* | |
C29 | −0.01979 (15) | −0.2518 (4) | 0.0635 (4) | 0.0247 (11) | |
H29 | −0.0338 | −0.2109 | 0.1089 | 0.030* | |
C30 | −0.02039 (16) | −0.3714 (4) | 0.0648 (4) | 0.0244 (11) | |
H30 | −0.0348 | −0.4107 | 0.1102 | 0.029* | |
C31 | 0.0000 | −0.4373 (6) | 0.0000 | 0.0203 (13) | |
C32 | 0.0000 | −0.5677 (6) | 0.0000 | 0.0190 (12) | |
C33 | −0.00751 (16) | −0.6329 (4) | 0.0897 (4) | 0.0254 (10) | |
H33 | −0.0127 | −0.5936 | 0.1529 | 0.031* | |
C34 | −0.00747 (16) | −0.7553 (4) | 0.0868 (4) | 0.0224 (10) | |
H34 | −0.0129 | −0.7973 | 0.1482 | 0.027* | |
C35 | −0.1254 (2) | −0.4085 (8) | −0.3245 (7) | 0.076 (2) | |
H35 | −0.1546 | −0.4016 | −0.3173 | 0.091* | |
C36 | −0.3756 (2) | −0.2593 (6) | −0.1289 (7) | 0.065 (2) | |
H36 | −0.3816 | −0.3428 | −0.1153 | 0.078* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0186 (4) | 0.0128 (4) | 0.0173 (4) | 0.000 | 0.0074 (3) | 0.000 |
Ni2 | 0.0178 (3) | 0.0106 (3) | 0.0172 (4) | 0.000 | 0.0065 (3) | 0.000 |
Cl1 | 0.0818 (14) | 0.0600 (10) | 0.1241 (18) | −0.0001 (10) | 0.0527 (13) | 0.0096 (12) |
Cl2 | 0.0875 (17) | 0.290 (5) | 0.0814 (17) | −0.024 (3) | 0.0252 (14) | −0.027 (3) |
Cl3 | 0.1148 (19) | 0.0560 (12) | 0.129 (2) | −0.0087 (12) | −0.0049 (15) | 0.0095 (13) |
Cl4 | 0.1077 (18) | 0.126 (2) | 0.0700 (13) | −0.0482 (17) | 0.0160 (13) | −0.0111 (14) |
Cl5 | 0.0523 (10) | 0.1024 (16) | 0.0633 (11) | −0.0076 (10) | 0.0024 (8) | 0.0082 (11) |
Cl6 | 0.0516 (11) | 0.0906 (16) | 0.188 (3) | 0.0042 (11) | 0.0316 (15) | −0.0045 (17) |
S1 | 0.0212 (5) | 0.0268 (6) | 0.0180 (5) | 0.0025 (5) | 0.0079 (4) | 0.0000 (5) |
S2 | 0.0210 (5) | 0.0271 (6) | 0.0207 (5) | 0.0010 (5) | 0.0099 (4) | 0.0033 (5) |
S3 | 0.0207 (5) | 0.0218 (5) | 0.0192 (5) | −0.0008 (5) | 0.0087 (4) | −0.0018 (5) |
S4 | 0.0200 (5) | 0.0255 (5) | 0.0170 (5) | −0.0003 (5) | 0.0070 (4) | 0.0007 (5) |
O1 | 0.0189 (16) | 0.078 (3) | 0.0273 (17) | 0.0061 (17) | 0.0083 (14) | 0.0211 (19) |
O2 | 0.0191 (15) | 0.0397 (19) | 0.0254 (15) | −0.0036 (13) | 0.0090 (13) | 0.0011 (14) |
N1 | 0.020 (3) | 0.015 (3) | 0.023 (3) | 0.000 | 0.009 (2) | 0.000 |
N2 | 0.019 (3) | 0.022 (3) | 0.020 (3) | 0.000 | 0.003 (2) | 0.000 |
N3 | 0.025 (3) | 0.008 (2) | 0.021 (3) | 0.000 | 0.009 (2) | 0.000 |
N4 | 0.019 (3) | 0.012 (3) | 0.027 (3) | 0.000 | 0.007 (2) | 0.000 |
C1 | 0.025 (2) | 0.024 (2) | 0.021 (2) | −0.0027 (19) | 0.0125 (17) | 0.0033 (18) |
C2 | 0.021 (2) | 0.047 (3) | 0.0174 (19) | 0.006 (2) | 0.0085 (17) | 0.007 (2) |
C3 | 0.027 (2) | 0.041 (3) | 0.030 (2) | −0.001 (2) | 0.0096 (19) | −0.002 (2) |
C4 | 0.034 (3) | 0.060 (3) | 0.043 (3) | 0.007 (3) | 0.022 (2) | −0.007 (3) |
C5 | 0.027 (3) | 0.053 (3) | 0.053 (3) | 0.008 (2) | 0.013 (2) | 0.004 (3) |
C6 | 0.025 (2) | 0.049 (3) | 0.029 (2) | 0.007 (2) | −0.001 (2) | 0.002 (2) |
C7 | 0.031 (2) | 0.039 (3) | 0.038 (3) | 0.009 (2) | 0.007 (2) | 0.002 (2) |
C8 | 0.049 (4) | 0.059 (4) | 0.058 (4) | −0.015 (3) | 0.019 (3) | −0.015 (3) |
C9 | 0.035 (3) | 0.035 (3) | 0.035 (3) | 0.010 (2) | 0.014 (2) | 0.002 (2) |
C10 | 0.052 (3) | 0.055 (3) | 0.043 (3) | 0.009 (3) | 0.017 (3) | 0.019 (3) |
C11 | 0.063 (4) | 0.045 (3) | 0.069 (4) | 0.023 (3) | 0.023 (3) | 0.011 (3) |
C12 | 0.0205 (19) | 0.016 (2) | 0.0203 (19) | −0.0011 (17) | 0.0063 (16) | −0.0041 (17) |
C13 | 0.019 (2) | 0.031 (2) | 0.021 (2) | −0.0036 (17) | 0.0056 (16) | 0.0027 (18) |
C14 | 0.019 (2) | 0.037 (2) | 0.038 (3) | −0.0023 (18) | 0.0010 (19) | 0.001 (2) |
C15 | 0.021 (2) | 0.086 (5) | 0.043 (3) | −0.015 (3) | 0.010 (2) | 0.001 (3) |
C16 | 0.052 (4) | 0.048 (3) | 0.052 (3) | −0.020 (3) | −0.001 (3) | 0.018 (3) |
C17 | 0.037 (3) | 0.034 (3) | 0.045 (3) | −0.005 (2) | 0.007 (2) | −0.010 (2) |
C18 | 0.033 (3) | 0.038 (3) | 0.041 (3) | 0.005 (2) | 0.006 (2) | −0.003 (2) |
C19 | 0.042 (3) | 0.043 (3) | 0.081 (5) | 0.011 (3) | −0.012 (3) | −0.014 (3) |
C20 | 0.026 (2) | 0.046 (3) | 0.028 (2) | −0.005 (2) | 0.0019 (19) | 0.009 (2) |
C21 | 0.050 (3) | 0.084 (5) | 0.033 (3) | −0.031 (3) | −0.001 (2) | 0.016 (3) |
C22 | 0.031 (3) | 0.051 (3) | 0.057 (4) | −0.013 (2) | −0.012 (2) | 0.006 (3) |
C23 | 0.025 (2) | 0.028 (3) | 0.024 (2) | 0.001 (2) | 0.013 (2) | −0.001 (2) |
C24 | 0.037 (3) | 0.015 (2) | 0.033 (3) | −0.001 (2) | 0.022 (2) | 0.000 (2) |
C25 | 0.024 (3) | 0.014 (3) | 0.025 (3) | 0.000 | 0.004 (3) | 0.000 |
C26 | 0.026 (3) | 0.018 (3) | 0.021 (3) | 0.000 | 0.010 (3) | 0.000 |
C27 | 0.034 (3) | 0.015 (2) | 0.035 (3) | 0.003 (2) | 0.024 (2) | 0.000 (2) |
C28 | 0.036 (3) | 0.008 (2) | 0.027 (2) | −0.0006 (18) | 0.017 (2) | 0.0015 (18) |
C29 | 0.026 (2) | 0.024 (3) | 0.031 (3) | 0.001 (2) | 0.018 (2) | 0.001 (2) |
C30 | 0.033 (3) | 0.016 (2) | 0.027 (2) | 0.0001 (19) | 0.013 (2) | 0.003 (2) |
C31 | 0.022 (3) | 0.012 (3) | 0.027 (3) | 0.000 | 0.008 (3) | 0.000 |
C32 | 0.025 (3) | 0.014 (3) | 0.020 (3) | 0.000 | 0.010 (3) | 0.000 |
C33 | 0.037 (3) | 0.020 (3) | 0.021 (2) | 0.000 (2) | 0.012 (2) | −0.0057 (19) |
C34 | 0.040 (3) | 0.007 (2) | 0.027 (2) | −0.0002 (18) | 0.020 (2) | 0.0025 (18) |
C35 | 0.049 (4) | 0.085 (5) | 0.090 (6) | −0.005 (4) | 0.017 (4) | 0.017 (5) |
C36 | 0.053 (4) | 0.040 (3) | 0.091 (5) | −0.013 (3) | 0.008 (4) | 0.016 (3) |
Ni1—S1 | 2.4288 (10) | C10—H10A | 0.9700 |
Ni1—S1i | 2.4288 (10) | C10—H10B | 0.9700 |
Ni1—S2i | 2.4305 (10) | C10—H10C | 0.9700 |
Ni1—S2 | 2.4305 (10) | C11—H11A | 0.9700 |
Ni1—N1 | 2.123 (5) | C11—H11B | 0.9700 |
Ni1—N2ii | 2.102 (6) | C11—H11C | 0.9700 |
Ni2—S3 | 2.4283 (10) | C13—C18 | 1.535 (7) |
Ni2—S4 | 2.4628 (10) | C13—C14 | 1.530 (6) |
Ni2—N3 | 2.101 (5) | C13—H13 | 0.9900 |
Ni2—N4ii | 2.124 (5) | C14—C15 | 1.520 (7) |
Ni2—S3iii | 2.4283 (10) | C14—C20 | 1.551 (7) |
Ni2—S4iii | 2.4628 (10) | C14—C19 | 1.506 (8) |
Cl1—C35 | 1.778 (9) | C15—C16 | 1.545 (9) |
Cl2—C35 | 1.699 (9) | C15—H15A | 0.9800 |
Cl3—C35 | 1.745 (8) | C15—H15B | 0.9800 |
Cl4—C36 | 1.762 (8) | C16—C17 | 1.504 (8) |
Cl5—C36 | 1.716 (7) | C16—H16A | 0.9800 |
Cl6—C36 | 1.765 (7) | C16—H16B | 0.9800 |
S1—C1 | 1.695 (4) | C17—C20 | 1.539 (8) |
S2—C1 | 1.701 (4) | C17—C18 | 1.564 (7) |
O1—C1 | 1.319 (6) | C17—H17 | 0.9900 |
S3—C12 | 1.679 (4) | C18—H18A | 0.9800 |
S4—C12 | 1.688 (4) | C18—H18B | 0.9800 |
O1—C2 | 1.440 (5) | C19—H19A | 0.9700 |
O2—C12 | 1.339 (5) | C19—H19B | 0.9700 |
O2—C13 | 1.466 (5) | C19—H19C | 0.9700 |
N1—C23 | 1.341 (6) | C20—C22 | 1.517 (7) |
N1—C23i | 1.341 (6) | C20—C21 | 1.505 (7) |
N2—C28 | 1.327 (5) | C21—H21A | 0.9700 |
N2—C28i | 1.327 (5) | C21—H21B | 0.9700 |
N2—Ni1iv | 2.102 (6) | C21—H21C | 0.9700 |
N3—C29 | 1.359 (5) | C22—H22A | 0.9700 |
N3—C29iii | 1.359 (5) | C22—H22B | 0.9700 |
N4—C34iii | 1.328 (5) | C22—H22C | 0.9700 |
N4—C34 | 1.328 (5) | C23—C24 | 1.370 (7) |
N4—Ni2iv | 2.124 (5) | C23—H23 | 0.9400 |
C2—C3 | 1.535 (7) | C24—C25 | 1.397 (6) |
C2—C7 | 1.540 (7) | C24—H24 | 0.9400 |
C2—H2 | 0.9900 | C25—C24i | 1.397 (6) |
C3—C8 | 1.520 (8) | C25—C26 | 1.499 (9) |
C3—C9 | 1.568 (7) | C26—C27 | 1.388 (6) |
C3—C4 | 1.522 (7) | C26—C27i | 1.388 (6) |
C4—C5 | 1.557 (8) | C27—C28 | 1.404 (6) |
C4—H4A | 0.9800 | C27—H27 | 0.9400 |
C4—H4B | 0.9800 | C28—H28 | 0.9400 |
C5—C6 | 1.535 (7) | C29—C30 | 1.356 (7) |
C5—H5A | 0.9800 | C29—H29 | 0.9400 |
C5—H5B | 0.9800 | C30—C31 | 1.395 (6) |
C6—C7 | 1.519 (7) | C30—H30 | 0.9400 |
C6—C9 | 1.569 (8) | C31—C30iii | 1.395 (6) |
C6—H6 | 0.9900 | C31—C32 | 1.477 (8) |
C7—H7A | 0.9800 | C32—C33 | 1.390 (6) |
C7—H7B | 0.9800 | C32—C33iii | 1.390 (6) |
C8—H8A | 0.9700 | C33—C34 | 1.388 (7) |
C8—H8B | 0.9700 | C33—H33 | 0.9400 |
C8—H8C | 0.9700 | C34—H34 | 0.9400 |
C9—C10 | 1.501 (7) | C35—H35 | 0.9900 |
C9—C11 | 1.514 (8) | C36—H36 | 0.9900 |
S1—Ni1—S2 | 74.05 (3) | O2—C12—S4 | 124.0 (3) |
S1—Ni1—S1i | 176.64 (7) | O2—C12—S3 | 115.1 (3) |
S1—Ni1—S2i | 105.80 (3) | S4—C12—S3 | 120.8 (2) |
S2i—Ni1—S2 | 175.03 (7) | O2—C13—C18 | 113.3 (4) |
S3—Ni2—S4 | 73.54 (3) | O2—C13—C14 | 108.5 (3) |
S3—Ni2—S3iii | 174.96 (7) | C18—C13—C14 | 104.6 (4) |
S3—Ni2—S4iii | 106.36 (3) | O2—C13—H13 | 110.1 |
S4iii—Ni2—S4 | 177.74 (7) | C18—C13—H13 | 110.1 |
N2ii—Ni1—N1 | 180 | C14—C13—H13 | 110.1 |
N2ii—Ni1—S1 | 91.68 (3) | C15—C14—C20 | 101.6 (4) |
N1—Ni1—S1 | 88.32 (3) | C15—C14—C19 | 114.3 (5) |
N2ii—Ni1—S1i | 91.68 (3) | C20—C14—C19 | 117.9 (5) |
N1—Ni1—S1i | 88.32 (3) | C15—C14—C13 | 107.0 (4) |
N2ii—Ni1—S2i | 92.48 (3) | C20—C14—C13 | 100.7 (4) |
N1—Ni1—S2i | 87.52 (3) | C19—C14—C13 | 113.7 (4) |
S1i—Ni1—S2 | 105.80 (3) | C14—C15—C16 | 104.8 (4) |
S1i—Ni1—S2i | 74.05 (3) | C14—C15—H15A | 110.8 |
N2ii—Ni1—S2 | 92.48 (3) | C16—C15—H15A | 110.8 |
N1—Ni1—S2 | 87.52 (3) | C14—C15—H15B | 110.8 |
N3—Ni2—N4ii | 180 | C16—C15—H15B | 110.8 |
N3—Ni2—S3 | 92.52 (3) | H15A—C15—H15B | 108.9 |
N4ii—Ni2—S3 | 87.48 (3) | C17—C16—C15 | 102.1 (4) |
N3—Ni2—S3iii | 92.52 (3) | C17—C16—H16A | 111.3 |
N4ii—Ni2—S3iii | 87.48 (3) | C15—C16—H16A | 111.3 |
N3—Ni2—S4iii | 91.13 (3) | C17—C16—H16B | 111.3 |
N4ii—Ni2—S4iii | 88.87 (3) | C15—C16—H16B | 111.3 |
S3iii—Ni2—S4iii | 73.54 (3) | H16A—C16—H16B | 109.2 |
N3—Ni2—S4 | 91.13 (3) | C16—C17—C20 | 104.2 (5) |
N4ii—Ni2—S4 | 88.87 (3) | C16—C17—C18 | 106.9 (5) |
S3iii—Ni2—S4 | 106.36 (3) | C20—C17—C18 | 101.5 (4) |
C1—S1—Ni1 | 83.30 (16) | C16—C17—H17 | 114.3 |
C1—S2—Ni1 | 83.14 (15) | C20—C17—H17 | 114.3 |
C12—S3—Ni2 | 83.28 (14) | C18—C17—H17 | 114.3 |
C12—S4—Ni2 | 82.03 (14) | C13—C18—C17 | 102.1 (4) |
C1—O1—C2 | 121.8 (3) | C13—C18—H18A | 111.4 |
C12—O2—C13 | 121.9 (3) | C17—C18—H18A | 111.4 |
C23—N1—C23i | 116.3 (6) | C13—C18—H18B | 111.4 |
C23—N1—Ni1 | 121.9 (3) | C17—C18—H18B | 111.4 |
C23i—N1—Ni1 | 121.9 (3) | H18A—C18—H18B | 109.2 |
C28—N2—C28i | 118.1 (5) | C14—C19—H19A | 109.5 |
C28—N2—Ni1iv | 120.9 (3) | C14—C19—H19B | 109.5 |
C28i—N2—Ni1iv | 120.9 (3) | H19A—C19—H19B | 109.5 |
C29—N3—C29iii | 115.6 (5) | C14—C19—H19C | 109.5 |
C29—N3—Ni2 | 122.2 (3) | H19A—C19—H19C | 109.5 |
C29iii—N3—Ni2 | 122.2 (3) | H19B—C19—H19C | 109.5 |
C34iii—N4—C34 | 118.8 (5) | C22—C20—C14 | 113.8 (5) |
C34iii—N4—Ni2iv | 120.6 (3) | C22—C20—C17 | 113.8 (5) |
C34—N4—Ni2iv | 120.6 (3) | C14—C20—C17 | 93.3 (4) |
O1—C1—S1 | 125.2 (3) | C22—C20—C21 | 105.4 (5) |
O1—C1—S2 | 115.8 (3) | C14—C20—C21 | 115.0 (5) |
S1—C1—S2 | 119.0 (3) | C17—C20—C21 | 115.7 (5) |
O1—C2—C3 | 109.4 (4) | C20—C21—H21A | 109.5 |
O1—C2—C7 | 111.2 (4) | C20—C21—H21B | 109.5 |
C3—C2—C7 | 104.6 (4) | H21A—C21—H21B | 109.5 |
O1—C2—H2 | 110.5 | C20—C21—H21C | 109.5 |
C3—C2—H2 | 110.5 | H21A—C21—H21C | 109.5 |
C7—C2—H2 | 110.5 | H21B—C21—H21C | 109.5 |
C2—C3—C8 | 112.9 (4) | C20—C22—H22A | 109.5 |
C2—C3—C9 | 100.3 (4) | C20—C22—H22B | 109.5 |
C8—C3—C9 | 118.2 (5) | H22A—C22—H22B | 109.5 |
C2—C3—C4 | 108.0 (4) | C20—C22—H22C | 109.5 |
C8—C3—C4 | 114.1 (4) | H22A—C22—H22C | 109.5 |
C9—C3—C4 | 101.8 (4) | H22B—C22—H22C | 109.5 |
C5—C4—C3 | 104.6 (4) | N1—C23—C24 | 124.2 (5) |
C5—C4—H4A | 110.8 | N1—C23—H23 | 117.9 |
C3—C4—H4A | 110.8 | C24—C23—H23 | 117.9 |
C5—C4—H4B | 110.8 | C23—C24—C25 | 118.8 (5) |
C3—C4—H4B | 110.8 | C23—C24—H24 | 120.6 |
H4A—C4—H4B | 108.9 | C25—C24—H24 | 120.6 |
C6—C5—C4 | 102.0 (4) | C24—C25—C24i | 117.7 (6) |
C6—C5—H5A | 111.4 | C24—C25—C26 | 121.1 (3) |
C4—C5—H5A | 111.4 | C24i—C25—C26 | 121.1 (3) |
C6—C5—H5B | 111.4 | C27—C26—C27i | 117.3 (6) |
C4—C5—H5B | 111.4 | C27—C26—C25 | 121.4 (3) |
H5A—C5—H5B | 109.2 | C27i—C26—C25 | 121.4 (3) |
C5—C6—C7 | 107.0 (4) | C28—C27—C26 | 119.4 (4) |
C5—C6—C9 | 102.9 (4) | C28—C27—H27 | 120.3 |
C7—C6—C9 | 103.0 (4) | C26—C27—H27 | 120.3 |
C5—C6—H6 | 114.2 | N2—C28—C27 | 122.9 (4) |
C7—C6—H6 | 114.2 | N2—C28—H28 | 118.6 |
C9—C6—H6 | 114.2 | C27—C28—H28 | 118.6 |
C6—C7—C2 | 102.7 (4) | C30—C29—N3 | 123.4 (4) |
C6—C7—H7A | 111.2 | C30—C29—H29 | 118.3 |
C2—C7—H7A | 111.2 | N3—C29—H29 | 118.3 |
C6—C7—H7B | 111.2 | C29—C30—C31 | 121.1 (5) |
C2—C7—H7B | 111.2 | C29—C30—H30 | 119.4 |
H7A—C7—H7B | 109.1 | C31—C30—H30 | 119.4 |
C3—C8—H8A | 109.5 | C30—C31—C30iii | 115.3 (6) |
C3—C8—H8B | 109.5 | C30—C31—C32 | 122.3 (3) |
H8A—C8—H8B | 109.5 | C30iii—C31—C32 | 122.3 (3) |
C3—C8—H8C | 109.5 | C33—C32—C33iii | 115.8 (6) |
H8A—C8—H8C | 109.5 | C33—C32—C31 | 122.1 (3) |
H8B—C8—H8C | 109.5 | C33iii—C32—C31 | 122.1 (3) |
C10—C9—C3 | 114.6 (4) | C32—C33—C34 | 120.7 (5) |
C10—C9—C11 | 107.4 (5) | C32—C33—H33 | 119.6 |
C3—C9—C11 | 114.6 (5) | C34—C33—H33 | 119.6 |
C10—C9—C6 | 113.5 (5) | N4—C34—C33 | 122.0 (4) |
C3—C9—C6 | 92.3 (4) | N4—C34—H34 | 119.0 |
C11—C9—C6 | 114.2 (5) | C33—C34—H34 | 119.0 |
C9—C10—H10A | 109.5 | Cl3—C35—Cl2 | 110.2 (5) |
C9—C10—H10B | 109.5 | Cl3—C35—Cl1 | 107.4 (4) |
H10A—C10—H10B | 109.5 | Cl2—C35—Cl1 | 112.8 (5) |
C9—C10—H10C | 109.5 | Cl3—C35—H35 | 108.8 |
H10A—C10—H10C | 109.5 | Cl2—C35—H35 | 108.8 |
H10B—C10—H10C | 109.5 | Cl1—C35—H35 | 108.8 |
C9—C11—H11A | 109.5 | Cl5—C36—Cl6 | 110.9 (4) |
C9—C11—H11B | 109.5 | Cl5—C36—Cl4 | 109.9 (4) |
H11A—C11—H11B | 109.5 | Cl6—C36—Cl4 | 109.3 (4) |
C9—C11—H11C | 109.5 | Cl5—C36—H36 | 108.9 |
H11A—C11—H11C | 109.5 | Cl6—C36—H36 | 108.9 |
H11B—C11—H11C | 109.5 | Cl4—C36—H36 | 108.9 |
N2ii—Ni1—S1—C1 | −96.54 (17) | C5—C6—C9—C11 | 62.8 (6) |
N1—Ni1—S1—C1 | 83.46 (17) | C7—C6—C9—C11 | 173.9 (5) |
S2i—Ni1—S1—C1 | 170.40 (17) | C13—O2—C12—S4 | −2.0 (6) |
S2—Ni1—S1—C1 | −4.44 (17) | C13—O2—C12—S3 | 178.8 (3) |
N2ii—Ni1—S2—C1 | 95.46 (17) | Ni2—S4—C12—O2 | 175.3 (4) |
N1—Ni1—S2—C1 | −84.54 (17) | Ni2—S4—C12—S3 | −5.5 (3) |
S1—Ni1—S2—C1 | 4.43 (17) | Ni2—S3—C12—O2 | −175.2 (4) |
S1i—Ni1—S2—C1 | −172.09 (17) | Ni2—S3—C12—S4 | 5.5 (3) |
N3—Ni2—S3—C12 | −93.82 (16) | C12—O2—C13—C18 | −79.6 (5) |
N4ii—Ni2—S3—C12 | 86.18 (16) | C12—O2—C13—C14 | 164.7 (4) |
S4iii—Ni2—S3—C12 | 174.26 (16) | O2—C13—C14—C15 | 52.4 (5) |
S4—Ni2—S3—C12 | −3.39 (16) | C18—C13—C14—C15 | −68.8 (5) |
N3—Ni2—S4—C12 | 95.67 (16) | O2—C13—C14—C20 | 158.2 (4) |
N4ii—Ni2—S4—C12 | −84.33 (16) | C18—C13—C14—C20 | 37.0 (5) |
S3—Ni2—S4—C12 | 3.38 (16) | O2—C13—C14—C19 | −74.7 (6) |
S3iii—Ni2—S4—C12 | −171.37 (16) | C18—C13—C14—C19 | 164.1 (5) |
S1—Ni1—N1—C23 | 51.2 (2) | C20—C14—C15—C16 | −34.6 (5) |
S1i—Ni1—N1—C23 | −128.8 (2) | C19—C14—C15—C16 | −162.7 (5) |
S2i—Ni1—N1—C23 | −54.7 (2) | C13—C14—C15—C16 | 70.6 (5) |
S2—Ni1—N1—C23 | 125.3 (2) | C14—C15—C16—C17 | 0.3 (6) |
S1—Ni1—N1—C23i | −128.8 (2) | C15—C16—C17—C20 | 34.9 (6) |
S1i—Ni1—N1—C23i | 51.2 (2) | C15—C16—C17—C18 | −72.0 (5) |
S2i—Ni1—N1—C23i | 125.3 (2) | O2—C13—C18—C17 | −119.3 (4) |
S2—Ni1—N1—C23i | −54.7 (2) | C14—C13—C18—C17 | −1.3 (5) |
S3—Ni2—N3—C29 | 143.2 (3) | C16—C17—C18—C13 | 73.6 (5) |
S3iii—Ni2—N3—C29 | −36.8 (3) | C20—C17—C18—C13 | −35.2 (5) |
S4iii—Ni2—N3—C29 | −110.3 (3) | C15—C14—C20—C22 | −64.7 (6) |
S4—Ni2—N3—C29 | 69.7 (3) | C19—C14—C20—C22 | 61.0 (6) |
S3—Ni2—N3—C29iii | −36.8 (3) | C13—C14—C20—C22 | −174.7 (5) |
S3iii—Ni2—N3—C29iii | 143.2 (3) | C15—C14—C20—C17 | 53.1 (4) |
S4iii—Ni2—N3—C29iii | 69.7 (3) | C19—C14—C20—C17 | 178.8 (5) |
S4—Ni2—N3—C29iii | −110.3 (3) | C13—C14—C20—C17 | −56.9 (4) |
C2—O1—C1—S1 | 19.0 (7) | C15—C14—C20—C21 | 173.5 (5) |
C2—O1—C1—S2 | −160.9 (4) | C19—C14—C20—C21 | −60.7 (7) |
Ni1—S1—C1—O1 | −173.0 (5) | C13—C14—C20—C21 | 63.5 (6) |
Ni1—S1—C1—S2 | 7.0 (3) | C16—C17—C20—C22 | 63.3 (6) |
Ni1—S2—C1—O1 | 173.0 (4) | C18—C17—C20—C22 | 174.1 (5) |
Ni1—S2—C1—S1 | −7.0 (3) | C16—C17—C20—C14 | −54.6 (5) |
C1—O1—C2—C3 | 112.4 (5) | C18—C17—C20—C14 | 56.3 (4) |
C1—O1—C2—C7 | −132.6 (5) | C16—C17—C20—C21 | −174.5 (5) |
O1—C2—C3—C8 | −75.9 (5) | C18—C17—C20—C21 | −63.6 (6) |
C7—C2—C3—C8 | 165.0 (4) | C23i—N1—C23—C24 | −0.2 (4) |
O1—C2—C3—C9 | 157.4 (4) | Ni1—N1—C23—C24 | 179.8 (4) |
C7—C2—C3—C9 | 38.3 (4) | N1—C23—C24—C25 | 0.3 (7) |
O1—C2—C3—C4 | 51.3 (5) | C23—C24—C25—C24i | −0.2 (3) |
C7—C2—C3—C4 | −67.8 (5) | C23—C24—C25—C26 | 179.8 (3) |
C2—C3—C4—C5 | 68.8 (5) | C24—C25—C26—C27 | 19.5 (3) |
C8—C3—C4—C5 | −164.7 (5) | C24i—C25—C26—C27 | −160.5 (3) |
C9—C3—C4—C5 | −36.2 (5) | C24—C25—C26—C27i | −160.5 (3) |
C3—C4—C5—C6 | 0.5 (6) | C24i—C25—C26—C27i | 19.5 (3) |
C4—C5—C6—C7 | −72.6 (5) | C27i—C26—C27—C28 | 1.0 (3) |
C4—C5—C6—C9 | 35.5 (5) | C25—C26—C27—C28 | −179.0 (3) |
C5—C6—C7—C2 | 74.2 (5) | C28i—N2—C28—C27 | 1.1 (4) |
C9—C6—C7—C2 | −33.9 (5) | Ni1iv—N2—C28—C27 | −178.9 (4) |
O1—C2—C7—C6 | −120.8 (4) | C26—C27—C28—N2 | −2.2 (7) |
C3—C2—C7—C6 | −2.8 (5) | C29iii—N3—C29—C30 | −0.2 (4) |
C2—C3—C9—C10 | 61.3 (5) | Ni2—N3—C29—C30 | 179.8 (4) |
C8—C3—C9—C10 | −61.8 (6) | N3—C29—C30—C31 | 0.4 (8) |
C4—C3—C9—C10 | 172.3 (5) | C29—C30—C31—C30iii | −0.2 (4) |
C2—C3—C9—C11 | −173.8 (5) | C29—C30—C31—C32 | 179.8 (4) |
C8—C3—C9—C11 | 63.0 (6) | C30—C31—C32—C33 | −20.9 (3) |
C4—C3—C9—C11 | −62.8 (6) | C30iii—C31—C32—C33 | 159.1 (3) |
C2—C3—C9—C6 | −55.9 (4) | C30—C31—C32—C33iii | 159.1 (3) |
C8—C3—C9—C6 | −179.0 (5) | C30iii—C31—C32—C33iii | −20.9 (3) |
C4—C3—C9—C6 | 55.2 (4) | C33iii—C32—C33—C34 | −0.3 (4) |
C5—C6—C9—C10 | −173.8 (4) | C31—C32—C33—C34 | 179.7 (4) |
C7—C6—C9—C10 | −62.6 (6) | C34iii—N4—C34—C33 | −0.3 (4) |
C5—C6—C9—C3 | −55.6 (4) | Ni2iv—N4—C34—C33 | 179.7 (4) |
C7—C6—C9—C3 | 55.5 (4) | C32—C33—C34—N4 | 0.6 (7) |
Symmetry codes: (i) −x, y, −z−1; (ii) x, y+1, z; (iii) −x, y, −z; (iv) x, y−1, z. |