Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802004816/ob6113sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802004816/ob6113Isup2.hkl |
CCDC reference: 183759
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.009 Å
- R factor = 0.093
- wR factor = 0.271
- Data-to-parameter ratio = 20.5
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
RFACR_01 Alert C The value of the weighted R factor is > 0.25 Weighted R factor given 0.271 PLAT_371 Alert C Long C(sp2)-C(sp1) Bond C(4) - C(6) = 1.43 Ang.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check
Data collection: CrystalClear (Molecular Structure Corporation & Rigaku Corporation, 2001); cell refinement: CrystalClear; data reduction: TEXSAN (Molecular Structure Corporation & Rigaku Corporation, 2000); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: SHELXL97.
(C16H36N)2[Ni(C6N2S4)2] | Z = 1 |
Mr = 1000.33 | F(000) = 534 |
Triclinic, P1 | Dx = 1.260 Mg m−3 |
Hall symbol: -P 1 | Melting point: 521 K |
a = 8.252 (4) Å | Mo Kα radiation, λ = 0.71070 Å |
b = 12.012 (6) Å | Cell parameters from 4920 reflections |
c = 13.867 (6) Å | θ = 3.1–27.5° |
α = 76.26 (3)° | µ = 0.72 mm−1 |
β = 80.99 (3)° | T = 173 K |
γ = 89.69 (4)° | Plate, green–black |
V = 1317.9 (10) Å3 | 0.60 × 0.20 × 0.05 mm |
Rigaku/MSC Mercury CCD diffractometer | 5808 independent reflections |
Radiation source: Rigaku rotating anode | 4177 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.069 |
Detector resolution: 14.62 pixels mm-1 | θmax = 27.5°, θmin = 3.1° |
φ and ω scans | h = −10→9 |
Absorption correction: multi-scan (Jacobson, 1998) | k = −14→15 |
Tmin = 0.672, Tmax = 0.965 | l = −17→15 |
12833 measured reflections |
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)] = 0.093 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.271 | H-atom parameters constrained |
S = 1.11 | w = 1/[σ2(Fo2) + (0.1389P)2 + 1.6175P] where P = (Fo2 + 2Fc2)/3 |
5808 reflections | (Δ/σ)max < 0.001 |
283 parameters | Δρmax = 1.18 e Å−3 |
2 restraints | Δρmin = −0.97 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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 7.5493 (0.0056) x + 4.4900 (0.0085) y + 1.0143 (0.0069) z = 5.5125 (0.0065) * 0.0000 (0.0000) Ni1 * 0.1712 (0.0021) S1 * 0.1160 (0.0018) S2 * 0.1612 (0.0022) S3 * 0.1258 (0.0020) S4 * -0.1493 (0.0044) N1 * -0.0954 (0.0039) N2 * 0.1721 (0.0053) C1 * 0.1594 (0.0047) C2 * 0.0798 (0.0048) C3 * -0.0140 (0.0047) C4 * -0.0856 (0.0050) C5 * -0.0557 (0.0046) C6 * -0.1712 (0.0021) S1_$1 * -0.1160 (0.0018) S2_$1 * -0.1612 (0.0022) S3_$1 * -0.1258 (0.0020) S4_$1 * 0.1493 (0.0044) N1_$1 * 0.0954 (0.0039) N2_$1 * -0.1721 (0.0053) C1_$1 * -0.1594 (0.0047) C2_$1 * -0.0798 (0.0048) C3_$1 * 0.0140 (0.0047) C4_$1 * 0.0856 (0.0050) C5_$1 * 0.0557 (0.0046) C6_$1 Rms deviation of fitted atoms = 0.1202 Operators for generating equivalent atoms: $1 - x + 1, -y + 1, -z - 1 The terminal methyl group (C18A, H18A, H18B, H18C, H17A, H17B and C18B, H18D, H18E, H18F, H17C, H17D) of the tetrabutylammonium cation is disordered over two sites with 0.414 (15) and 0.586 (15) of occupancies, respectively. |
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 | Occ. (<1) | |
Ni1 | 0.5000 | 0.5000 | −0.5000 | 0.0387 (3) | |
S1 | 0.41910 (19) | 0.67241 (12) | −0.49230 (10) | 0.0495 (4) | |
S2 | 0.52337 (15) | 0.45060 (11) | −0.34088 (10) | 0.0417 (3) | |
S3 | 0.33232 (19) | 0.77528 (12) | −0.31158 (10) | 0.0475 (4) | |
S4 | 0.42873 (16) | 0.57436 (11) | −0.17466 (9) | 0.0408 (3) | |
N1 | 0.1635 (8) | 0.9510 (5) | −0.1395 (5) | 0.0703 (16) | |
N2 | 0.3226 (6) | 0.6484 (5) | 0.0696 (4) | 0.0594 (13) | |
N3 | 0.0163 (5) | 0.2592 (4) | −0.2869 (3) | 0.0401 (9) | |
C1 | 0.4068 (7) | 0.6646 (5) | −0.3650 (4) | 0.0446 (12) | |
C2 | 0.4522 (6) | 0.5709 (5) | −0.3009 (4) | 0.0398 (11) | |
C3 | 0.3462 (6) | 0.7062 (5) | −0.1895 (4) | 0.0435 (12) | |
C4 | 0.2933 (6) | 0.7561 (4) | −0.1087 (4) | 0.0410 (11) | |
C5 | 0.2220 (7) | 0.8636 (5) | −0.1250 (4) | 0.0486 (13) | |
C6 | 0.3096 (6) | 0.6967 (5) | −0.0088 (4) | 0.0431 (11) | |
C7 | −0.0628 (6) | 0.3749 (4) | −0.2997 (4) | 0.0448 (12) | |
H7A | −0.1501 | 0.3762 | −0.3415 | 0.054* | |
H7B | −0.1159 | 0.3833 | −0.2328 | 0.054* | |
C8 | 0.0535 (7) | 0.4767 (5) | −0.3476 (5) | 0.0497 (13) | |
H8A | 0.1021 | 0.4722 | −0.4164 | 0.060* | |
H8B | 0.1438 | 0.4751 | −0.3080 | 0.060* | |
C9 | −0.0363 (7) | 0.5882 (5) | −0.3520 (4) | 0.0512 (13) | |
H9A | −0.1341 | 0.5849 | −0.3846 | 0.061* | |
H9B | 0.0367 | 0.6522 | −0.3946 | 0.061* | |
C10 | −0.0910 (9) | 0.6134 (6) | −0.2493 (6) | 0.0695 (18) | |
H10A | −0.1711 | 0.5541 | −0.2086 | 0.104* | |
H10B | −0.1414 | 0.6885 | −0.2580 | 0.104* | |
H10C | 0.0044 | 0.6139 | −0.2153 | 0.104* | |
C11 | 0.1575 (6) | 0.2517 (5) | −0.2283 (4) | 0.0437 (12) | |
H11A | 0.2499 | 0.3011 | −0.2709 | 0.052* | |
H11B | 0.1947 | 0.1718 | −0.2147 | 0.052* | |
C12 | 0.1193 (7) | 0.2865 (5) | −0.1294 (4) | 0.0499 (13) | |
H12A | 0.0953 | 0.3691 | −0.1423 | 0.060* | |
H12B | 0.0207 | 0.2428 | −0.0882 | 0.060* | |
C13 | 0.2626 (8) | 0.2639 (6) | −0.0724 (5) | 0.0573 (15) | |
H13A | 0.3616 | 0.3061 | −0.1145 | 0.069* | |
H13B | 0.2849 | 0.1810 | −0.0584 | 0.069* | |
C14 | 0.2286 (10) | 0.3006 (8) | 0.0259 (5) | 0.082 (2) | |
H14A | 0.2106 | 0.3832 | 0.0121 | 0.122* | |
H14B | 0.3227 | 0.2833 | 0.0616 | 0.122* | |
H14C | 0.1304 | 0.2590 | 0.0676 | 0.122* | |
C15 | −0.1110 (6) | 0.1678 (4) | −0.2285 (4) | 0.0438 (12) | |
H15A | −0.1488 | 0.1844 | −0.1621 | 0.053* | |
H15B | −0.0565 | 0.0933 | −0.2162 | 0.053* | |
C16 | −0.2606 (8) | 0.1544 (6) | −0.2757 (6) | 0.0637 (17) | |
H16A | −0.3169 | 0.2283 | −0.2880 | 0.076* | |
H16B | −0.2247 | 0.1363 | −0.3417 | 0.076* | |
C17 | −0.3786 (9) | 0.0638 (7) | −0.2132 (6) | 0.082 (2) | |
H17A | −0.3481 | −0.0073 | −0.2349 | 0.099* | 0.414 (15) |
H17B | −0.4869 | 0.0843 | −0.2333 | 0.099* | 0.414 (15) |
H17C | −0.4673 | 0.0569 | −0.2521 | 0.099* | 0.586 (15) |
H17D | −0.4291 | 0.0906 | −0.1535 | 0.099* | 0.586 (15) |
C18A | −0.408 (2) | 0.0306 (15) | −0.0977 (8) | 0.066 (5) | 0.414 (15) |
H18A | −0.4893 | −0.0328 | −0.0735 | 0.099* | 0.414 (15) |
H18B | −0.4477 | 0.0967 | −0.0721 | 0.099* | 0.414 (15) |
H18C | −0.3042 | 0.0066 | −0.0738 | 0.099* | 0.414 (15) |
C18B | −0.3180 (19) | −0.0532 (10) | −0.1769 (13) | 0.103 (7) | 0.586 (15) |
H18D | −0.2729 | −0.0838 | −0.2346 | 0.155* | 0.586 (15) |
H18E | −0.4091 | −0.1034 | −0.1359 | 0.155* | 0.586 (15) |
H18F | −0.2321 | −0.0494 | −0.1362 | 0.155* | 0.586 (15) |
C19 | 0.0797 (7) | 0.2417 (5) | −0.3912 (4) | 0.0490 (13) | |
H19A | −0.0113 | 0.2542 | −0.4310 | 0.059* | |
H19B | 0.1665 | 0.3010 | −0.4247 | 0.059* | |
C20 | 0.1476 (9) | 0.1267 (6) | −0.3937 (5) | 0.0583 (15) | |
H20A | 0.0628 | 0.0654 | −0.3621 | 0.070* | |
H20B | 0.2425 | 0.1130 | −0.3572 | 0.070* | |
C21 | 0.2020 (9) | 0.1288 (6) | −0.5073 (5) | 0.0691 (18) | |
H21A | 0.1059 | 0.1432 | −0.5427 | 0.083* | |
H21B | 0.2842 | 0.1920 | −0.5382 | 0.083* | |
C22 | 0.2746 (13) | 0.0173 (8) | −0.5193 (7) | 0.099 (3) | |
H22A | 0.3604 | −0.0019 | −0.4771 | 0.148* | |
H22B | 0.3224 | 0.0243 | −0.5898 | 0.148* | |
H22C | 0.1885 | −0.0434 | −0.4987 | 0.148* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0354 (5) | 0.0413 (5) | 0.0387 (5) | −0.0001 (4) | −0.0044 (4) | −0.0092 (4) |
S1 | 0.0677 (9) | 0.0420 (7) | 0.0380 (7) | 0.0057 (6) | −0.0086 (6) | −0.0078 (5) |
S2 | 0.0412 (7) | 0.0455 (7) | 0.0402 (7) | 0.0087 (5) | −0.0092 (5) | −0.0120 (5) |
S3 | 0.0630 (9) | 0.0376 (7) | 0.0419 (7) | 0.0073 (6) | −0.0099 (6) | −0.0087 (5) |
S4 | 0.0445 (7) | 0.0424 (7) | 0.0365 (7) | 0.0071 (5) | −0.0091 (5) | −0.0100 (5) |
N1 | 0.083 (4) | 0.049 (3) | 0.082 (4) | 0.016 (3) | −0.021 (3) | −0.015 (3) |
N2 | 0.061 (3) | 0.069 (4) | 0.046 (3) | 0.012 (3) | −0.006 (2) | −0.011 (2) |
N3 | 0.039 (2) | 0.040 (2) | 0.041 (2) | 0.0038 (17) | −0.0075 (17) | −0.0068 (18) |
C1 | 0.048 (3) | 0.040 (3) | 0.050 (3) | 0.004 (2) | −0.009 (2) | −0.018 (2) |
C2 | 0.037 (2) | 0.051 (3) | 0.033 (2) | −0.004 (2) | 0.0027 (19) | −0.017 (2) |
C3 | 0.035 (3) | 0.048 (3) | 0.045 (3) | 0.001 (2) | −0.004 (2) | −0.006 (2) |
C4 | 0.040 (3) | 0.039 (3) | 0.044 (3) | 0.002 (2) | −0.007 (2) | −0.009 (2) |
C5 | 0.052 (3) | 0.047 (3) | 0.049 (3) | 0.005 (2) | −0.011 (2) | −0.015 (2) |
C6 | 0.041 (3) | 0.048 (3) | 0.042 (3) | 0.008 (2) | 0.000 (2) | −0.018 (2) |
C7 | 0.043 (3) | 0.040 (3) | 0.048 (3) | 0.009 (2) | −0.007 (2) | −0.005 (2) |
C8 | 0.041 (3) | 0.049 (3) | 0.055 (3) | 0.003 (2) | −0.005 (2) | −0.006 (3) |
C9 | 0.055 (3) | 0.045 (3) | 0.050 (3) | 0.002 (2) | −0.009 (3) | −0.003 (2) |
C10 | 0.081 (5) | 0.048 (4) | 0.079 (5) | −0.003 (3) | 0.001 (4) | −0.022 (3) |
C11 | 0.038 (3) | 0.044 (3) | 0.049 (3) | 0.005 (2) | −0.012 (2) | −0.008 (2) |
C12 | 0.045 (3) | 0.053 (3) | 0.053 (3) | 0.002 (2) | −0.012 (2) | −0.013 (3) |
C13 | 0.058 (3) | 0.066 (4) | 0.052 (3) | −0.001 (3) | −0.022 (3) | −0.012 (3) |
C14 | 0.073 (5) | 0.120 (7) | 0.053 (4) | −0.019 (4) | −0.009 (3) | −0.024 (4) |
C15 | 0.039 (3) | 0.041 (3) | 0.052 (3) | 0.000 (2) | −0.009 (2) | −0.012 (2) |
C16 | 0.062 (4) | 0.050 (3) | 0.081 (5) | 0.000 (3) | −0.031 (3) | −0.006 (3) |
C17 | 0.057 (4) | 0.105 (6) | 0.087 (5) | −0.025 (4) | −0.019 (4) | −0.023 (5) |
C18A | 0.068 (10) | 0.066 (11) | 0.054 (9) | −0.006 (8) | −0.003 (7) | 0.002 (7) |
C18B | 0.100 (11) | 0.077 (10) | 0.113 (13) | −0.033 (8) | −0.037 (10) | 0.028 (9) |
C19 | 0.051 (3) | 0.055 (3) | 0.039 (3) | 0.001 (2) | −0.004 (2) | −0.008 (2) |
C20 | 0.072 (4) | 0.057 (4) | 0.047 (3) | 0.013 (3) | −0.007 (3) | −0.017 (3) |
C21 | 0.074 (4) | 0.063 (4) | 0.067 (4) | 0.001 (3) | 0.004 (3) | −0.019 (3) |
C22 | 0.128 (8) | 0.085 (6) | 0.088 (6) | 0.022 (5) | 0.001 (5) | −0.044 (5) |
Ni1—S1 | 2.1940 (18) | C12—H12B | 0.9900 |
Ni1—S1i | 2.1940 (18) | C13—C14 | 1.515 (9) |
Ni1—S2 | 2.1836 (16) | C13—H13A | 0.9900 |
Ni1—S2i | 2.1836 (16) | C13—H13B | 0.9900 |
S1—C1 | 1.732 (6) | C14—H14A | 0.9800 |
S2—C2 | 1.735 (5) | C14—H14B | 0.9800 |
S3—C3 | 1.720 (5) | C14—H14C | 0.9800 |
S3—C1 | 1.735 (5) | C15—C16 | 1.512 (8) |
S4—C3 | 1.701 (6) | C15—H15A | 0.9900 |
S4—C2 | 1.742 (5) | C15—H15B | 0.9900 |
N1—C5 | 1.140 (8) | C16—C17 | 1.478 (10) |
N2—C6 | 1.125 (7) | C16—H16A | 0.9900 |
N3—C15 | 1.512 (6) | C16—H16B | 0.9900 |
N3—C11 | 1.512 (6) | C17—C18B | 1.487 (9) |
N3—C7 | 1.516 (7) | C17—C18A | 1.535 (9) |
N3—C19 | 1.522 (7) | C17—H17A | 0.9900 |
C1—C2 | 1.350 (8) | C17—H17B | 0.9900 |
C3—C4 | 1.403 (8) | C17—H17C | 0.9900 |
C4—C5 | 1.400 (8) | C17—H17D | 0.9900 |
C4—C6 | 1.426 (7) | C18A—H18A | 0.9800 |
C7—C8 | 1.512 (7) | C18A—H18B | 0.9800 |
C7—H7A | 0.9900 | C18A—H18C | 0.9800 |
C7—H7B | 0.9900 | C18B—H18D | 0.9800 |
C8—C9 | 1.519 (8) | C18B—H18E | 0.9800 |
C8—H8A | 0.9900 | C18B—H18F | 0.9800 |
C8—H8B | 0.9900 | C19—C20 | 1.494 (8) |
C9—C10 | 1.526 (9) | C19—H19A | 0.9900 |
C9—H9A | 0.9900 | C19—H19B | 0.9900 |
C9—H9B | 0.9900 | C20—C21 | 1.563 (9) |
C10—H10A | 0.9800 | C20—H20A | 0.9900 |
C10—H10B | 0.9800 | C20—H20B | 0.9900 |
C10—H10C | 0.9800 | C21—C22 | 1.498 (11) |
C11—C12 | 1.514 (8) | C21—H21A | 0.9900 |
C11—H11A | 0.9900 | C21—H21B | 0.9900 |
C11—H11B | 0.9900 | C22—H22A | 0.9800 |
C12—C13 | 1.511 (8) | C22—H22B | 0.9800 |
C12—H12A | 0.9900 | C22—H22C | 0.9800 |
S2—Ni1—S2i | 180.0 | C14—C13—H13A | 109.3 |
S2—Ni1—S1i | 86.71 (6) | C12—C13—H13B | 109.3 |
S2i—Ni1—S1i | 93.29 (6) | C14—C13—H13B | 109.3 |
S2—Ni1—S1 | 93.29 (6) | H13A—C13—H13B | 108.0 |
S2i—Ni1—S1 | 86.71 (6) | C13—C14—H14A | 109.5 |
S1i—Ni1—S1 | 180.0 | C13—C14—H14B | 109.5 |
C1—S1—Ni1 | 101.25 (19) | H14A—C14—H14B | 109.5 |
C2—S2—Ni1 | 101.39 (18) | C13—C14—H14C | 109.5 |
C3—S3—C1 | 96.2 (3) | H14A—C14—H14C | 109.5 |
C3—S4—C2 | 96.0 (3) | H14B—C14—H14C | 109.5 |
C15—N3—C11 | 107.5 (4) | N3—C15—C16 | 117.1 (5) |
C15—N3—C7 | 108.5 (4) | N3—C15—H15A | 108.0 |
C11—N3—C7 | 112.2 (4) | C16—C15—H15A | 108.0 |
C15—N3—C19 | 111.7 (4) | N3—C15—H15B | 108.0 |
C11—N3—C19 | 109.2 (4) | C16—C15—H15B | 108.0 |
C7—N3—C19 | 107.8 (4) | H15A—C15—H15B | 107.3 |
C2—C1—S1 | 121.9 (4) | C17—C16—C15 | 113.4 (6) |
C2—C1—S3 | 115.9 (4) | C17—C16—H16A | 108.9 |
S1—C1—S3 | 122.3 (3) | C15—C16—H16A | 108.9 |
C1—C2—S2 | 122.0 (4) | C17—C16—H16B | 108.9 |
C1—C2—S4 | 116.7 (4) | C15—C16—H16B | 108.9 |
S2—C2—S4 | 121.3 (3) | H16A—C16—H16B | 107.7 |
C4—C3—S4 | 122.9 (4) | C16—C17—C18B | 118.7 (8) |
C4—C3—S3 | 122.0 (4) | C16—C17—C18A | 124.6 (8) |
S4—C3—S3 | 115.1 (3) | C16—C17—H17A | 106.2 |
C5—C4—C3 | 120.5 (5) | C18A—C17—H17A | 106.2 |
C5—C4—C6 | 119.4 (5) | C16—C17—H17B | 106.2 |
C3—C4—C6 | 120.1 (5) | C18A—C17—H17B | 106.2 |
N1—C5—C4 | 179.1 (6) | H17A—C17—H17B | 106.4 |
N2—C6—C4 | 179.0 (6) | C16—C17—H17C | 107.6 |
C8—C7—N3 | 114.9 (4) | C18B—C17—H17C | 107.6 |
C8—C7—H7A | 108.5 | C16—C17—H17D | 107.6 |
N3—C7—H7A | 108.5 | C18B—C17—H17D | 107.6 |
C8—C7—H7B | 108.5 | H17C—C17—H17D | 107.1 |
N3—C7—H7B | 108.5 | C17—C18A—H18A | 109.5 |
H7A—C7—H7B | 107.5 | C17—C18A—H18B | 109.5 |
C7—C8—C9 | 110.6 (4) | C17—C18A—H18C | 109.5 |
C7—C8—H8A | 109.5 | C17—C18B—H18D | 109.5 |
C9—C8—H8A | 109.5 | C17—C18B—H18E | 109.5 |
C7—C8—H8B | 109.5 | H18D—C18B—H18E | 109.5 |
C9—C8—H8B | 109.5 | C17—C18B—H18F | 109.5 |
H8A—C8—H8B | 108.1 | H18D—C18B—H18F | 109.5 |
C8—C9—C10 | 113.8 (5) | H18E—C18B—H18F | 109.5 |
C8—C9—H9A | 108.8 | C20—C19—N3 | 115.4 (4) |
C10—C9—H9A | 108.8 | C20—C19—H19A | 108.4 |
C8—C9—H9B | 108.8 | N3—C19—H19A | 108.4 |
C10—C9—H9B | 108.8 | C20—C19—H19B | 108.4 |
H9A—C9—H9B | 107.7 | N3—C19—H19B | 108.4 |
C9—C10—H10A | 109.5 | H19A—C19—H19B | 107.5 |
C9—C10—H10B | 109.5 | C19—C20—C21 | 106.1 (5) |
H10A—C10—H10B | 109.5 | C19—C20—H20A | 110.5 |
C9—C10—H10C | 109.5 | C21—C20—H20A | 110.5 |
H10A—C10—H10C | 109.5 | C19—C20—H20B | 110.5 |
H10B—C10—H10C | 109.5 | C21—C20—H20B | 110.5 |
N3—C11—C12 | 115.2 (4) | H20A—C20—H20B | 108.7 |
N3—C11—H11A | 108.5 | C22—C21—C20 | 110.9 (7) |
C12—C11—H11A | 108.5 | C22—C21—H21A | 109.5 |
N3—C11—H11B | 108.5 | C20—C21—H21A | 109.5 |
C12—C11—H11B | 108.5 | C22—C21—H21B | 109.5 |
H11A—C11—H11B | 107.5 | C20—C21—H21B | 109.5 |
C13—C12—C11 | 110.6 (5) | H21A—C21—H21B | 108.0 |
C13—C12—H12A | 109.5 | C21—C22—H22A | 109.5 |
C11—C12—H12A | 109.5 | C21—C22—H22B | 109.5 |
C13—C12—H12B | 109.5 | H22A—C22—H22B | 109.5 |
C11—C12—H12B | 109.5 | C21—C22—H22C | 109.5 |
H12A—C12—H12B | 108.1 | H22A—C22—H22C | 109.5 |
C12—C13—C14 | 111.5 (6) | H22B—C22—H22C | 109.5 |
C12—C13—H13A | 109.3 | ||
S2—Ni1—S1—C1 | −4.18 (19) | S3—C3—C4—C6 | −178.9 (4) |
S2i—Ni1—S1—C1 | 175.82 (19) | C15—N3—C7—C8 | 174.0 (4) |
S1i—Ni1—S2—C2 | −176.18 (18) | C11—N3—C7—C8 | 55.3 (6) |
S1—Ni1—S2—C2 | 3.82 (18) | C19—N3—C7—C8 | −64.8 (6) |
Ni1—S1—C1—C2 | 3.9 (5) | N3—C7—C8—C9 | −177.1 (4) |
Ni1—S1—C1—S3 | −175.0 (3) | C7—C8—C9—C10 | 69.0 (7) |
C3—S3—C1—C2 | −1.9 (5) | C15—N3—C11—C12 | −68.2 (6) |
C3—S3—C1—S1 | 177.0 (3) | C7—N3—C11—C12 | 51.0 (6) |
S1—C1—C2—S2 | −1.0 (7) | C19—N3—C11—C12 | 170.4 (5) |
S3—C1—C2—S2 | 178.0 (3) | N3—C11—C12—C13 | 174.0 (5) |
S1—C1—C2—S4 | −178.7 (3) | C11—C12—C13—C14 | 178.7 (6) |
S3—C1—C2—S4 | 0.3 (6) | C11—N3—C15—C16 | −176.6 (5) |
Ni1—S2—C2—C1 | −2.6 (5) | C7—N3—C15—C16 | 61.8 (6) |
Ni1—S2—C2—S4 | 175.0 (3) | C19—N3—C15—C16 | −56.9 (6) |
C3—S4—C2—C1 | 1.5 (5) | N3—C15—C16—C17 | −179.6 (6) |
C3—S4—C2—S2 | −176.2 (3) | C15—C16—C17—C18B | −53.1 (12) |
C2—S4—C3—C4 | 177.4 (4) | C15—C16—C17—C18A | 31.7 (13) |
C2—S4—C3—S3 | −2.8 (3) | C15—N3—C19—C20 | −55.2 (6) |
C1—S3—C3—C4 | −177.2 (4) | C11—N3—C19—C20 | 63.6 (6) |
C1—S3—C3—S4 | 2.9 (4) | C7—N3—C19—C20 | −174.3 (5) |
S4—C3—C4—C5 | −178.2 (4) | N3—C19—C20—C21 | 179.3 (5) |
S3—C3—C4—C5 | 2.0 (7) | C19—C20—C21—C22 | 179.3 (6) |
S4—C3—C4—C6 | 0.9 (7) |
Symmetry code: (i) −x+1, −y+1, −z−1. |