Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680502430X/xu6034sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680502430X/xu6034Isup2.hkl |
CCDC reference: 284008
Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
[K(C14H20O5)2][Ni(C3S5)2] | F(000) = 2124 |
Mr = 1027.07 | Dx = 1.542 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 2431 reflections |
a = 18.270 (6) Å | θ = 2.5–20.1° |
b = 11.800 (4) Å | µ = 1.06 mm−1 |
c = 21.927 (8) Å | T = 293 K |
β = 110.648 (8)° | Block, colourless |
V = 4424 (3) Å3 | 0.34 × 0.23 × 0.16 mm |
Z = 4 |
Bruker SMART CCD area-detector diffractometer | 7813 independent reflections |
Radiation source: fine-focus sealed tube | 3106 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.074 |
φ and ω scans | θmax = 25.0°, θmin = 1.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −21→21 |
Tmin = 0.715, Tmax = 0.849 | k = −14→13 |
22348 measured reflections | l = −26→16 |
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)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.057 | H-atom parameters constrained |
S = 0.85 | w = 1/[σ2(Fo2)] where P = (Fo2 + 2Fc2)/3 |
7813 reflections | (Δ/σ)max = 0.001 |
505 parameters | Δρmax = 0.39 e Å−3 |
1310 restraints | Δρmin = −0.26 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 | ||
Ni1 | 0.74989 (3) | 0.90590 (5) | 0.19863 (3) | 0.05125 (19) | |
K1 | 0.13998 (5) | 0.11069 (9) | 0.39499 (5) | 0.0581 (3) | |
O1 | 0.16013 (18) | −0.0847 (3) | 0.47083 (17) | 0.0772 (10) | |
O2 | 0.03744 (17) | −0.0750 (3) | 0.36706 (16) | 0.0672 (10) | |
O3 | −0.03263 (18) | 0.1216 (3) | 0.37153 (18) | 0.0844 (11) | |
O4 | 0.0694 (2) | 0.2924 (3) | 0.44366 (18) | 0.0776 (11) | |
O5 | 0.1675 (2) | 0.1292 (3) | 0.53019 (16) | 0.0827 (11) | |
O6 | 0.2376 (2) | −0.0499 (3) | 0.35580 (18) | 0.0863 (12) | |
O7 | 0.1255 (2) | 0.0290 (3) | 0.26338 (17) | 0.0957 (12) | |
O8 | 0.09638 (19) | 0.2500 (3) | 0.27836 (18) | 0.0836 (11) | |
O9 | 0.2323 (2) | 0.2957 (3) | 0.38936 (19) | 0.0864 (11) | |
O10 | 0.30351 (17) | 0.0945 (3) | 0.45831 (16) | 0.0767 (10) | |
S1 | 0.62239 (7) | 0.81867 (12) | 0.34760 (7) | 0.0723 (4) | |
S2 | 0.56570 (7) | 1.03503 (11) | 0.29006 (7) | 0.0716 (4) | |
S3 | 0.50508 (7) | 0.94305 (12) | 0.38810 (7) | 0.0818 (5) | |
S4 | 0.66889 (7) | 1.03107 (11) | 0.20806 (7) | 0.0699 (4) | |
S5 | 0.73243 (7) | 0.79750 (11) | 0.27162 (6) | 0.0593 (4) | |
S6 | 0.89683 (7) | 0.74945 (12) | 0.07912 (7) | 0.0711 (4) | |
S7 | 0.86941 (9) | 0.98480 (13) | 0.04345 (8) | 0.0915 (5) | |
S8 | 0.94967 (9) | 0.83982 (15) | −0.02476 (8) | 0.1178 (6) | |
S9 | 0.78050 (8) | 1.02210 (11) | 0.13539 (7) | 0.0727 (4) | |
S10 | 0.81290 (7) | 0.76785 (10) | 0.17632 (6) | 0.0601 (4) | |
C1 | 0.1258 (3) | −0.1858 (5) | 0.4474 (3) | 0.0616 (14) | |
C2 | 0.1545 (3) | −0.2893 (5) | 0.4743 (3) | 0.0784 (16) | |
H2 | 0.1993 | −0.2927 | 0.5114 | 0.094* | |
C3 | 0.1168 (3) | −0.3884 (5) | 0.4463 (3) | 0.0930 (19) | |
H3 | 0.1363 | −0.4586 | 0.4640 | 0.112* | |
C4 | 0.0513 (3) | −0.3815 (5) | 0.3928 (3) | 0.0917 (18) | |
H4 | 0.0256 | −0.4480 | 0.3745 | 0.110* | |
C5 | 0.0214 (3) | −0.2800 (5) | 0.3645 (3) | 0.0812 (17) | |
H5 | −0.0240 | −0.2779 | 0.3278 | 0.097* | |
C6 | 0.0598 (3) | −0.1803 (5) | 0.3913 (3) | 0.0568 (13) | |
C7 | −0.0408 (3) | −0.0593 (4) | 0.3233 (2) | 0.0778 (17) | |
H7A | −0.0774 | −0.0917 | 0.3415 | 0.093* | |
H7B | −0.0481 | −0.0964 | 0.2821 | 0.093* | |
C8 | −0.0545 (3) | 0.0656 (5) | 0.3131 (3) | 0.0849 (18) | |
H8A | −0.0248 | 0.0945 | 0.2875 | 0.102* | |
H8B | −0.1095 | 0.0794 | 0.2890 | 0.102* | |
C9 | −0.0500 (3) | 0.2393 (5) | 0.3654 (3) | 0.0934 (19) | |
H9A | −0.1061 | 0.2507 | 0.3509 | 0.112* | |
H9B | −0.0308 | 0.2728 | 0.3335 | 0.112* | |
C10 | −0.0123 (3) | 0.2928 (4) | 0.4289 (3) | 0.0926 (18) | |
H10A | −0.0308 | 0.3701 | 0.4278 | 0.111* | |
H10B | −0.0251 | 0.2516 | 0.4621 | 0.111* | |
C11 | 0.1141 (3) | 0.3127 (5) | 0.5105 (3) | 0.0977 (19) | |
H11A | 0.0875 | 0.3687 | 0.5275 | 0.117* | |
H11B | 0.1646 | 0.3437 | 0.5138 | 0.117* | |
C12 | 0.1262 (3) | 0.2120 (5) | 0.5497 (3) | 0.101 (2) | |
H12A | 0.1546 | 0.2316 | 0.5948 | 0.121* | |
H12B | 0.0758 | 0.1816 | 0.5469 | 0.121* | |
C13 | 0.1704 (4) | 0.0273 (5) | 0.5622 (3) | 0.111 (2) | |
H13A | 0.2056 | 0.0365 | 0.6069 | 0.134* | |
H13B | 0.1188 | 0.0126 | 0.5635 | 0.134* | |
C14 | 0.1931 (3) | −0.0651 (5) | 0.5375 (3) | 0.116 (2) | |
H14A | 0.1826 | −0.1309 | 0.5596 | 0.139* | |
H14B | 0.2494 | −0.0607 | 0.5488 | 0.139* | |
C15 | 0.1946 (3) | −0.1301 (5) | 0.3128 (3) | 0.0692 (15) | |
C16 | 0.2082 (3) | −0.2445 (5) | 0.3171 (3) | 0.0828 (16) | |
H16 | 0.2488 | −0.2756 | 0.3517 | 0.099* | |
C17 | 0.1588 (4) | −0.3126 (5) | 0.2675 (3) | 0.0930 (19) | |
H17 | 0.1673 | −0.3904 | 0.2693 | 0.112* | |
C18 | 0.0991 (3) | −0.2690 (5) | 0.2170 (3) | 0.0908 (19) | |
H18 | 0.0672 | −0.3166 | 0.1848 | 0.109* | |
C19 | 0.0858 (3) | −0.1551 (5) | 0.2136 (3) | 0.0831 (17) | |
H19 | 0.0444 | −0.1250 | 0.1793 | 0.100* | |
C20 | 0.1336 (3) | −0.0847 (5) | 0.2610 (3) | 0.0683 (15) | |
C21 | 0.0861 (3) | 0.0908 (5) | 0.2103 (3) | 0.1070 (19) | |
H21A | 0.0303 | 0.0810 | 0.2000 | 0.128* | |
H21B | 0.0989 | 0.0644 | 0.1734 | 0.128* | |
C22 | 0.1059 (3) | 0.2093 (5) | 0.2217 (3) | 0.0947 (18) | |
H22A | 0.1598 | 0.2201 | 0.2251 | 0.114* | |
H22B | 0.0731 | 0.2530 | 0.1847 | 0.114* | |
C23 | 0.1268 (3) | 0.3598 (5) | 0.2995 (3) | 0.119 (2) | |
H23A | 0.1006 | 0.3900 | 0.3276 | 0.143* | |
H23B | 0.1142 | 0.4089 | 0.2617 | 0.143* | |
C24 | 0.2091 (3) | 0.3642 (5) | 0.3337 (3) | 0.121 (2) | |
H24A | 0.2359 | 0.3397 | 0.3049 | 0.146* | |
H24B | 0.2243 | 0.4419 | 0.3464 | 0.146* | |
C25 | 0.3143 (3) | 0.2813 (4) | 0.4165 (3) | 0.0879 (17) | |
H25A | 0.3395 | 0.3542 | 0.4297 | 0.105* | |
H25B | 0.3333 | 0.2490 | 0.3842 | 0.105* | |
C26 | 0.3339 (3) | 0.2056 (5) | 0.4733 (3) | 0.0904 (18) | |
H26A | 0.3903 | 0.2011 | 0.4935 | 0.109* | |
H26B | 0.3139 | 0.2385 | 0.5049 | 0.109* | |
C27 | 0.3489 (3) | 0.0243 (5) | 0.4343 (3) | 0.0882 (18) | |
H27A | 0.3977 | 0.0067 | 0.4691 | 0.106* | |
H27B | 0.3611 | 0.0637 | 0.4002 | 0.106* | |
C28 | 0.3067 (3) | −0.0822 (4) | 0.4078 (3) | 0.0810 (16) | |
H28A | 0.3387 | −0.1312 | 0.3920 | 0.097* | |
H28B | 0.2936 | −0.1222 | 0.4412 | 0.097* | |
C29 | 0.5617 (2) | 0.9319 (4) | 0.3440 (2) | 0.0561 (14) | |
C30 | 0.6356 (2) | 0.9708 (4) | 0.2648 (2) | 0.0529 (13) | |
C31 | 0.6630 (2) | 0.8700 (4) | 0.2911 (2) | 0.0523 (13) | |
C32 | 0.9078 (2) | 0.8574 (4) | 0.0293 (2) | 0.0708 (15) | |
C33 | 0.8328 (2) | 0.9364 (4) | 0.1020 (2) | 0.0523 (14) | |
C34 | 0.8473 (2) | 0.8274 (4) | 0.1199 (2) | 0.0506 (13) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0500 (4) | 0.0519 (4) | 0.0535 (5) | −0.0016 (3) | 0.0203 (3) | −0.0050 (4) |
K1 | 0.0575 (6) | 0.0592 (8) | 0.0575 (8) | 0.0005 (6) | 0.0201 (6) | 0.0028 (6) |
O1 | 0.096 (2) | 0.062 (2) | 0.052 (2) | −0.016 (2) | −0.001 (2) | 0.000 (2) |
O2 | 0.059 (2) | 0.061 (2) | 0.073 (2) | −0.0022 (18) | 0.0128 (19) | 0.005 (2) |
O3 | 0.078 (2) | 0.084 (3) | 0.074 (3) | 0.017 (2) | 0.006 (2) | 0.004 (3) |
O4 | 0.070 (2) | 0.083 (3) | 0.072 (3) | 0.018 (2) | 0.016 (2) | 0.007 (2) |
O5 | 0.123 (3) | 0.057 (3) | 0.063 (3) | 0.019 (2) | 0.027 (2) | 0.008 (2) |
O6 | 0.091 (3) | 0.078 (3) | 0.070 (3) | 0.025 (2) | 0.003 (2) | −0.007 (2) |
O7 | 0.131 (3) | 0.068 (3) | 0.059 (3) | 0.034 (2) | −0.003 (2) | 0.003 (2) |
O8 | 0.112 (3) | 0.062 (3) | 0.077 (3) | 0.002 (2) | 0.034 (2) | 0.006 (2) |
O9 | 0.087 (3) | 0.081 (3) | 0.087 (3) | −0.002 (2) | 0.024 (3) | 0.015 (2) |
O10 | 0.066 (2) | 0.084 (3) | 0.079 (3) | 0.001 (2) | 0.025 (2) | −0.012 (2) |
S1 | 0.0790 (10) | 0.0805 (11) | 0.0683 (11) | 0.0133 (8) | 0.0395 (9) | 0.0124 (9) |
S2 | 0.0745 (9) | 0.0622 (10) | 0.0947 (12) | 0.0085 (8) | 0.0504 (9) | 0.0051 (9) |
S3 | 0.0748 (10) | 0.1046 (13) | 0.0803 (12) | −0.0020 (9) | 0.0451 (10) | −0.0053 (10) |
S4 | 0.0804 (10) | 0.0531 (10) | 0.0928 (12) | 0.0076 (8) | 0.0513 (9) | 0.0098 (9) |
S5 | 0.0609 (8) | 0.0672 (10) | 0.0537 (9) | 0.0123 (7) | 0.0252 (8) | 0.0028 (8) |
S6 | 0.0774 (9) | 0.0759 (11) | 0.0700 (10) | 0.0059 (8) | 0.0383 (9) | −0.0082 (9) |
S7 | 0.1167 (13) | 0.0884 (13) | 0.0960 (13) | 0.0108 (10) | 0.0706 (11) | 0.0215 (10) |
S8 | 0.1269 (13) | 0.1530 (18) | 0.1027 (14) | −0.0108 (12) | 0.0765 (12) | −0.0162 (13) |
S9 | 0.0902 (10) | 0.0577 (10) | 0.0857 (11) | 0.0123 (8) | 0.0504 (9) | 0.0084 (9) |
S10 | 0.0697 (9) | 0.0564 (10) | 0.0608 (10) | 0.0036 (7) | 0.0312 (8) | 0.0008 (8) |
C1 | 0.070 (3) | 0.053 (3) | 0.069 (4) | −0.004 (3) | 0.033 (3) | 0.002 (3) |
C2 | 0.083 (4) | 0.068 (4) | 0.084 (4) | 0.007 (3) | 0.029 (3) | 0.008 (4) |
C3 | 0.102 (4) | 0.060 (4) | 0.111 (5) | 0.010 (4) | 0.031 (4) | 0.006 (4) |
C4 | 0.105 (4) | 0.065 (4) | 0.109 (5) | −0.010 (4) | 0.042 (4) | −0.014 (4) |
C5 | 0.081 (4) | 0.065 (4) | 0.095 (4) | −0.015 (3) | 0.028 (3) | −0.008 (4) |
C6 | 0.057 (3) | 0.058 (3) | 0.062 (3) | −0.004 (3) | 0.030 (3) | −0.005 (3) |
C7 | 0.051 (3) | 0.095 (4) | 0.076 (4) | −0.006 (3) | 0.008 (3) | −0.010 (4) |
C8 | 0.064 (3) | 0.101 (5) | 0.071 (4) | 0.014 (3) | 0.001 (3) | −0.001 (4) |
C9 | 0.071 (4) | 0.087 (4) | 0.100 (5) | 0.029 (3) | 0.002 (4) | 0.011 (4) |
C10 | 0.076 (4) | 0.097 (4) | 0.102 (5) | 0.025 (3) | 0.028 (4) | 0.000 (4) |
C11 | 0.113 (4) | 0.085 (4) | 0.082 (4) | 0.008 (4) | 0.018 (4) | −0.014 (4) |
C12 | 0.132 (4) | 0.092 (5) | 0.064 (4) | 0.015 (4) | 0.015 (4) | −0.008 (4) |
C13 | 0.174 (5) | 0.087 (5) | 0.064 (4) | 0.034 (4) | 0.030 (4) | 0.013 (4) |
C14 | 0.164 (5) | 0.085 (4) | 0.071 (4) | 0.026 (4) | 0.008 (4) | 0.015 (4) |
C15 | 0.085 (3) | 0.063 (4) | 0.067 (4) | 0.012 (3) | 0.037 (3) | −0.002 (3) |
C16 | 0.099 (4) | 0.080 (4) | 0.082 (4) | 0.012 (4) | 0.046 (3) | 0.010 (4) |
C17 | 0.120 (5) | 0.065 (4) | 0.108 (5) | −0.007 (4) | 0.058 (4) | −0.001 (4) |
C18 | 0.093 (4) | 0.087 (5) | 0.098 (5) | −0.022 (4) | 0.042 (4) | −0.021 (4) |
C19 | 0.087 (4) | 0.082 (4) | 0.080 (4) | 0.002 (3) | 0.029 (3) | −0.015 (4) |
C20 | 0.084 (4) | 0.060 (4) | 0.068 (4) | 0.003 (3) | 0.035 (3) | −0.006 (3) |
C21 | 0.153 (5) | 0.093 (5) | 0.071 (4) | 0.014 (4) | 0.035 (4) | 0.007 (4) |
C22 | 0.128 (4) | 0.091 (5) | 0.076 (4) | 0.022 (4) | 0.049 (4) | 0.022 (4) |
C23 | 0.131 (4) | 0.070 (4) | 0.131 (5) | −0.001 (4) | 0.013 (4) | 0.024 (4) |
C24 | 0.107 (4) | 0.087 (4) | 0.142 (5) | −0.008 (4) | 0.010 (4) | 0.046 (4) |
C25 | 0.090 (4) | 0.091 (4) | 0.080 (4) | −0.027 (3) | 0.026 (4) | −0.009 (4) |
C26 | 0.079 (4) | 0.105 (5) | 0.082 (4) | −0.019 (4) | 0.021 (3) | −0.013 (4) |
C27 | 0.067 (4) | 0.119 (5) | 0.080 (4) | 0.015 (4) | 0.028 (3) | −0.027 (4) |
C28 | 0.074 (3) | 0.088 (4) | 0.079 (4) | 0.028 (3) | 0.025 (3) | 0.001 (4) |
C29 | 0.053 (3) | 0.061 (4) | 0.056 (3) | −0.004 (3) | 0.020 (3) | −0.004 (3) |
C30 | 0.048 (3) | 0.054 (3) | 0.060 (3) | −0.004 (3) | 0.023 (3) | −0.009 (3) |
C31 | 0.052 (3) | 0.060 (3) | 0.048 (3) | −0.007 (3) | 0.021 (3) | −0.005 (3) |
C32 | 0.079 (3) | 0.081 (4) | 0.063 (4) | 0.001 (3) | 0.037 (3) | −0.008 (3) |
C33 | 0.057 (3) | 0.057 (3) | 0.053 (3) | −0.005 (3) | 0.032 (3) | −0.007 (3) |
C34 | 0.044 (3) | 0.057 (3) | 0.055 (3) | 0.003 (3) | 0.022 (3) | −0.008 (3) |
Ni1—S4 | 2.1518 (14) | C4—C5 | 1.372 (6) |
Ni1—S5 | 2.1586 (15) | C4—H4 | 0.9300 |
Ni1—S9 | 2.1594 (15) | C5—C6 | 1.390 (6) |
Ni1—S10 | 2.1484 (14) | C5—H5 | 0.9300 |
K1—O1 | 2.790 (3) | C7—C8 | 1.499 (5) |
K1—O2 | 2.807 (3) | C7—H7A | 0.9700 |
K1—O3 | 3.014 (3) | C7—H7B | 0.9700 |
K1—O4 | 2.892 (3) | C8—H8A | 0.9700 |
K1—O5 | 2.835 (4) | C8—H8B | 0.9700 |
K1—O6 | 2.931 (3) | C9—C10 | 1.461 (6) |
K1—O7 | 2.965 (4) | C9—H9A | 0.9700 |
K1—O8 | 2.905 (4) | C9—H9B | 0.9700 |
K1—O9 | 2.788 (4) | C10—H10A | 0.9700 |
K1—O10 | 2.822 (3) | C10—H10B | 0.9700 |
O1—C1 | 1.361 (5) | C11—C12 | 1.437 (6) |
O1—C14 | 1.390 (5) | C11—H11A | 0.9700 |
O2—C6 | 1.356 (5) | C11—H11B | 0.9700 |
O2—C7 | 1.425 (4) | C12—H12A | 0.9700 |
O3—C8 | 1.370 (5) | C12—H12B | 0.9700 |
O3—C9 | 1.420 (5) | C13—C14 | 1.346 (6) |
O4—C10 | 1.412 (4) | C13—H13A | 0.9700 |
O4—C11 | 1.424 (5) | C13—H13B | 0.9700 |
O5—C13 | 1.383 (6) | C14—H14A | 0.9700 |
O5—C12 | 1.391 (5) | C14—H14B | 0.9700 |
O6—C15 | 1.371 (5) | C15—C16 | 1.370 (6) |
O6—C28 | 1.422 (5) | C15—C20 | 1.387 (6) |
O7—C21 | 1.346 (5) | C16—C17 | 1.397 (6) |
O7—C20 | 1.353 (5) | C16—H16 | 0.9300 |
O8—C22 | 1.399 (5) | C17—C18 | 1.352 (6) |
O8—C23 | 1.423 (5) | C17—H17 | 0.9300 |
O9—C24 | 1.398 (6) | C18—C19 | 1.364 (6) |
O9—C25 | 1.414 (5) | C18—H18 | 0.9300 |
O10—C27 | 1.400 (5) | C19—C20 | 1.376 (6) |
O10—C26 | 1.416 (5) | C19—H19 | 0.9300 |
S1—C29 | 1.720 (4) | C21—C22 | 1.444 (6) |
S1—C31 | 1.760 (4) | C21—H21A | 0.9700 |
S2—C29 | 1.717 (4) | C21—H21B | 0.9700 |
S2—C30 | 1.735 (4) | C22—H22A | 0.9700 |
S2—S10i | 3.444 (2) | C22—H22B | 0.9700 |
S3—C29 | 1.651 (4) | C23—C24 | 1.424 (6) |
S4—C30 | 1.721 (5) | C23—H23A | 0.9700 |
S4—S5i | 3.573 (2) | C23—H23B | 0.9700 |
S5—C31 | 1.705 (4) | C24—H24A | 0.9700 |
S6—C32 | 1.735 (5) | C24—H24B | 0.9700 |
S6—C34 | 1.742 (4) | C25—C26 | 1.471 (6) |
S7—C32 | 1.733 (5) | C25—H25A | 0.9700 |
S7—C33 | 1.740 (4) | C25—H25B | 0.9700 |
S8—C32 | 1.635 (5) | C26—H26A | 0.9700 |
S9—C33 | 1.722 (4) | C26—H26B | 0.9700 |
S10—C34 | 1.723 (5) | C27—C28 | 1.481 (6) |
C1—C2 | 1.377 (6) | C27—H27A | 0.9700 |
C1—C6 | 1.387 (6) | C27—H27B | 0.9700 |
C2—C3 | 1.387 (6) | C28—H28A | 0.9700 |
C2—H2 | 0.9300 | C28—H28B | 0.9700 |
C3—C4 | 1.350 (6) | C30—C31 | 1.340 (5) |
C3—H3 | 0.9300 | C33—C34 | 1.344 (5) |
S10—Ni1—S4 | 169.82 (6) | H8A—C8—H8B | 108.0 |
S10—Ni1—S5 | 87.17 (6) | O3—C9—C10 | 108.5 (5) |
S4—Ni1—S5 | 92.81 (6) | O3—C9—H9A | 110.0 |
S10—Ni1—S9 | 93.12 (6) | C10—C9—H9A | 110.0 |
S4—Ni1—S9 | 88.19 (6) | O3—C9—H9B | 110.0 |
S5—Ni1—S9 | 172.70 (6) | C10—C9—H9B | 110.0 |
O9—K1—O1 | 135.95 (11) | H9A—C9—H9B | 108.4 |
O9—K1—O2 | 165.78 (11) | O4—C10—C9 | 108.8 (5) |
O1—K1—O2 | 54.72 (10) | O4—C10—H10A | 109.9 |
O9—K1—O10 | 61.49 (11) | C9—C10—H10A | 109.9 |
O1—K1—O10 | 75.92 (10) | O4—C10—H10B | 109.9 |
O2—K1—O10 | 124.33 (11) | C9—C10—H10B | 109.9 |
O9—K1—O5 | 95.68 (11) | H10A—C10—H10B | 108.3 |
O1—K1—O5 | 60.20 (11) | O4—C11—C12 | 112.8 (5) |
O2—K1—O5 | 98.45 (10) | O4—C11—H11A | 109.0 |
O10—K1—O5 | 73.99 (10) | C12—C11—H11A | 109.0 |
O9—K1—O4 | 77.95 (10) | O4—C11—H11B | 109.0 |
O1—K1—O4 | 112.02 (10) | C12—C11—H11B | 109.0 |
O2—K1—O4 | 108.02 (10) | H11A—C11—H11B | 107.8 |
O10—K1—O4 | 113.62 (11) | O5—C12—C11 | 112.5 (5) |
O5—K1—O4 | 59.67 (10) | O5—C12—H12A | 109.1 |
O9—K1—O8 | 60.03 (11) | C11—C12—H12A | 109.1 |
O1—K1—O8 | 158.39 (11) | O5—C12—H12B | 109.1 |
O2—K1—O8 | 107.15 (11) | C11—C12—H12B | 109.1 |
O10—K1—O8 | 112.67 (10) | H12A—C12—H12B | 107.8 |
O5—K1—O8 | 140.31 (12) | C14—C13—O5 | 117.5 (6) |
O4—K1—O8 | 83.45 (11) | C14—C13—H13A | 107.9 |
O9—K1—O6 | 93.06 (11) | O5—C13—H13A | 107.9 |
O1—K1—O6 | 70.99 (10) | C14—C13—H13B | 107.9 |
O2—K1—O6 | 81.91 (10) | O5—C13—H13B | 107.9 |
O10—K1—O6 | 56.81 (11) | H13A—C13—H13B | 107.2 |
O5—K1—O6 | 117.03 (11) | C13—C14—O1 | 118.5 (5) |
O4—K1—O6 | 169.66 (11) | C13—C14—H14A | 107.7 |
O8—K1—O6 | 96.55 (11) | O1—C14—H14A | 107.7 |
O9—K1—O7 | 93.40 (11) | C13—C14—H14B | 107.7 |
O1—K1—O7 | 105.02 (12) | O1—C14—H14B | 107.7 |
O2—K1—O7 | 73.14 (11) | H14A—C14—H14B | 107.1 |
O10—K1—O7 | 99.94 (10) | C16—C15—O6 | 125.9 (6) |
O5—K1—O7 | 164.79 (12) | C16—C15—C20 | 120.8 (6) |
O4—K1—O7 | 134.56 (11) | O6—C15—C20 | 113.4 (6) |
O8—K1—O7 | 54.85 (11) | C15—C16—C17 | 117.5 (6) |
O6—K1—O7 | 50.14 (10) | C15—C16—H16 | 121.3 |
O9—K1—O3 | 124.88 (11) | C17—C16—H16 | 121.3 |
O1—K1—O3 | 92.72 (10) | C18—C17—C16 | 122.1 (6) |
O2—K1—O3 | 54.45 (10) | C18—C17—H17 | 118.9 |
O10—K1—O3 | 161.70 (11) | C16—C17—H17 | 118.9 |
O5—K1—O3 | 87.96 (10) | C17—C18—C19 | 119.8 (6) |
O4—K1—O3 | 57.02 (10) | C17—C18—H18 | 120.1 |
O8—K1—O3 | 83.10 (10) | C19—C18—H18 | 120.1 |
O6—K1—O3 | 133.30 (11) | C18—C19—C20 | 120.0 (6) |
O7—K1—O3 | 96.82 (11) | C18—C19—H19 | 120.0 |
C1—O1—C14 | 120.9 (5) | C20—C19—H19 | 120.0 |
C1—O1—K1 | 123.6 (3) | O7—C20—C19 | 125.4 (6) |
C14—O1—K1 | 114.0 (3) | O7—C20—C15 | 114.8 (6) |
C6—O2—C7 | 118.4 (4) | C19—C20—C15 | 119.8 (6) |
C6—O2—K1 | 122.9 (3) | O7—C21—C22 | 110.5 (5) |
C7—O2—K1 | 118.6 (3) | O7—C21—H21A | 109.6 |
C8—O3—C9 | 113.7 (4) | C22—C21—H21A | 109.6 |
C8—O3—K1 | 94.7 (3) | O7—C21—H21B | 109.6 |
C9—O3—K1 | 104.1 (3) | C22—C21—H21B | 109.6 |
C10—O4—C11 | 114.4 (4) | H21A—C21—H21B | 108.1 |
C10—O4—K1 | 119.4 (3) | O8—C22—C21 | 112.5 (5) |
C11—O4—K1 | 109.6 (3) | O8—C22—H22A | 109.1 |
C13—O5—C12 | 112.5 (5) | C21—C22—H22A | 109.1 |
C13—O5—K1 | 115.1 (3) | O8—C22—H22B | 109.1 |
C12—O5—K1 | 117.4 (3) | C21—C22—H22B | 109.1 |
C15—O6—C28 | 119.9 (4) | H22A—C22—H22B | 107.8 |
C15—O6—K1 | 112.8 (3) | O8—C23—C24 | 115.0 (5) |
C28—O6—K1 | 113.4 (3) | O8—C23—H23A | 108.5 |
C21—O7—C20 | 122.4 (5) | C24—C23—H23A | 108.5 |
C21—O7—K1 | 120.1 (3) | O8—C23—H23B | 108.5 |
C20—O7—K1 | 112.7 (3) | C24—C23—H23B | 108.5 |
C22—O8—C23 | 116.5 (5) | H23A—C23—H23B | 107.5 |
C22—O8—K1 | 120.4 (3) | O9—C24—C23 | 112.2 (5) |
C23—O8—K1 | 105.9 (3) | O9—C24—H24A | 109.2 |
C24—O9—C25 | 112.8 (4) | C23—C24—H24A | 109.2 |
C24—O9—K1 | 119.3 (3) | O9—C24—H24B | 109.2 |
C25—O9—K1 | 117.1 (3) | C23—C24—H24B | 109.2 |
C27—O10—C26 | 113.6 (4) | H24A—C24—H24B | 107.9 |
C27—O10—K1 | 121.3 (3) | O9—C25—C26 | 109.5 (5) |
C26—O10—K1 | 108.2 (3) | O9—C25—H25A | 109.8 |
C29—S1—C31 | 97.2 (2) | C26—C25—H25A | 109.8 |
C29—S2—C30 | 97.2 (2) | O9—C25—H25B | 109.8 |
C29—S2—S10i | 126.76 (15) | C26—C25—H25B | 109.8 |
C30—S2—S10i | 85.75 (16) | H25A—C25—H25B | 108.2 |
C30—S4—Ni1 | 102.50 (17) | O10—C26—C25 | 114.0 (5) |
C30—S4—S5i | 124.40 (16) | O10—C26—H26A | 108.7 |
Ni1—S4—S5i | 106.38 (6) | C25—C26—H26A | 108.7 |
C31—S5—Ni1 | 101.91 (17) | O10—C26—H26B | 108.7 |
C32—S6—C34 | 97.6 (2) | C25—C26—H26B | 108.7 |
C32—S7—C33 | 97.6 (2) | H26A—C26—H26B | 107.6 |
C33—S9—Ni1 | 102.03 (17) | O10—C27—C28 | 110.8 (4) |
C34—S10—Ni1 | 102.39 (17) | O10—C27—H27A | 109.5 |
O1—C1—C2 | 124.1 (6) | C28—C27—H27A | 109.5 |
O1—C1—C6 | 115.7 (5) | O10—C27—H27B | 109.5 |
C2—C1—C6 | 120.1 (6) | C28—C27—H27B | 109.5 |
C1—C2—C3 | 120.3 (6) | H27A—C27—H27B | 108.1 |
C1—C2—H2 | 119.9 | O6—C28—C27 | 106.2 (4) |
C3—C2—H2 | 119.9 | O6—C28—H28A | 110.5 |
C4—C3—C2 | 118.9 (6) | C27—C28—H28A | 110.5 |
C4—C3—H3 | 120.5 | O6—C28—H28B | 110.5 |
C2—C3—H3 | 120.5 | C27—C28—H28B | 110.5 |
C3—C4—C5 | 122.4 (6) | H28A—C28—H28B | 108.7 |
C3—C4—H4 | 118.8 | S3—C29—S2 | 122.3 (3) |
C5—C4—H4 | 118.8 | S3—C29—S1 | 124.2 (3) |
C4—C5—C6 | 119.1 (6) | S2—C29—S1 | 113.5 (2) |
C4—C5—H5 | 120.5 | C31—C30—S4 | 120.3 (4) |
C6—C5—H5 | 120.5 | C31—C30—S2 | 117.1 (4) |
O2—C6—C1 | 116.0 (5) | S4—C30—S2 | 122.5 (3) |
O2—C6—C5 | 124.8 (5) | C30—C31—S5 | 122.4 (4) |
C1—C6—C5 | 119.1 (6) | C30—C31—S1 | 115.0 (4) |
O2—C7—C8 | 107.7 (4) | S5—C31—S1 | 122.6 (3) |
O2—C7—H7A | 110.2 | S8—C32—S7 | 124.2 (3) |
C8—C7—H7A | 110.2 | S8—C32—S6 | 123.4 (3) |
O2—C7—H7B | 110.2 | S7—C32—S6 | 112.4 (3) |
C8—C7—H7B | 110.2 | C34—C33—S9 | 121.3 (4) |
H7A—C7—H7B | 108.5 | C34—C33—S7 | 116.2 (4) |
O3—C8—C7 | 110.9 (5) | S9—C33—S7 | 122.5 (3) |
O3—C8—H8A | 109.5 | C33—C34—S10 | 121.1 (4) |
C7—C8—H8A | 109.5 | C33—C34—S6 | 116.1 (4) |
O3—C8—H8B | 109.5 | S10—C34—S6 | 122.7 (3) |
C7—C8—H8B | 109.5 |
Symmetry code: (i) −x+3/2, y+1/2, −z+1/2. |