Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520613034665/bi5029sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520613034665/bi5029Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520613034665/bi5029IIsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520613034665/bi5029IIIsup4.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2052520613034665/bi5029sup5.pdf |
CCDC references: 885882; 885884; 885883
For all compounds, data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Bruker, 2008); software used to prepare material for publication: SHELXTL.
C34H36N6NiO8S2 | F(000) = 1624 |
Mr = 779.52 | Dx = 1.408 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 9912 reflections |
a = 11.8719 (4) Å | θ = 2.4–28.3° |
b = 14.1629 (5) Å | µ = 0.70 mm−1 |
c = 21.9663 (7) Å | T = 100 K |
β = 95.342 (1)° | Needle, blue |
V = 3677.4 (2) Å3 | 0.45 × 0.14 × 0.12 mm |
Z = 4 |
Bruker APEX-II CCD diffractometer | 14290 independent reflections |
Radiation source: fine-focus sealed tube | 12276 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.000 |
φ and ω scans | θmax = 26.0°, θmin = 1.7° |
Absorption correction: multi-scan SADABS (Bruker, 2008) | h = −14→14 |
Tmin = 0.745, Tmax = 0.922 | k = −17→17 |
50874 measured reflections | l = 0→27 |
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)] = 0.030 | H-atom parameters constrained |
wR(F2) = 0.072 | w = 1/[σ2(Fo2) + (0.0288P)2 + 1.7597P] where P = (Fo2 + 2Fc2)/3 |
S = 0.96 | (Δ/σ)max = 0.001 |
14290 reflections | Δρmax = 0.55 e Å−3 |
938 parameters | Δρmin = −0.35 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 6750 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.008 (6) |
C34H36N6NiO8S2 | V = 3677.4 (2) Å3 |
Mr = 779.52 | Z = 4 |
Monoclinic, P21 | Mo Kα radiation |
a = 11.8719 (4) Å | µ = 0.70 mm−1 |
b = 14.1629 (5) Å | T = 100 K |
c = 21.9663 (7) Å | 0.45 × 0.14 × 0.12 mm |
β = 95.342 (1)° |
Bruker APEX-II CCD diffractometer | 14290 independent reflections |
Absorption correction: multi-scan SADABS (Bruker, 2008) | 12276 reflections with I > 2σ(I) |
Tmin = 0.745, Tmax = 0.922 | Rint = 0.000 |
50874 measured reflections |
R[F2 > 2σ(F2)] = 0.030 | H-atom parameters constrained |
wR(F2) = 0.072 | Δρmax = 0.55 e Å−3 |
S = 0.96 | Δρmin = −0.35 e Å−3 |
14290 reflections | Absolute structure: Flack (1983), 6750 Friedel pairs |
938 parameters | Absolute structure parameter: −0.008 (6) |
1 restraint |
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 | Occ. (<1) | |
Ni1 | 0.78792 (2) | 0.42955 (2) | 0.455963 (12) | 0.01400 (7) | |
Ni2 | 0.20607 (2) | 0.92946 (2) | 0.038954 (12) | 0.01384 (7) | |
S1 | 0.72957 (6) | 0.73669 (5) | 0.37599 (3) | 0.03172 (16) | |
S2 | 0.82940 (6) | 0.10683 (5) | 0.52022 (3) | 0.03093 (16) | |
S3 | 0.25275 (7) | 1.23037 (5) | 0.13301 (3) | 0.03698 (17) | |
S4 | 0.15880 (6) | 0.61497 (5) | −0.03888 (3) | 0.03210 (17) | |
O1 | 0.35589 (15) | 0.59960 (12) | 0.62056 (8) | 0.0273 (4) | |
O2 | 0.28446 (13) | 0.45432 (11) | 0.59968 (7) | 0.0201 (4) | |
O3 | 0.58387 (17) | 0.32957 (13) | 0.14655 (8) | 0.0321 (4) | |
O4 | 0.61791 (15) | 0.18396 (12) | 0.18495 (7) | 0.0224 (4) | |
O5 | 1.28816 (14) | 0.30199 (13) | 0.33125 (8) | 0.0254 (4) | |
O6 | 1.34447 (14) | 0.25948 (12) | 0.42818 (8) | 0.0272 (4) | |
O7 | 0.9335 (3) | 0.5160 (2) | 0.76785 (9) | 0.0788 (10) | |
O8 | 0.99459 (17) | 0.65286 (15) | 0.73346 (8) | 0.0346 (5) | |
O9 | 0.11904 (17) | 1.07806 (16) | −0.26913 (8) | 0.0395 (5) | |
O11 | 0.65884 (14) | 1.10276 (12) | −0.11003 (8) | 0.0260 (4) | |
O12 | 0.72046 (13) | 0.95377 (11) | −0.09416 (7) | 0.0202 (4) | |
O13 | 0.40584 (16) | 0.83053 (13) | 0.34910 (7) | 0.0283 (4) | |
O14 | 0.37501 (15) | 0.68399 (12) | 0.31145 (7) | 0.0211 (4) | |
O15 | −0.35005 (14) | 0.75607 (12) | 0.06573 (8) | 0.0258 (4) | |
O16 | −0.29622 (14) | 0.80458 (13) | 0.16178 (8) | 0.0265 (4) | |
N1 | 0.80384 (16) | 0.56017 (14) | 0.41930 (9) | 0.0181 (4) | |
N2 | 0.77846 (16) | 0.29545 (14) | 0.49117 (9) | 0.0179 (4) | |
N3 | 0.62190 (15) | 0.46288 (13) | 0.48125 (8) | 0.0154 (4) | |
N4 | 0.72444 (16) | 0.37876 (13) | 0.36772 (8) | 0.0162 (4) | |
N5 | 0.95662 (16) | 0.39794 (13) | 0.43762 (8) | 0.0172 (4) | |
N6 | 0.84360 (16) | 0.48150 (14) | 0.54420 (8) | 0.0165 (4) | |
N7 | 0.18957 (16) | 1.05940 (14) | 0.07713 (9) | 0.0176 (4) | |
N8 | 0.21654 (16) | 0.79722 (14) | 0.00179 (8) | 0.0179 (4) | |
N9 | 0.15178 (16) | 0.98596 (14) | −0.04828 (8) | 0.0163 (4) | |
N10 | 0.37366 (15) | 0.96239 (13) | 0.01638 (8) | 0.0154 (4) | |
N11 | 0.26829 (16) | 0.87817 (13) | 0.12731 (8) | 0.0157 (4) | |
N12 | 0.03716 (16) | 0.89590 (13) | 0.05527 (8) | 0.0167 (4) | |
C1 | 0.77517 (19) | 0.63359 (16) | 0.40048 (10) | 0.0165 (5) | |
C2 | 0.79992 (19) | 0.21693 (18) | 0.50385 (10) | 0.0186 (5) | |
C3 | 0.54879 (19) | 0.39473 (16) | 0.49377 (10) | 0.0167 (5) | |
H3 | 0.5592 | 0.3331 | 0.4782 | 0.020* | |
C4 | 0.45807 (18) | 0.41070 (16) | 0.52872 (9) | 0.0161 (5) | |
H4 | 0.4078 | 0.3611 | 0.5369 | 0.019* | |
C5 | 0.44359 (19) | 0.50066 (17) | 0.55100 (10) | 0.0168 (5) | |
C6 | 0.51510 (19) | 0.57289 (17) | 0.53549 (10) | 0.0178 (5) | |
H6 | 0.5039 | 0.6359 | 0.5485 | 0.021* | |
C7 | 0.60277 (19) | 0.55099 (16) | 0.50073 (10) | 0.0175 (5) | |
H7 | 0.6516 | 0.6003 | 0.4901 | 0.021* | |
C8 | 0.3563 (2) | 0.52479 (17) | 0.59359 (10) | 0.0194 (5) | |
C9 | 0.1955 (2) | 0.47341 (18) | 0.63923 (11) | 0.0264 (6) | |
H9A | 0.1308 | 0.4307 | 0.6282 | 0.032* | |
H9B | 0.1687 | 0.5392 | 0.6327 | 0.032* | |
C10 | 0.2361 (3) | 0.4597 (2) | 0.70583 (12) | 0.0360 (7) | |
H10A | 0.2635 | 0.3949 | 0.7123 | 0.054* | |
H10B | 0.1735 | 0.4713 | 0.7310 | 0.054* | |
H10C | 0.2978 | 0.5041 | 0.7174 | 0.054* | |
C11 | 0.66904 (17) | 0.43497 (18) | 0.32566 (10) | 0.0187 (5) | |
H11 | 0.6548 | 0.4986 | 0.3364 | 0.022* | |
C12 | 0.63184 (19) | 0.40446 (16) | 0.26755 (10) | 0.0198 (5) | |
H12 | 0.5933 | 0.4463 | 0.2390 | 0.024* | |
C13 | 0.65185 (19) | 0.31130 (16) | 0.25161 (10) | 0.0164 (5) | |
C14 | 0.7081 (2) | 0.25278 (17) | 0.29470 (10) | 0.0189 (5) | |
H14 | 0.7230 | 0.1888 | 0.2853 | 0.023* | |
C15 | 0.7424 (2) | 0.28952 (17) | 0.35179 (10) | 0.0193 (5) | |
H15 | 0.7809 | 0.2490 | 0.3813 | 0.023* | |
C16 | 0.6135 (2) | 0.27761 (18) | 0.18811 (11) | 0.0193 (5) | |
C17 | 0.5821 (2) | 0.14118 (18) | 0.12558 (10) | 0.0239 (6) | |
H17A | 0.6240 | 0.1693 | 0.0932 | 0.029* | |
H17B | 0.5001 | 0.1512 | 0.1149 | 0.029* | |
C18 | 0.6078 (2) | 0.03763 (18) | 0.13211 (11) | 0.0270 (6) | |
H18A | 0.6893 | 0.0289 | 0.1425 | 0.040* | |
H18B | 0.5847 | 0.0054 | 0.0935 | 0.040* | |
H18C | 0.5664 | 0.0110 | 0.1646 | 0.040* | |
C19 | 0.99095 (18) | 0.41614 (17) | 0.38237 (10) | 0.0186 (5) | |
H19 | 0.9427 | 0.4517 | 0.3540 | 0.022* | |
C20 | 1.0940 (2) | 0.38519 (17) | 0.36486 (11) | 0.0197 (5) | |
H20 | 1.1151 | 0.3979 | 0.3250 | 0.024* | |
C21 | 1.16578 (19) | 0.33523 (16) | 0.40681 (11) | 0.0189 (5) | |
C22 | 1.1334 (2) | 0.32039 (17) | 0.46494 (10) | 0.0202 (5) | |
H22 | 1.1827 | 0.2894 | 0.4952 | 0.024* | |
C23 | 1.0284 (2) | 0.35136 (17) | 0.47813 (10) | 0.0197 (5) | |
H23 | 1.0055 | 0.3393 | 0.5177 | 0.024* | |
C24 | 1.2764 (2) | 0.29491 (17) | 0.39109 (11) | 0.0207 (5) | |
C25 | 1.3919 (2) | 0.26161 (19) | 0.31079 (13) | 0.0299 (6) | |
H25A | 1.4555 | 0.2727 | 0.3424 | 0.036* | |
H25B | 1.4097 | 0.2936 | 0.2728 | 0.036* | |
C26 | 1.3796 (2) | 0.1578 (2) | 0.29920 (13) | 0.0324 (7) | |
H26A | 1.3647 | 0.1257 | 0.3372 | 0.049* | |
H26B | 1.4496 | 0.1331 | 0.2849 | 0.049* | |
H26C | 1.3165 | 0.1466 | 0.2680 | 0.049* | |
C27 | 0.80593 (19) | 0.43872 (18) | 0.59324 (10) | 0.0209 (5) | |
H27 | 0.7565 | 0.3862 | 0.5869 | 0.025* | |
C28 | 0.8365 (2) | 0.46834 (18) | 0.65220 (10) | 0.0231 (5) | |
H28 | 0.8096 | 0.4358 | 0.6858 | 0.028* | |
C29 | 0.9066 (2) | 0.54585 (18) | 0.66199 (10) | 0.0201 (5) | |
C30 | 0.9422 (2) | 0.59297 (17) | 0.61167 (10) | 0.0198 (5) | |
H30 | 0.9875 | 0.6482 | 0.6168 | 0.024* | |
C31 | 0.91003 (18) | 0.55738 (17) | 0.55378 (10) | 0.0170 (5) | |
H31 | 0.9363 | 0.5883 | 0.5194 | 0.020* | |
C32 | 0.9446 (2) | 0.5707 (2) | 0.72694 (12) | 0.0299 (6) | |
C33 | 1.0370 (3) | 0.6771 (2) | 0.79649 (13) | 0.0405 (8) | |
H33A | 1.1139 | 0.6510 | 0.8063 | 0.049* | |
H33B | 0.9866 | 0.6508 | 0.8257 | 0.049* | |
C34 | 1.0395 (3) | 0.7810 (2) | 0.80065 (15) | 0.0508 (9) | |
H34A | 1.0825 | 0.8066 | 0.7684 | 0.076* | |
H34B | 1.0757 | 0.8000 | 0.8407 | 0.076* | |
H34C | 0.9621 | 0.8056 | 0.7956 | 0.076* | |
C35 | 0.21388 (19) | 1.13039 (17) | 0.10068 (10) | 0.0174 (5) | |
C36 | 0.19317 (19) | 0.72139 (18) | −0.01494 (10) | 0.0179 (5) | |
C37 | 0.08350 (19) | 1.06111 (17) | −0.05546 (10) | 0.0176 (5) | |
H37 | 0.0508 | 1.0852 | −0.0208 | 0.021* | |
C38 | 0.05840 (19) | 1.10528 (17) | −0.11139 (10) | 0.0190 (5) | |
H38 | 0.0104 | 1.1591 | −0.1147 | 0.023* | |
C39 | 0.10433 (19) | 1.06974 (18) | −0.16219 (10) | 0.0206 (5) | |
C40 | 0.1746 (2) | 0.99209 (18) | −0.15529 (10) | 0.0214 (5) | |
H40 | 0.2072 | 0.9664 | −0.1895 | 0.026* | |
C41 | 0.19692 (19) | 0.95199 (16) | −0.09774 (10) | 0.0198 (5) | |
H41 | 0.2457 | 0.8988 | −0.0932 | 0.024* | |
C42 | 0.0829 (2) | 1.1127 (2) | −0.22474 (11) | 0.0300 (6) | |
C45 | 0.39600 (19) | 1.05091 (16) | −0.00098 (10) | 0.0171 (5) | |
H45 | 0.3466 | 1.1002 | 0.0088 | 0.020* | |
C46 | 0.48779 (19) | 1.07318 (17) | −0.03252 (10) | 0.0177 (5) | |
H46 | 0.5012 | 1.1366 | −0.0439 | 0.021* | |
C47 | 0.55998 (19) | 1.00151 (17) | −0.04724 (10) | 0.0164 (5) | |
C48 | 0.54096 (18) | 0.91019 (16) | −0.02744 (9) | 0.0155 (5) | |
H48 | 0.5908 | 0.8601 | −0.0354 | 0.019* | |
C49 | 0.44662 (19) | 0.89425 (16) | 0.00442 (10) | 0.0168 (5) | |
H49 | 0.4334 | 0.8321 | 0.0183 | 0.020* | |
C50 | 0.6519 (2) | 1.02616 (17) | −0.08666 (10) | 0.0194 (5) | |
C51 | 0.8125 (2) | 0.97295 (19) | −0.13162 (12) | 0.0264 (6) | |
H51A | 0.8743 | 0.9270 | −0.1215 | 0.032* | |
H51B | 0.8428 | 1.0370 | −0.1222 | 0.032* | |
C52 | 0.7741 (2) | 0.96643 (19) | −0.19904 (12) | 0.0327 (6) | |
H52A | 0.7474 | 0.9022 | −0.2088 | 0.049* | |
H52B | 0.8375 | 0.9815 | −0.2229 | 0.049* | |
H52C | 0.7124 | 1.0113 | −0.2091 | 0.049* | |
C53 | 0.32376 (17) | 0.93413 (18) | 0.16975 (10) | 0.0188 (5) | |
H53 | 0.3384 | 0.9977 | 0.1591 | 0.023* | |
C54 | 0.36033 (19) | 0.90350 (16) | 0.22796 (10) | 0.0191 (5) | |
H54 | 0.3992 | 0.9451 | 0.2566 | 0.023* | |
C55 | 0.33920 (19) | 0.81078 (17) | 0.24383 (10) | 0.0166 (5) | |
C56 | 0.2838 (2) | 0.75239 (16) | 0.20067 (10) | 0.0184 (5) | |
H56 | 0.2696 | 0.6883 | 0.2100 | 0.022* | |
C57 | 0.2493 (2) | 0.78891 (17) | 0.14328 (11) | 0.0195 (5) | |
H57 | 0.2103 | 0.7485 | 0.1139 | 0.023* | |
C58 | 0.3778 (2) | 0.77777 (17) | 0.30744 (11) | 0.0185 (5) | |
C59 | 0.4068 (2) | 0.64354 (18) | 0.37221 (10) | 0.0235 (6) | |
H59A | 0.3623 | 0.6730 | 0.4031 | 0.028* | |
H59B | 0.4882 | 0.6541 | 0.3845 | 0.028* | |
C60 | 0.3817 (2) | 0.53946 (18) | 0.36697 (12) | 0.0270 (6) | |
H60A | 0.3011 | 0.5302 | 0.3545 | 0.040* | |
H60B | 0.4011 | 0.5091 | 0.4066 | 0.040* | |
H60C | 0.4266 | 0.5114 | 0.3364 | 0.040* | |
C61 | 0.00253 (18) | 0.91512 (16) | 0.11036 (10) | 0.0182 (5) | |
H61 | 0.0505 | 0.9514 | 0.1384 | 0.022* | |
C62 | −0.1003 (2) | 0.88425 (17) | 0.12808 (11) | 0.0194 (5) | |
H62 | −0.1213 | 0.8978 | 0.1678 | 0.023* | |
C63 | −0.17235 (19) | 0.83302 (16) | 0.08659 (10) | 0.0180 (5) | |
C64 | −0.13892 (19) | 0.81724 (16) | 0.02847 (10) | 0.0178 (5) | |
H64 | −0.1876 | 0.7854 | −0.0016 | 0.021* | |
C65 | −0.0340 (2) | 0.84847 (16) | 0.01511 (10) | 0.0182 (5) | |
H65 | −0.0109 | 0.8358 | −0.0243 | 0.022* | |
C66 | −0.2826 (2) | 0.79347 (17) | 0.10244 (11) | 0.0202 (5) | |
C67 | −0.4022 (2) | 0.76841 (19) | 0.18211 (13) | 0.0290 (6) | |
H67A | −0.4640 | 0.7777 | 0.1491 | 0.035* | |
H67B | −0.4213 | 0.8049 | 0.2182 | 0.035* | |
C68 | −0.3946 (2) | 0.6659 (2) | 0.19839 (13) | 0.0304 (7) | |
H68A | −0.3760 | 0.6295 | 0.1628 | 0.046* | |
H68B | −0.4674 | 0.6445 | 0.2110 | 0.046* | |
H68C | −0.3355 | 0.6567 | 0.2321 | 0.046* | |
O10A | 0.02516 (19) | 1.19485 (17) | −0.22386 (9) | 0.0240 (5) | 0.848 (3) |
C43A | 0.0109 (3) | 1.2477 (2) | −0.28162 (14) | 0.0283 (8) | 0.848 (3) |
H43A | 0.0842 | 1.2504 | −0.2997 | 0.034* | 0.848 (3) |
H43B | −0.0124 | 1.3133 | −0.2733 | 0.034* | 0.848 (3) |
C44A | −0.0759 (3) | 1.2029 (3) | −0.32627 (16) | 0.0371 (9) | 0.848 (3) |
H44A | −0.0486 | 1.1411 | −0.3385 | 0.056* | 0.848 (3) |
H44B | −0.0893 | 1.2434 | −0.3624 | 0.056* | 0.848 (3) |
H44C | −0.1466 | 1.1950 | −0.3072 | 0.056* | 0.848 (3) |
O10B | −0.0138 (11) | 1.1435 (10) | −0.2357 (5) | 0.0240 (5) | 0.152 (3) |
C43B | −0.0479 (17) | 1.1714 (14) | −0.2983 (8) | 0.0283 (8) | 0.152 (3) |
H43C | −0.0055 | 1.1336 | −0.3265 | 0.034* | 0.152 (3) |
H43D | −0.1295 | 1.1583 | −0.3079 | 0.034* | 0.152 (3) |
C44B | −0.0258 (18) | 1.2750 (15) | −0.3081 (10) | 0.0371 (9) | 0.152 (3) |
H44D | −0.0559 | 1.3118 | −0.2755 | 0.056* | 0.152 (3) |
H44E | −0.0630 | 1.2946 | −0.3478 | 0.056* | 0.152 (3) |
H44F | 0.0559 | 1.2857 | −0.3074 | 0.056* | 0.152 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.01637 (14) | 0.01316 (15) | 0.01275 (13) | 0.00039 (13) | 0.00292 (10) | 0.00038 (14) |
Ni2 | 0.01665 (14) | 0.01230 (15) | 0.01285 (13) | −0.00059 (13) | 0.00284 (10) | −0.00049 (14) |
S1 | 0.0433 (4) | 0.0194 (4) | 0.0337 (4) | 0.0079 (3) | 0.0096 (3) | 0.0082 (3) |
S2 | 0.0343 (4) | 0.0205 (4) | 0.0392 (4) | 0.0096 (3) | 0.0101 (3) | 0.0100 (3) |
S3 | 0.0551 (5) | 0.0183 (4) | 0.0356 (4) | −0.0002 (3) | −0.0059 (3) | −0.0107 (3) |
S4 | 0.0351 (4) | 0.0226 (4) | 0.0403 (4) | −0.0126 (3) | 0.0125 (3) | −0.0150 (3) |
O1 | 0.0314 (10) | 0.0217 (10) | 0.0310 (9) | −0.0020 (8) | 0.0142 (8) | −0.0083 (8) |
O2 | 0.0210 (8) | 0.0181 (9) | 0.0226 (8) | 0.0008 (7) | 0.0090 (7) | 0.0008 (7) |
O3 | 0.0482 (12) | 0.0292 (11) | 0.0172 (9) | −0.0025 (9) | −0.0072 (8) | 0.0030 (8) |
O4 | 0.0292 (10) | 0.0231 (10) | 0.0146 (9) | −0.0003 (8) | 0.0002 (7) | −0.0041 (7) |
O5 | 0.0186 (9) | 0.0296 (10) | 0.0296 (9) | 0.0061 (7) | 0.0115 (7) | 0.0042 (8) |
O6 | 0.0228 (9) | 0.0282 (10) | 0.0299 (10) | 0.0086 (8) | −0.0018 (8) | −0.0048 (8) |
O7 | 0.137 (3) | 0.0784 (19) | 0.0166 (11) | −0.0631 (18) | −0.0155 (13) | 0.0099 (12) |
O8 | 0.0463 (12) | 0.0387 (12) | 0.0185 (9) | −0.0125 (10) | 0.0012 (8) | −0.0077 (8) |
O9 | 0.0433 (12) | 0.0568 (14) | 0.0188 (9) | 0.0158 (10) | 0.0054 (8) | 0.0049 (9) |
O10A | 0.0332 (13) | 0.0233 (14) | 0.0157 (10) | 0.0060 (10) | 0.0025 (9) | 0.0063 (9) |
O11 | 0.0292 (10) | 0.0182 (9) | 0.0325 (9) | −0.0003 (7) | 0.0136 (8) | 0.0055 (8) |
O12 | 0.0204 (8) | 0.0198 (10) | 0.0216 (8) | 0.0006 (7) | 0.0083 (7) | 0.0011 (7) |
O13 | 0.0405 (11) | 0.0256 (10) | 0.0175 (9) | 0.0025 (8) | −0.0033 (8) | −0.0038 (8) |
O14 | 0.0256 (10) | 0.0233 (10) | 0.0142 (8) | 0.0013 (7) | 0.0010 (7) | 0.0040 (7) |
O15 | 0.0220 (9) | 0.0267 (10) | 0.0278 (9) | −0.0090 (7) | −0.0030 (8) | 0.0029 (8) |
O16 | 0.0174 (9) | 0.0329 (11) | 0.0306 (10) | −0.0067 (8) | 0.0099 (7) | −0.0073 (8) |
N1 | 0.0215 (11) | 0.0176 (12) | 0.0156 (10) | −0.0010 (9) | 0.0040 (8) | −0.0007 (8) |
N2 | 0.0200 (11) | 0.0161 (11) | 0.0184 (10) | −0.0001 (8) | 0.0051 (8) | 0.0000 (8) |
N3 | 0.0167 (10) | 0.0156 (10) | 0.0138 (9) | 0.0003 (8) | 0.0004 (8) | −0.0009 (7) |
N4 | 0.0154 (10) | 0.0162 (11) | 0.0173 (10) | −0.0001 (8) | 0.0025 (8) | 0.0018 (8) |
N5 | 0.0178 (10) | 0.0156 (10) | 0.0181 (10) | 0.0023 (8) | 0.0024 (8) | −0.0003 (8) |
N6 | 0.0176 (10) | 0.0185 (11) | 0.0134 (9) | 0.0024 (8) | 0.0021 (8) | 0.0029 (8) |
N7 | 0.0184 (10) | 0.0167 (11) | 0.0177 (10) | 0.0002 (8) | 0.0019 (8) | 0.0002 (8) |
N8 | 0.0193 (11) | 0.0170 (11) | 0.0175 (10) | −0.0011 (8) | 0.0030 (8) | −0.0007 (8) |
N9 | 0.0176 (10) | 0.0164 (11) | 0.0146 (9) | −0.0028 (8) | 0.0013 (8) | −0.0014 (8) |
N10 | 0.0178 (10) | 0.0153 (10) | 0.0131 (9) | −0.0003 (8) | 0.0015 (8) | 0.0018 (7) |
N11 | 0.0172 (10) | 0.0138 (10) | 0.0167 (10) | −0.0002 (8) | 0.0043 (8) | −0.0004 (8) |
N12 | 0.0198 (10) | 0.0152 (10) | 0.0154 (9) | 0.0010 (8) | 0.0031 (8) | 0.0003 (8) |
C1 | 0.0218 (13) | 0.0149 (13) | 0.0137 (11) | −0.0036 (10) | 0.0067 (9) | −0.0010 (9) |
C2 | 0.0181 (12) | 0.0241 (14) | 0.0142 (11) | −0.0013 (10) | 0.0052 (9) | −0.0022 (10) |
C3 | 0.0209 (13) | 0.0135 (12) | 0.0155 (11) | 0.0002 (9) | 0.0010 (9) | −0.0025 (9) |
C4 | 0.0158 (11) | 0.0159 (13) | 0.0164 (11) | 0.0006 (9) | 0.0013 (9) | 0.0005 (9) |
C5 | 0.0177 (12) | 0.0171 (12) | 0.0153 (11) | 0.0009 (9) | −0.0005 (9) | 0.0020 (9) |
C6 | 0.0203 (12) | 0.0133 (12) | 0.0196 (12) | −0.0002 (9) | 0.0007 (10) | −0.0042 (9) |
C7 | 0.0197 (12) | 0.0142 (12) | 0.0189 (12) | −0.0020 (9) | 0.0034 (9) | 0.0007 (9) |
C8 | 0.0227 (13) | 0.0187 (13) | 0.0172 (11) | −0.0005 (10) | 0.0033 (10) | −0.0002 (10) |
C9 | 0.0263 (14) | 0.0237 (14) | 0.0316 (14) | 0.0027 (11) | 0.0167 (11) | −0.0004 (11) |
C10 | 0.0505 (18) | 0.0325 (17) | 0.0274 (14) | −0.0020 (13) | 0.0160 (13) | 0.0015 (12) |
C11 | 0.0183 (11) | 0.0159 (12) | 0.0216 (11) | 0.0001 (10) | 0.0009 (9) | −0.0006 (11) |
C12 | 0.0196 (12) | 0.0187 (13) | 0.0208 (12) | −0.0003 (9) | 0.0009 (9) | 0.0030 (9) |
C13 | 0.0148 (12) | 0.0175 (13) | 0.0175 (11) | −0.0048 (9) | 0.0047 (9) | 0.0001 (10) |
C14 | 0.0269 (13) | 0.0133 (12) | 0.0170 (12) | −0.0011 (10) | 0.0047 (10) | −0.0001 (9) |
C15 | 0.0250 (13) | 0.0159 (13) | 0.0171 (12) | 0.0001 (10) | 0.0027 (10) | 0.0021 (9) |
C16 | 0.0171 (12) | 0.0252 (14) | 0.0158 (12) | −0.0034 (10) | 0.0023 (10) | 0.0000 (10) |
C17 | 0.0279 (14) | 0.0303 (15) | 0.0127 (11) | −0.0013 (11) | −0.0024 (10) | −0.0058 (10) |
C18 | 0.0316 (14) | 0.0283 (15) | 0.0208 (13) | −0.0067 (11) | 0.0009 (11) | −0.0094 (11) |
C19 | 0.0194 (11) | 0.0186 (13) | 0.0176 (11) | −0.0003 (10) | 0.0016 (9) | 0.0034 (10) |
C20 | 0.0181 (12) | 0.0219 (14) | 0.0196 (12) | −0.0013 (10) | 0.0045 (10) | 0.0019 (10) |
C21 | 0.0167 (12) | 0.0142 (12) | 0.0259 (13) | −0.0017 (10) | 0.0025 (10) | −0.0033 (10) |
C22 | 0.0223 (13) | 0.0171 (13) | 0.0205 (12) | 0.0000 (10) | −0.0012 (10) | 0.0001 (10) |
C23 | 0.0231 (13) | 0.0213 (13) | 0.0143 (11) | 0.0001 (10) | −0.0001 (9) | 0.0004 (9) |
C24 | 0.0180 (12) | 0.0146 (12) | 0.0292 (13) | −0.0029 (10) | 0.0008 (10) | −0.0029 (10) |
C25 | 0.0203 (13) | 0.0334 (16) | 0.0382 (16) | 0.0065 (11) | 0.0138 (12) | 0.0015 (12) |
C26 | 0.0297 (16) | 0.0347 (17) | 0.0333 (15) | 0.0040 (12) | 0.0055 (12) | −0.0047 (13) |
C27 | 0.0234 (12) | 0.0205 (13) | 0.0190 (11) | −0.0028 (11) | 0.0036 (9) | 0.0002 (11) |
C28 | 0.0278 (13) | 0.0263 (14) | 0.0156 (11) | −0.0060 (11) | 0.0051 (10) | 0.0051 (10) |
C29 | 0.0224 (13) | 0.0257 (14) | 0.0123 (11) | 0.0020 (10) | 0.0018 (9) | 0.0019 (10) |
C30 | 0.0201 (12) | 0.0183 (13) | 0.0209 (12) | 0.0007 (10) | 0.0012 (10) | 0.0014 (10) |
C31 | 0.0160 (11) | 0.0189 (13) | 0.0165 (11) | 0.0005 (10) | 0.0040 (9) | 0.0033 (9) |
C32 | 0.0371 (16) | 0.0345 (17) | 0.0172 (13) | −0.0074 (13) | −0.0020 (11) | 0.0002 (12) |
C33 | 0.049 (2) | 0.048 (2) | 0.0234 (15) | −0.0081 (15) | −0.0009 (14) | −0.0140 (13) |
C34 | 0.062 (2) | 0.053 (2) | 0.0388 (18) | −0.0131 (18) | 0.0174 (17) | −0.0237 (16) |
C35 | 0.0209 (13) | 0.0181 (14) | 0.0135 (11) | 0.0022 (10) | 0.0029 (9) | 0.0017 (10) |
C36 | 0.0167 (12) | 0.0209 (14) | 0.0167 (11) | −0.0015 (10) | 0.0048 (9) | −0.0028 (10) |
C37 | 0.0178 (12) | 0.0194 (13) | 0.0160 (11) | −0.0018 (10) | 0.0037 (9) | −0.0016 (9) |
C38 | 0.0161 (12) | 0.0201 (13) | 0.0211 (12) | 0.0005 (10) | 0.0027 (9) | 0.0022 (10) |
C39 | 0.0175 (12) | 0.0278 (14) | 0.0163 (12) | −0.0057 (10) | 0.0015 (9) | 0.0025 (10) |
C40 | 0.0229 (13) | 0.0274 (14) | 0.0145 (11) | −0.0013 (10) | 0.0051 (10) | −0.0025 (10) |
C41 | 0.0237 (12) | 0.0179 (14) | 0.0180 (11) | 0.0023 (10) | 0.0032 (9) | −0.0022 (9) |
C42 | 0.0255 (14) | 0.0467 (18) | 0.0182 (12) | 0.0082 (13) | 0.0050 (11) | 0.0045 (13) |
C43A | 0.0359 (18) | 0.0305 (19) | 0.0179 (16) | 0.0089 (15) | −0.0016 (14) | 0.0107 (14) |
C44A | 0.042 (2) | 0.042 (2) | 0.0256 (18) | 0.0102 (16) | −0.0034 (15) | −0.0008 (16) |
C45 | 0.0186 (12) | 0.0148 (12) | 0.0177 (11) | 0.0013 (9) | 0.0013 (9) | −0.0018 (9) |
C46 | 0.0224 (12) | 0.0141 (12) | 0.0162 (11) | 0.0000 (10) | −0.0004 (9) | 0.0021 (9) |
C47 | 0.0152 (11) | 0.0201 (12) | 0.0132 (11) | −0.0019 (10) | −0.0017 (9) | 0.0004 (9) |
C48 | 0.0158 (11) | 0.0161 (13) | 0.0142 (10) | 0.0014 (9) | −0.0007 (8) | 0.0002 (9) |
C49 | 0.0203 (12) | 0.0143 (12) | 0.0156 (11) | −0.0015 (9) | 0.0006 (9) | 0.0004 (9) |
C50 | 0.0215 (13) | 0.0194 (14) | 0.0173 (12) | −0.0031 (10) | 0.0011 (10) | 0.0000 (10) |
C51 | 0.0226 (13) | 0.0252 (14) | 0.0334 (14) | 0.0000 (11) | 0.0140 (11) | −0.0006 (11) |
C52 | 0.0442 (17) | 0.0279 (15) | 0.0280 (14) | −0.0012 (12) | 0.0139 (13) | 0.0006 (11) |
C53 | 0.0194 (11) | 0.0146 (12) | 0.0230 (11) | −0.0007 (11) | 0.0045 (9) | 0.0029 (11) |
C54 | 0.0171 (12) | 0.0198 (13) | 0.0199 (12) | −0.0004 (9) | −0.0006 (9) | −0.0022 (9) |
C55 | 0.0146 (11) | 0.0202 (13) | 0.0156 (11) | 0.0050 (10) | 0.0054 (9) | 0.0004 (10) |
C56 | 0.0268 (13) | 0.0132 (12) | 0.0155 (12) | 0.0027 (10) | 0.0038 (10) | −0.0003 (9) |
C57 | 0.0232 (13) | 0.0165 (13) | 0.0189 (12) | −0.0008 (10) | 0.0026 (10) | −0.0023 (10) |
C58 | 0.0162 (12) | 0.0206 (14) | 0.0188 (13) | 0.0041 (10) | 0.0025 (10) | −0.0017 (10) |
C59 | 0.0258 (14) | 0.0285 (15) | 0.0158 (12) | 0.0030 (11) | −0.0013 (10) | 0.0086 (10) |
C60 | 0.0317 (14) | 0.0245 (14) | 0.0240 (13) | 0.0050 (11) | −0.0008 (11) | 0.0059 (11) |
C61 | 0.0179 (11) | 0.0184 (13) | 0.0182 (11) | −0.0019 (10) | 0.0010 (9) | −0.0030 (10) |
C62 | 0.0217 (13) | 0.0193 (13) | 0.0172 (11) | 0.0021 (10) | 0.0026 (10) | −0.0023 (10) |
C63 | 0.0165 (12) | 0.0143 (12) | 0.0228 (12) | 0.0027 (10) | −0.0004 (9) | 0.0016 (10) |
C64 | 0.0185 (12) | 0.0154 (12) | 0.0187 (11) | −0.0014 (10) | −0.0028 (9) | −0.0008 (9) |
C65 | 0.0230 (13) | 0.0181 (13) | 0.0131 (11) | 0.0023 (10) | −0.0010 (9) | −0.0010 (9) |
C66 | 0.0210 (13) | 0.0160 (12) | 0.0241 (13) | 0.0048 (10) | 0.0046 (10) | 0.0025 (10) |
C67 | 0.0194 (13) | 0.0324 (16) | 0.0372 (15) | −0.0061 (11) | 0.0147 (11) | −0.0098 (12) |
C68 | 0.0221 (14) | 0.0386 (17) | 0.0315 (15) | 0.0002 (12) | 0.0080 (12) | 0.0044 (12) |
O10B | 0.0332 (13) | 0.0233 (14) | 0.0157 (10) | 0.0060 (10) | 0.0025 (9) | 0.0063 (9) |
C43B | 0.0359 (18) | 0.0305 (19) | 0.0179 (16) | 0.0089 (15) | −0.0016 (14) | 0.0107 (14) |
C44B | 0.042 (2) | 0.042 (2) | 0.0256 (18) | 0.0102 (16) | −0.0034 (15) | −0.0008 (16) |
Ni1—N1 | 2.033 (2) | C21—C22 | 1.383 (3) |
Ni1—N2 | 2.058 (2) | C21—C24 | 1.501 (3) |
Ni1—N6 | 2.1205 (19) | C22—C23 | 1.378 (3) |
Ni1—N5 | 2.1270 (18) | C22—H22 | 0.9500 |
Ni1—N4 | 2.1379 (19) | C23—H23 | 0.9500 |
Ni1—N3 | 2.1494 (18) | C25—C26 | 1.497 (4) |
Ni2—N7 | 2.039 (2) | C25—H25A | 0.9900 |
Ni2—N8 | 2.051 (2) | C25—H25B | 0.9900 |
Ni2—N9 | 2.1207 (19) | C26—H26A | 0.9800 |
Ni2—N12 | 2.1236 (19) | C26—H26B | 0.9800 |
Ni2—N11 | 2.1384 (19) | C26—H26C | 0.9800 |
Ni2—N10 | 2.1460 (18) | C27—C28 | 1.377 (3) |
S1—C1 | 1.631 (2) | C27—H27 | 0.9500 |
S2—C2 | 1.631 (3) | C28—C29 | 1.383 (3) |
S3—C35 | 1.631 (2) | C28—H28 | 0.9500 |
S4—C36 | 1.635 (3) | C29—C30 | 1.390 (3) |
O1—C8 | 1.214 (3) | C29—C32 | 1.498 (3) |
O2—C8 | 1.327 (3) | C30—C31 | 1.388 (3) |
O2—C9 | 1.454 (3) | C30—H30 | 0.9500 |
O3—C16 | 1.199 (3) | C31—H31 | 0.9500 |
O4—C16 | 1.330 (3) | C33—C34 | 1.474 (4) |
O4—C17 | 1.465 (3) | C33—H33A | 0.9900 |
O5—C24 | 1.339 (3) | C33—H33B | 0.9900 |
O5—C25 | 1.465 (3) | C34—H34A | 0.9800 |
O6—C24 | 1.203 (3) | C34—H34B | 0.9800 |
O7—C32 | 1.203 (3) | C34—H34C | 0.9800 |
O8—C32 | 1.309 (3) | C37—C38 | 1.386 (3) |
O8—C33 | 1.469 (3) | C37—H37 | 0.9500 |
O9—C42 | 1.206 (3) | C38—C39 | 1.382 (3) |
O10A—C42 | 1.351 (3) | C38—H38 | 0.9500 |
O10A—C43A | 1.470 (3) | C39—C40 | 1.380 (3) |
O11—C50 | 1.206 (3) | C39—C42 | 1.503 (3) |
O12—C50 | 1.329 (3) | C40—C41 | 1.389 (3) |
O12—C51 | 1.454 (3) | C40—H40 | 0.9500 |
O13—C58 | 1.204 (3) | C41—H41 | 0.9500 |
O14—C58 | 1.332 (3) | C42—O10B | 1.230 (13) |
O14—C59 | 1.469 (3) | C43A—C44A | 1.496 (5) |
O15—C66 | 1.205 (3) | C43A—H43A | 0.9900 |
O16—C66 | 1.338 (3) | C43A—H43B | 0.9900 |
O16—C67 | 1.466 (3) | C44A—H44A | 0.9800 |
N1—C1 | 1.158 (3) | C44A—H44B | 0.9800 |
N2—C2 | 1.169 (3) | C44A—H44C | 0.9800 |
N3—C3 | 1.344 (3) | C45—C46 | 1.381 (3) |
N3—C7 | 1.345 (3) | C45—H45 | 0.9500 |
N4—C15 | 1.334 (3) | C46—C47 | 1.386 (3) |
N4—C11 | 1.344 (3) | C46—H46 | 0.9500 |
N5—C19 | 1.341 (3) | C47—C48 | 1.390 (3) |
N5—C23 | 1.346 (3) | C47—C50 | 1.496 (3) |
N6—C31 | 1.338 (3) | C48—C49 | 1.393 (3) |
N6—C27 | 1.348 (3) | C48—H48 | 0.9500 |
N7—C35 | 1.155 (3) | C49—H49 | 0.9500 |
N8—C36 | 1.160 (3) | C51—C52 | 1.511 (4) |
N9—C37 | 1.338 (3) | C51—H51A | 0.9900 |
N9—C41 | 1.344 (3) | C51—H51B | 0.9900 |
N10—C49 | 1.339 (3) | C52—H52A | 0.9800 |
N10—C45 | 1.344 (3) | C52—H52B | 0.9800 |
N11—C57 | 1.337 (3) | C52—H52C | 0.9800 |
N11—C53 | 1.348 (3) | C53—C54 | 1.381 (3) |
N12—C61 | 1.342 (3) | C53—H53 | 0.9500 |
N12—C65 | 1.343 (3) | C54—C55 | 1.387 (3) |
C3—C4 | 1.398 (3) | C54—H54 | 0.9500 |
C3—H3 | 0.9500 | C55—C56 | 1.378 (3) |
C4—C5 | 1.381 (3) | C55—C58 | 1.504 (3) |
C4—H4 | 0.9500 | C56—C57 | 1.389 (3) |
C5—C6 | 1.392 (3) | C56—H56 | 0.9500 |
C5—C8 | 1.499 (3) | C57—H57 | 0.9500 |
C6—C7 | 1.382 (3) | C59—C60 | 1.506 (3) |
C6—H6 | 0.9500 | C59—H59A | 0.9900 |
C7—H7 | 0.9500 | C59—H59B | 0.9900 |
C9—C10 | 1.510 (4) | C60—H60A | 0.9800 |
C9—H9A | 0.9900 | C60—H60B | 0.9800 |
C9—H9B | 0.9900 | C60—H60C | 0.9800 |
C10—H10A | 0.9800 | C61—C62 | 1.386 (3) |
C10—H10B | 0.9800 | C61—H61 | 0.9500 |
C10—H10C | 0.9800 | C62—C63 | 1.394 (3) |
C11—C12 | 1.381 (3) | C62—H62 | 0.9500 |
C11—H11 | 0.9500 | C63—C64 | 1.390 (3) |
C12—C13 | 1.391 (3) | C63—C66 | 1.494 (3) |
C12—H12 | 0.9500 | C64—C65 | 1.379 (3) |
C13—C14 | 1.383 (3) | C64—H64 | 0.9500 |
C13—C16 | 1.504 (3) | C65—H65 | 0.9500 |
C14—C15 | 1.384 (3) | C67—C68 | 1.495 (4) |
C14—H14 | 0.9500 | C67—H67A | 0.9900 |
C15—H15 | 0.9500 | C67—H67B | 0.9900 |
C17—C18 | 1.502 (3) | C68—H68A | 0.9800 |
C17—H17A | 0.9900 | C68—H68B | 0.9800 |
C17—H17B | 0.9900 | C68—H68C | 0.9800 |
C18—H18A | 0.9800 | O10B—C43B | 1.45 (2) |
C18—H18B | 0.9800 | C43B—C44B | 1.51 (3) |
C18—H18C | 0.9800 | C43B—H43C | 0.9900 |
C19—C20 | 1.388 (3) | C43B—H43D | 0.9900 |
C19—H19 | 0.9500 | C44B—H44D | 0.9800 |
C20—C21 | 1.389 (3) | C44B—H44E | 0.9800 |
C20—H20 | 0.9500 | C44B—H44F | 0.9800 |
N1—Ni1—N2 | 177.31 (8) | C28—C27—H27 | 118.8 |
N1—Ni1—N6 | 90.79 (8) | C27—C28—C29 | 119.3 (2) |
N2—Ni1—N6 | 90.00 (7) | C27—C28—H28 | 120.3 |
N1—Ni1—N5 | 89.58 (7) | C29—C28—H28 | 120.3 |
N2—Ni1—N5 | 87.83 (7) | C28—C29—C30 | 118.7 (2) |
N6—Ni1—N5 | 91.56 (7) | C28—C29—C32 | 117.3 (2) |
N1—Ni1—N4 | 89.14 (7) | C30—C29—C32 | 123.9 (2) |
N2—Ni1—N4 | 90.18 (8) | C29—C30—C31 | 118.4 (2) |
N6—Ni1—N4 | 177.52 (8) | C29—C30—H30 | 120.8 |
N5—Ni1—N4 | 90.92 (7) | C31—C30—H30 | 120.8 |
N1—Ni1—N3 | 91.36 (7) | N6—C31—C30 | 122.9 (2) |
N2—Ni1—N3 | 91.27 (7) | N6—C31—H31 | 118.5 |
N6—Ni1—N3 | 84.43 (7) | C30—C31—H31 | 118.5 |
N5—Ni1—N3 | 175.89 (7) | O7—C32—O8 | 124.8 (3) |
N4—Ni1—N3 | 93.09 (7) | O7—C32—C29 | 121.1 (3) |
N7—Ni2—N8 | 177.68 (8) | O8—C32—C29 | 114.0 (2) |
N7—Ni2—N9 | 89.90 (8) | O8—C33—C34 | 107.2 (3) |
N8—Ni2—N9 | 90.54 (7) | O8—C33—H33A | 110.3 |
N7—Ni2—N12 | 90.24 (7) | C34—C33—H33A | 110.3 |
N8—Ni2—N12 | 87.47 (7) | O8—C33—H33B | 110.3 |
N9—Ni2—N12 | 91.41 (7) | C34—C33—H33B | 110.3 |
N7—Ni2—N11 | 88.37 (7) | H33A—C33—H33B | 108.5 |
N8—Ni2—N11 | 91.29 (7) | C33—C34—H34A | 109.5 |
N9—Ni2—N11 | 176.80 (8) | C33—C34—H34B | 109.5 |
N12—Ni2—N11 | 91.29 (7) | H34A—C34—H34B | 109.5 |
N7—Ni2—N10 | 91.46 (7) | C33—C34—H34C | 109.5 |
N8—Ni2—N10 | 90.84 (7) | H34A—C34—H34C | 109.5 |
N9—Ni2—N10 | 85.39 (7) | H34B—C34—H34C | 109.5 |
N12—Ni2—N10 | 176.37 (7) | N7—C35—S3 | 177.9 (2) |
N11—Ni2—N10 | 91.96 (7) | N8—C36—S4 | 179.3 (2) |
C8—O2—C9 | 115.43 (18) | N9—C37—C38 | 122.8 (2) |
C16—O4—C17 | 116.71 (19) | N9—C37—H37 | 118.6 |
C24—O5—C25 | 116.07 (19) | C38—C37—H37 | 118.6 |
C32—O8—C33 | 115.1 (2) | C39—C38—C37 | 118.9 (2) |
C42—O10A—C43A | 116.4 (2) | C39—C38—H38 | 120.6 |
C50—O12—C51 | 115.32 (18) | C37—C38—H38 | 120.6 |
C58—O14—C59 | 116.30 (19) | C40—C39—C38 | 118.8 (2) |
C66—O16—C67 | 116.14 (19) | C40—C39—C42 | 118.2 (2) |
C1—N1—Ni1 | 157.36 (19) | C38—C39—C42 | 123.0 (2) |
C2—N2—Ni1 | 161.72 (19) | C39—C40—C41 | 119.2 (2) |
C3—N3—C7 | 118.03 (19) | C39—C40—H40 | 120.4 |
C3—N3—Ni1 | 121.37 (15) | C41—C40—H40 | 120.4 |
C7—N3—Ni1 | 118.16 (15) | N9—C41—C40 | 122.2 (2) |
C15—N4—C11 | 117.4 (2) | N9—C41—H41 | 118.9 |
C15—N4—Ni1 | 120.34 (15) | C40—C41—H41 | 118.9 |
C11—N4—Ni1 | 122.17 (16) | O9—C42—O10B | 112.5 (6) |
C19—N5—C23 | 117.7 (2) | O9—C42—O10A | 125.5 (2) |
C19—N5—Ni1 | 120.12 (15) | O9—C42—C39 | 122.2 (2) |
C23—N5—Ni1 | 121.82 (15) | O10B—C42—C39 | 113.4 (6) |
C31—N6—C27 | 118.0 (2) | O10A—C42—C39 | 112.2 (2) |
C31—N6—Ni1 | 123.47 (15) | O10A—C43A—C44A | 111.5 (3) |
C27—N6—Ni1 | 118.43 (15) | O10A—C43A—H43A | 109.3 |
C35—N7—Ni2 | 160.08 (19) | C44A—C43A—H43A | 109.3 |
C36—N8—Ni2 | 161.70 (19) | O10A—C43A—H43B | 109.3 |
C37—N9—C41 | 118.2 (2) | C44A—C43A—H43B | 109.3 |
C37—N9—Ni2 | 122.44 (15) | H43A—C43A—H43B | 108.0 |
C41—N9—Ni2 | 118.99 (15) | N10—C45—C46 | 122.8 (2) |
C49—N10—C45 | 117.92 (19) | N10—C45—H45 | 118.6 |
C49—N10—Ni2 | 121.28 (15) | C46—C45—H45 | 118.6 |
C45—N10—Ni2 | 118.69 (15) | C45—C46—C47 | 118.9 (2) |
C57—N11—C53 | 117.3 (2) | C45—C46—H46 | 120.5 |
C57—N11—Ni2 | 120.47 (15) | C47—C46—H46 | 120.5 |
C53—N11—Ni2 | 122.23 (16) | C46—C47—C48 | 119.1 (2) |
C61—N12—C65 | 117.9 (2) | C46—C47—C50 | 117.7 (2) |
C61—N12—Ni2 | 118.70 (15) | C48—C47—C50 | 123.2 (2) |
C65—N12—Ni2 | 123.16 (15) | C47—C48—C49 | 118.0 (2) |
N1—C1—S1 | 177.2 (2) | C47—C48—H48 | 121.0 |
N2—C2—S2 | 178.9 (2) | C49—C48—H48 | 121.0 |
N3—C3—C4 | 122.8 (2) | N10—C49—C48 | 123.1 (2) |
N3—C3—H3 | 118.6 | N10—C49—H49 | 118.4 |
C4—C3—H3 | 118.6 | C48—C49—H49 | 118.4 |
C5—C4—C3 | 118.1 (2) | O11—C50—O12 | 125.0 (2) |
C5—C4—H4 | 120.9 | O11—C50—C47 | 122.6 (2) |
C3—C4—H4 | 120.9 | O12—C50—C47 | 112.33 (19) |
C4—C5—C6 | 119.5 (2) | O12—C51—C52 | 111.6 (2) |
C4—C5—C8 | 123.2 (2) | O12—C51—H51A | 109.3 |
C6—C5—C8 | 117.3 (2) | C52—C51—H51A | 109.3 |
C7—C6—C5 | 118.6 (2) | O12—C51—H51B | 109.3 |
C7—C6—H6 | 120.7 | C52—C51—H51B | 109.3 |
C5—C6—H6 | 120.7 | H51A—C51—H51B | 108.0 |
N3—C7—C6 | 122.8 (2) | C51—C52—H52A | 109.5 |
N3—C7—H7 | 118.6 | C51—C52—H52B | 109.5 |
C6—C7—H7 | 118.6 | H52A—C52—H52B | 109.5 |
O1—C8—O2 | 125.1 (2) | C51—C52—H52C | 109.5 |
O1—C8—C5 | 122.5 (2) | H52A—C52—H52C | 109.5 |
O2—C8—C5 | 112.29 (19) | H52B—C52—H52C | 109.5 |
O2—C9—C10 | 111.7 (2) | N11—C53—C54 | 123.1 (2) |
O2—C9—H9A | 109.3 | N11—C53—H53 | 118.4 |
C10—C9—H9A | 109.3 | C54—C53—H53 | 118.4 |
O2—C9—H9B | 109.3 | C53—C54—C55 | 118.8 (2) |
C10—C9—H9B | 109.3 | C53—C54—H54 | 120.6 |
H9A—C9—H9B | 107.9 | C55—C54—H54 | 120.6 |
C9—C10—H10A | 109.5 | C56—C55—C54 | 118.8 (2) |
C9—C10—H10B | 109.5 | C56—C55—C58 | 122.5 (2) |
H10A—C10—H10B | 109.5 | C54—C55—C58 | 118.8 (2) |
C9—C10—H10C | 109.5 | C55—C56—C57 | 118.9 (2) |
H10A—C10—H10C | 109.5 | C55—C56—H56 | 120.6 |
H10B—C10—H10C | 109.5 | C57—C56—H56 | 120.6 |
N4—C11—C12 | 123.0 (2) | N11—C57—C56 | 123.2 (2) |
N4—C11—H11 | 118.5 | N11—C57—H57 | 118.4 |
C12—C11—H11 | 118.5 | C56—C57—H57 | 118.4 |
C11—C12—C13 | 118.8 (2) | O13—C58—O14 | 125.1 (2) |
C11—C12—H12 | 120.6 | O13—C58—C55 | 123.5 (2) |
C13—C12—H12 | 120.6 | O14—C58—C55 | 111.4 (2) |
C14—C13—C12 | 118.6 (2) | O14—C59—C60 | 106.3 (2) |
C14—C13—C16 | 122.0 (2) | O14—C59—H59A | 110.5 |
C12—C13—C16 | 119.4 (2) | C60—C59—H59A | 110.5 |
C13—C14—C15 | 118.5 (2) | O14—C59—H59B | 110.5 |
C13—C14—H14 | 120.7 | C60—C59—H59B | 110.5 |
C15—C14—H14 | 120.7 | H59A—C59—H59B | 108.7 |
N4—C15—C14 | 123.6 (2) | C59—C60—H60A | 109.5 |
N4—C15—H15 | 118.2 | C59—C60—H60B | 109.5 |
C14—C15—H15 | 118.2 | H60A—C60—H60B | 109.5 |
O3—C16—O4 | 125.6 (2) | C59—C60—H60C | 109.5 |
O3—C16—C13 | 123.6 (2) | H60A—C60—H60C | 109.5 |
O4—C16—C13 | 110.8 (2) | H60B—C60—H60C | 109.5 |
O4—C17—C18 | 106.20 (19) | N12—C61—C62 | 122.8 (2) |
O4—C17—H17A | 110.5 | N12—C61—H61 | 118.6 |
C18—C17—H17A | 110.5 | C62—C61—H61 | 118.6 |
O4—C17—H17B | 110.5 | C61—C62—C63 | 118.9 (2) |
C18—C17—H17B | 110.5 | C61—C62—H62 | 120.5 |
H17A—C17—H17B | 108.7 | C63—C62—H62 | 120.5 |
C17—C18—H18A | 109.5 | C64—C63—C62 | 118.3 (2) |
C17—C18—H18B | 109.5 | C64—C63—C66 | 119.0 (2) |
H18A—C18—H18B | 109.5 | C62—C63—C66 | 122.7 (2) |
C17—C18—H18C | 109.5 | C65—C64—C63 | 119.0 (2) |
H18A—C18—H18C | 109.5 | C65—C64—H64 | 120.5 |
H18B—C18—H18C | 109.5 | C63—C64—H64 | 120.5 |
N5—C19—C20 | 122.7 (2) | N12—C65—C64 | 123.1 (2) |
N5—C19—H19 | 118.6 | N12—C65—H65 | 118.5 |
C20—C19—H19 | 118.6 | C64—C65—H65 | 118.5 |
C19—C20—C21 | 118.6 (2) | O15—C66—O16 | 124.8 (2) |
C19—C20—H20 | 120.7 | O15—C66—C63 | 123.4 (2) |
C21—C20—H20 | 120.7 | O16—C66—C63 | 111.8 (2) |
C22—C21—C20 | 118.9 (2) | O16—C67—C68 | 112.2 (2) |
C22—C21—C24 | 118.6 (2) | O16—C67—H67A | 109.2 |
C20—C21—C24 | 122.5 (2) | C68—C67—H67A | 109.2 |
C23—C22—C21 | 118.7 (2) | O16—C67—H67B | 109.2 |
C23—C22—H22 | 120.6 | C68—C67—H67B | 109.2 |
C21—C22—H22 | 120.6 | H67A—C67—H67B | 107.9 |
N5—C23—C22 | 123.1 (2) | C67—C68—H68A | 109.5 |
N5—C23—H23 | 118.4 | C67—C68—H68B | 109.5 |
C22—C23—H23 | 118.4 | H68A—C68—H68B | 109.5 |
O6—C24—O5 | 124.8 (2) | C67—C68—H68C | 109.5 |
O6—C24—C21 | 123.4 (2) | H68A—C68—H68C | 109.5 |
O5—C24—C21 | 111.8 (2) | H68B—C68—H68C | 109.5 |
O5—C25—C26 | 111.4 (2) | C42—O10B—C43B | 117.0 (12) |
O5—C25—H25A | 109.4 | C44B—C43B—O10B | 111.3 (17) |
C26—C25—H25A | 109.4 | C44B—C43B—H43C | 109.4 |
O5—C25—H25B | 109.4 | O10B—C43B—H43C | 109.4 |
C26—C25—H25B | 109.4 | C44B—C43B—H43D | 109.4 |
H25A—C25—H25B | 108.0 | O10B—C43B—H43D | 109.4 |
C25—C26—H26A | 109.5 | H43C—C43B—H43D | 108.0 |
C25—C26—H26B | 109.5 | C43B—C44B—H44D | 109.5 |
H26A—C26—H26B | 109.5 | C43B—C44B—H44E | 109.5 |
C25—C26—H26C | 109.5 | H44D—C44B—H44E | 109.5 |
H26A—C26—H26C | 109.5 | C43B—C44B—H44F | 109.5 |
H26B—C26—H26C | 109.5 | H44D—C44B—H44F | 109.5 |
N6—C27—C28 | 122.5 (2) | H44E—C44B—H44F | 109.5 |
N6—C27—H27 | 118.8 | ||
N6—Ni1—N1—C1 | −98.7 (5) | C12—C13—C16—O4 | −167.0 (2) |
N5—Ni1—N1—C1 | 169.7 (5) | C16—O4—C17—C18 | 173.5 (2) |
N4—Ni1—N1—C1 | 78.8 (5) | C23—N5—C19—C20 | 3.1 (3) |
N3—Ni1—N1—C1 | −14.3 (5) | Ni1—N5—C19—C20 | −170.64 (18) |
N6—Ni1—N2—C2 | −102.9 (6) | N5—C19—C20—C21 | −1.6 (4) |
N5—Ni1—N2—C2 | −11.3 (6) | C19—C20—C21—C22 | −1.8 (4) |
N4—Ni1—N2—C2 | 79.6 (6) | C19—C20—C21—C24 | 177.0 (2) |
N3—Ni1—N2—C2 | 172.7 (6) | C20—C21—C22—C23 | 3.4 (3) |
N1—Ni1—N3—C3 | 161.16 (17) | C24—C21—C22—C23 | −175.4 (2) |
N2—Ni1—N3—C3 | −18.30 (17) | C19—N5—C23—C22 | −1.3 (3) |
N6—Ni1—N3—C3 | −108.17 (17) | Ni1—N5—C23—C22 | 172.33 (18) |
N4—Ni1—N3—C3 | 71.96 (17) | C21—C22—C23—N5 | −2.0 (4) |
N1—Ni1—N3—C7 | −36.94 (16) | C25—O5—C24—O6 | 1.0 (3) |
N2—Ni1—N3—C7 | 143.60 (16) | C25—O5—C24—C21 | −178.0 (2) |
N6—Ni1—N3—C7 | 53.72 (16) | C22—C21—C24—O6 | −8.7 (4) |
N4—Ni1—N3—C7 | −126.15 (16) | C20—C21—C24—O6 | 172.6 (2) |
N1—Ni1—N4—C15 | 149.39 (18) | C22—C21—C24—O5 | 170.3 (2) |
N2—Ni1—N4—C15 | −28.00 (18) | C20—C21—C24—O5 | −8.5 (3) |
N5—Ni1—N4—C15 | 59.83 (17) | C24—O5—C25—C26 | 84.2 (3) |
N3—Ni1—N4—C15 | −119.29 (17) | C31—N6—C27—C28 | −2.3 (3) |
N1—Ni1—N4—C11 | −28.27 (18) | Ni1—N6—C27—C28 | −179.18 (19) |
N2—Ni1—N4—C11 | 154.34 (18) | N6—C27—C28—C29 | 1.2 (4) |
N5—Ni1—N4—C11 | −117.83 (18) | C27—C28—C29—C30 | 1.5 (4) |
N3—Ni1—N4—C11 | 63.06 (18) | C27—C28—C29—C32 | −175.4 (2) |
N1—Ni1—N5—C19 | −48.15 (18) | C28—C29—C30—C31 | −3.0 (4) |
N2—Ni1—N5—C19 | 131.13 (18) | C32—C29—C30—C31 | 173.6 (2) |
N6—Ni1—N5—C19 | −138.93 (18) | C27—N6—C31—C30 | 0.6 (3) |
N4—Ni1—N5—C19 | 40.98 (18) | Ni1—N6—C31—C30 | 177.33 (17) |
N1—Ni1—N5—C23 | 138.37 (18) | C29—C30—C31—N6 | 2.0 (4) |
N2—Ni1—N5—C23 | −42.35 (18) | C33—O8—C32—O7 | −1.0 (5) |
N6—Ni1—N5—C23 | 47.59 (18) | C33—O8—C32—C29 | −177.5 (2) |
N4—Ni1—N5—C23 | −132.50 (18) | C28—C29—C32—O7 | 14.2 (4) |
N1—Ni1—N6—C31 | −25.77 (18) | C30—C29—C32—O7 | −162.4 (3) |
N2—Ni1—N6—C31 | 151.66 (18) | C28—C29—C32—O8 | −169.2 (2) |
N5—Ni1—N6—C31 | 63.83 (18) | C30—C29—C32—O8 | 14.2 (4) |
N3—Ni1—N6—C31 | −117.06 (18) | C32—O8—C33—C34 | −153.7 (3) |
N1—Ni1—N6—C27 | 150.96 (17) | C41—N9—C37—C38 | −0.5 (3) |
N2—Ni1—N6—C27 | −31.61 (17) | Ni2—N9—C37—C38 | 172.13 (17) |
N5—Ni1—N6—C27 | −119.44 (17) | N9—C37—C38—C39 | 0.9 (3) |
N3—Ni1—N6—C27 | 59.67 (17) | C37—C38—C39—C40 | −0.7 (3) |
N9—Ni2—N7—C35 | −110.6 (5) | C37—C38—C39—C42 | −179.7 (2) |
N12—Ni2—N7—C35 | 158.0 (5) | C38—C39—C40—C41 | 0.1 (3) |
N11—Ni2—N7—C35 | 66.7 (5) | C42—C39—C40—C41 | 179.1 (2) |
N10—Ni2—N7—C35 | −25.2 (5) | C37—N9—C41—C40 | −0.2 (3) |
N9—Ni2—N8—C36 | −91.9 (6) | Ni2—N9—C41—C40 | −173.07 (18) |
N12—Ni2—N8—C36 | −0.5 (6) | C39—C40—C41—N9 | 0.4 (4) |
N11—Ni2—N8—C36 | 90.7 (6) | C43A—O10A—C42—O9 | −3.1 (4) |
N10—Ni2—N8—C36 | −177.3 (6) | C43A—O10A—C42—O10B | −86.1 (8) |
N7—Ni2—N9—C37 | −27.50 (18) | C43A—O10A—C42—C39 | 173.4 (2) |
N8—Ni2—N9—C37 | 150.22 (18) | C40—C39—C42—O9 | 4.7 (4) |
N12—Ni2—N9—C37 | 62.74 (18) | C38—C39—C42—O9 | −176.3 (3) |
N10—Ni2—N9—C37 | −118.98 (18) | C40—C39—C42—O10B | 144.6 (8) |
N7—Ni2—N9—C41 | 145.04 (17) | C38—C39—C42—O10B | −36.4 (8) |
N8—Ni2—N9—C41 | −37.23 (17) | C40—C39—C42—O10A | −172.0 (2) |
N12—Ni2—N9—C41 | −124.72 (17) | C38—C39—C42—O10A | 7.0 (4) |
N10—Ni2—N9—C41 | 53.57 (17) | C42—O10A—C43A—C44A | 74.8 (3) |
N7—Ni2—N10—C49 | 160.73 (17) | C49—N10—C45—C46 | 2.7 (3) |
N8—Ni2—N10—C49 | −19.01 (17) | Ni2—N10—C45—C46 | −161.00 (17) |
N9—Ni2—N10—C49 | −109.49 (17) | N10—C45—C46—C47 | 0.3 (3) |
N11—Ni2—N10—C49 | 72.31 (17) | C45—C46—C47—C48 | −2.9 (3) |
N7—Ni2—N10—C45 | −36.15 (16) | C45—C46—C47—C50 | 174.1 (2) |
N8—Ni2—N10—C45 | 144.12 (16) | C46—C47—C48—C49 | 2.6 (3) |
N9—Ni2—N10—C45 | 53.64 (16) | C50—C47—C48—C49 | −174.3 (2) |
N11—Ni2—N10—C45 | −124.57 (16) | C45—N10—C49—C48 | −3.0 (3) |
N7—Ni2—N11—C57 | 148.53 (17) | Ni2—N10—C49—C48 | 160.20 (17) |
N8—Ni2—N11—C57 | −29.17 (18) | C47—C48—C49—N10 | 0.4 (3) |
N12—Ni2—N11—C57 | 58.33 (17) | C51—O12—C50—O11 | 2.8 (3) |
N10—Ni2—N11—C57 | −120.06 (17) | C51—O12—C50—C47 | −179.49 (18) |
N7—Ni2—N11—C53 | −28.88 (18) | C46—C47—C50—O11 | −6.7 (3) |
N8—Ni2—N11—C53 | 153.41 (17) | C48—C47—C50—O11 | 170.2 (2) |
N12—Ni2—N11—C53 | −119.09 (17) | C46—C47—C50—O12 | 175.52 (19) |
N10—Ni2—N11—C53 | 62.53 (17) | C48—C47—C50—O12 | −7.6 (3) |
N7—Ni2—N12—C61 | −46.37 (17) | C50—O12—C51—C52 | −81.7 (3) |
N8—Ni2—N12—C61 | 133.24 (17) | C57—N11—C53—C54 | −0.4 (3) |
N9—Ni2—N12—C61 | −136.27 (17) | Ni2—N11—C53—C54 | 177.11 (16) |
N11—Ni2—N12—C61 | 42.01 (17) | N11—C53—C54—C55 | 0.0 (3) |
N7—Ni2—N12—C65 | 139.92 (18) | C53—C54—C55—C56 | 0.8 (3) |
N8—Ni2—N12—C65 | −40.47 (18) | C53—C54—C55—C58 | −179.3 (2) |
N9—Ni2—N12—C65 | 50.01 (18) | C54—C55—C56—C57 | −1.2 (3) |
N11—Ni2—N12—C65 | −131.71 (18) | C58—C55—C56—C57 | 178.9 (2) |
C7—N3—C3—C4 | −3.5 (3) | C53—N11—C57—C56 | 0.0 (3) |
Ni1—N3—C3—C4 | 158.40 (17) | Ni2—N11—C57—C56 | −177.58 (18) |
N3—C3—C4—C5 | 0.1 (3) | C55—C56—C57—N11 | 0.8 (4) |
C3—C4—C5—C6 | 3.4 (3) | C59—O14—C58—O13 | 1.2 (4) |
C3—C4—C5—C8 | −174.3 (2) | C59—O14—C58—C55 | −177.71 (18) |
C4—C5—C6—C7 | −3.5 (3) | C56—C55—C58—O13 | −164.9 (2) |
C8—C5—C6—C7 | 174.3 (2) | C54—C55—C58—O13 | 15.2 (4) |
C3—N3—C7—C6 | 3.4 (3) | C56—C55—C58—O14 | 14.0 (3) |
Ni1—N3—C7—C6 | −159.08 (18) | C54—C55—C58—O14 | −165.8 (2) |
C5—C6—C7—N3 | 0.0 (3) | C58—O14—C59—C60 | 172.4 (2) |
C9—O2—C8—O1 | 4.0 (3) | C65—N12—C61—C62 | 3.2 (3) |
C9—O2—C8—C5 | −178.57 (19) | Ni2—N12—C61—C62 | −170.89 (18) |
C4—C5—C8—O1 | 167.8 (2) | N12—C61—C62—C63 | −1.6 (4) |
C6—C5—C8—O1 | −9.9 (3) | C61—C62—C63—C64 | −1.7 (3) |
C4—C5—C8—O2 | −9.7 (3) | C61—C62—C63—C66 | 177.4 (2) |
C6—C5—C8—O2 | 172.6 (2) | C62—C63—C64—C65 | 3.2 (3) |
C8—O2—C9—C10 | −82.1 (3) | C66—C63—C64—C65 | −175.9 (2) |
C15—N4—C11—C12 | −0.7 (3) | C61—N12—C65—C64 | −1.5 (3) |
Ni1—N4—C11—C12 | 177.07 (16) | Ni2—N12—C65—C64 | 172.30 (17) |
N4—C11—C12—C13 | 0.3 (3) | C63—C64—C65—N12 | −1.7 (4) |
C11—C12—C13—C14 | 0.1 (3) | C67—O16—C66—O15 | −0.4 (4) |
C11—C12—C13—C16 | −179.0 (2) | C67—O16—C66—C63 | 179.8 (2) |
C12—C13—C14—C15 | −0.2 (3) | C64—C63—C66—O15 | −7.5 (4) |
C16—C13—C14—C15 | 178.9 (2) | C62—C63—C66—O15 | 173.5 (2) |
C11—N4—C15—C14 | 0.6 (3) | C64—C63—C66—O16 | 172.3 (2) |
Ni1—N4—C15—C14 | −177.18 (18) | C62—C63—C66—O16 | −6.7 (3) |
C13—C14—C15—N4 | −0.2 (4) | C66—O16—C67—C68 | 86.0 (3) |
C17—O4—C16—O3 | −0.8 (4) | O9—C42—O10B—C43B | −26.0 (15) |
C17—O4—C16—C13 | 179.63 (18) | O10A—C42—O10B—C43B | 93.1 (15) |
C14—C13—C16—O3 | −165.6 (2) | C39—C42—O10B—C43B | −169.8 (11) |
C12—C13—C16—O3 | 13.4 (4) | C42—O10B—C43B—C44B | −92.5 (18) |
C14—C13—C16—O4 | 14.0 (3) |
C30H28N6NiO8S2 | F(000) = 3740 |
Mr = 723.41 | Dx = 1.408 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 9676 reflections |
a = 11.8991 (3) Å | θ = 2.6–26.1° |
b = 51.4066 (12) Å | µ = 0.75 mm−1 |
c = 14.1366 (3) Å | T = 100 K |
β = 99.498 (1)° | Needle, blue |
V = 8528.7 (3) Å3 | 0.57 × 0.19 × 0.15 mm |
Z = 10 |
Bruker APEX-II CCD diffractometer | 14949 independent reflections |
Radiation source: fine-focus sealed tube | 11076 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.078 |
φ and ω scans | θmax = 25.0°, θmin = 1.5° |
Absorption correction: multi-scan SADABS (Bruker, 2008) | h = −14→13 |
Tmin = 0.843, Tmax = 0.894 | k = 0→61 |
79032 measured reflections | l = 0→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)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.127 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.063P)2 + 5.5441P] where P = (Fo2 + 2Fc2)/3 |
14949 reflections | (Δ/σ)max = 0.001 |
1078 parameters | Δρmax = 1.00 e Å−3 |
0 restraints | Δρmin = −0.55 e Å−3 |
C30H28N6NiO8S2 | V = 8528.7 (3) Å3 |
Mr = 723.41 | Z = 10 |
Monoclinic, P21/n | Mo Kα radiation |
a = 11.8991 (3) Å | µ = 0.75 mm−1 |
b = 51.4066 (12) Å | T = 100 K |
c = 14.1366 (3) Å | 0.57 × 0.19 × 0.15 mm |
β = 99.498 (1)° |
Bruker APEX-II CCD diffractometer | 14949 independent reflections |
Absorption correction: multi-scan SADABS (Bruker, 2008) | 11076 reflections with I > 2σ(I) |
Tmin = 0.843, Tmax = 0.894 | Rint = 0.078 |
79032 measured reflections |
R[F2 > 2σ(F2)] = 0.050 | 0 restraints |
wR(F2) = 0.127 | H-atom parameters constrained |
S = 1.07 | Δρmax = 1.00 e Å−3 |
14949 reflections | Δρmin = −0.55 e Å−3 |
1078 parameters |
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 | Occ. (<1) | |
Ni1 | 0.07424 (4) | 0.183082 (8) | 0.35592 (3) | 0.02717 (12) | |
S1 | −0.04958 (15) | 0.20068 (2) | 0.01887 (8) | 0.0729 (5) | |
S2 | 0.21851 (9) | 0.16558 (2) | 0.68982 (7) | 0.0436 (2) | |
O1 | −0.5069 (2) | 0.17014 (6) | 0.41726 (19) | 0.0464 (7) | |
O2 | −0.4125 (2) | 0.15758 (5) | 0.55996 (17) | 0.0349 (6) | |
O3 | 0.1148 (2) | 0.05293 (5) | 0.20134 (17) | 0.0337 (6) | |
O4 | 0.3008 (2) | 0.06241 (4) | 0.24550 (17) | 0.0320 (5) | |
O5 | 0.5803 (3) | 0.23577 (6) | 0.2214 (2) | 0.0544 (8) | |
O6 | 0.5502 (3) | 0.26175 (6) | 0.3442 (2) | 0.0548 (8) | |
O7 | −0.0996 (3) | 0.30667 (5) | 0.5136 (2) | 0.0566 (8) | |
O8 | −0.0398 (2) | 0.31685 (4) | 0.37630 (17) | 0.0323 (6) | |
N1 | 0.0124 (2) | 0.18826 (5) | 0.2123 (2) | 0.0294 (6) | |
N2 | 0.1374 (3) | 0.17661 (6) | 0.4972 (2) | 0.0337 (7) | |
N3 | −0.0915 (2) | 0.17109 (5) | 0.3816 (2) | 0.0275 (6) | |
N4 | 0.1208 (2) | 0.14500 (5) | 0.3217 (2) | 0.0283 (6) | |
N5 | 0.2335 (2) | 0.19950 (5) | 0.33642 (19) | 0.0286 (6) | |
N6 | 0.0238 (3) | 0.22185 (6) | 0.3846 (2) | 0.0317 (7) | |
C1 | −0.1840 (3) | 0.18378 (7) | 0.3361 (2) | 0.0320 (8) | |
H1 | −0.1753 | 0.1951 | 0.2846 | 0.038* | |
C2 | −0.2908 (3) | 0.18112 (7) | 0.3610 (2) | 0.0330 (8) | |
H2 | −0.3541 | 0.1902 | 0.3262 | 0.040* | |
C3 | −0.3052 (3) | 0.16514 (7) | 0.4373 (2) | 0.0299 (8) | |
C4 | −0.2115 (3) | 0.15109 (7) | 0.4814 (3) | 0.0327 (8) | |
H4 | −0.2186 | 0.1392 | 0.5316 | 0.039* | |
C5 | −0.1076 (3) | 0.15459 (7) | 0.4512 (3) | 0.0332 (8) | |
H5 | −0.0443 | 0.1447 | 0.4817 | 0.040* | |
C6 | −0.4198 (3) | 0.16444 (7) | 0.4684 (3) | 0.0333 (8) | |
C7 | −0.5196 (3) | 0.15910 (8) | 0.5967 (3) | 0.0430 (10) | |
H7A | −0.5507 | 0.1767 | 0.5870 | 0.065* | |
H7B | −0.5063 | 0.1550 | 0.6653 | 0.065* | |
H7C | −0.5739 | 0.1466 | 0.5624 | 0.065* | |
C8 | 0.0405 (3) | 0.13016 (7) | 0.2697 (3) | 0.0304 (8) | |
H8 | −0.0334 | 0.1373 | 0.2508 | 0.036* | |
C9 | 0.0601 (3) | 0.10524 (7) | 0.2428 (3) | 0.0325 (8) | |
H9 | −0.0001 | 0.0951 | 0.2088 | 0.039* | |
C10 | 0.1692 (3) | 0.09493 (6) | 0.2657 (2) | 0.0252 (7) | |
C11 | 0.2536 (3) | 0.11013 (6) | 0.3189 (2) | 0.0279 (7) | |
H11 | 0.3290 | 0.1037 | 0.3364 | 0.034* | |
C12 | 0.2250 (3) | 0.13491 (7) | 0.3458 (2) | 0.0294 (8) | |
H12 | 0.2823 | 0.1452 | 0.3832 | 0.035* | |
C13 | 0.1897 (3) | 0.06798 (7) | 0.2337 (2) | 0.0284 (8) | |
C14 | 0.3280 (3) | 0.03624 (7) | 0.2199 (3) | 0.0366 (9) | |
H14A | 0.2856 | 0.0238 | 0.2531 | 0.055* | |
H14B | 0.4100 | 0.0332 | 0.2389 | 0.055* | |
H14C | 0.3070 | 0.0339 | 0.1505 | 0.055* | |
C15 | 0.2782 (3) | 0.19594 (7) | 0.2561 (2) | 0.0308 (8) | |
H15 | 0.2432 | 0.1837 | 0.2102 | 0.037* | |
C16 | 0.3722 (3) | 0.20929 (7) | 0.2373 (3) | 0.0338 (8) | |
H16 | 0.4019 | 0.2062 | 0.1799 | 0.041* | |
C17 | 0.4230 (3) | 0.22740 (7) | 0.3036 (3) | 0.0331 (8) | |
C18 | 0.3770 (3) | 0.23125 (7) | 0.3871 (3) | 0.0370 (9) | |
H18 | 0.4092 | 0.2437 | 0.4334 | 0.044* | |
C19 | 0.2844 (3) | 0.21668 (7) | 0.4010 (3) | 0.0335 (8) | |
H19 | 0.2551 | 0.2189 | 0.4591 | 0.040* | |
C20 | 0.5255 (4) | 0.24180 (8) | 0.2838 (3) | 0.0446 (10) | |
C21 | 0.6473 (5) | 0.27748 (11) | 0.3298 (4) | 0.0785 (17) | |
H21A | 0.7158 | 0.2666 | 0.3374 | 0.118* | |
H21B | 0.6581 | 0.2916 | 0.3771 | 0.118* | |
H21C | 0.6335 | 0.2849 | 0.2650 | 0.118* | |
C22 | 0.0208 (3) | 0.24028 (7) | 0.3175 (3) | 0.0339 (8) | |
H22 | 0.0375 | 0.2355 | 0.2564 | 0.041* | |
C23 | −0.0056 (3) | 0.26595 (6) | 0.3330 (3) | 0.0330 (8) | |
H23 | −0.0066 | 0.2786 | 0.2837 | 0.040* | |
C24 | −0.0304 (3) | 0.27288 (6) | 0.4217 (2) | 0.0289 (8) | |
C25 | −0.0291 (3) | 0.25395 (7) | 0.4912 (3) | 0.0376 (9) | |
H25 | −0.0467 | 0.2581 | 0.5525 | 0.045* | |
C26 | −0.0016 (3) | 0.22896 (7) | 0.4698 (3) | 0.0359 (9) | |
H26 | −0.0006 | 0.2160 | 0.5179 | 0.043* | |
C27 | −0.0604 (3) | 0.30032 (7) | 0.4440 (3) | 0.0332 (8) | |
C28 | −0.0670 (4) | 0.34374 (7) | 0.3920 (3) | 0.0405 (9) | |
H28A | −0.1462 | 0.3450 | 0.4026 | 0.061* | |
H28B | −0.0572 | 0.3541 | 0.3357 | 0.061* | |
H28C | −0.0160 | 0.3504 | 0.4485 | 0.061* | |
C29 | −0.0143 (3) | 0.19312 (6) | 0.1325 (3) | 0.0332 (8) | |
C30 | 0.1712 (3) | 0.17216 (6) | 0.5771 (3) | 0.0284 (8) | |
Ni3 | 0.5000 | 0.0000 | 0.5000 | 0.02685 (15) | |
S5 | 0.56208 (8) | 0.088941 (19) | 0.41589 (8) | 0.0447 (3) | |
O17 | −0.1098 (2) | 0.01380 (7) | 0.3633 (2) | 0.0592 (9) | |
O18 | −0.0517 (2) | 0.05542 (7) | 0.36947 (19) | 0.0519 (8) | |
O19 | 0.3896 (2) | 0.01951 (5) | 0.97649 (18) | 0.0380 (6) | |
O20 | 0.5470 (2) | 0.04375 (5) | 0.97503 (17) | 0.0325 (5) | |
N13 | 0.5437 (2) | 0.03720 (6) | 0.4714 (2) | 0.0324 (7) | |
N14 | 0.3176 (2) | 0.00979 (6) | 0.4613 (2) | 0.0299 (6) | |
N15 | 0.4836 (2) | 0.01091 (5) | 0.6422 (2) | 0.0269 (6) | |
C61 | 0.5514 (3) | 0.05891 (7) | 0.4476 (2) | 0.0272 (7) | |
C62 | 0.2833 (3) | 0.03465 (7) | 0.4620 (3) | 0.0331 (8) | |
H62 | 0.3391 | 0.0477 | 0.4803 | 0.040* | |
C63 | 0.1706 (3) | 0.04218 (7) | 0.4372 (2) | 0.0340 (8) | |
H63 | 0.1502 | 0.0600 | 0.4397 | 0.041* | |
C64 | 0.0881 (3) | 0.02360 (8) | 0.4089 (2) | 0.0353 (9) | |
C65 | 0.1224 (3) | −0.00224 (8) | 0.4100 (3) | 0.0370 (9) | |
H65 | 0.0679 | −0.0156 | 0.3923 | 0.044* | |
C66 | 0.2363 (3) | −0.00831 (7) | 0.4368 (3) | 0.0320 (8) | |
H66 | 0.2582 | −0.0261 | 0.4381 | 0.038* | |
C67 | −0.0353 (3) | 0.02995 (9) | 0.3785 (3) | 0.0418 (10) | |
C68 | −0.1689 (4) | 0.06387 (12) | 0.3430 (3) | 0.0678 (15) | |
H68A | −0.2010 | 0.0566 | 0.2803 | 0.102* | |
H68B | −0.1715 | 0.0829 | 0.3396 | 0.102* | |
H68C | −0.2134 | 0.0579 | 0.3912 | 0.102* | |
C69 | 0.5591 (3) | 0.02666 (6) | 0.6942 (3) | 0.0278 (8) | |
H69 | 0.6172 | 0.0342 | 0.6644 | 0.033* | |
C70 | 0.5569 (3) | 0.03253 (6) | 0.7887 (3) | 0.0297 (8) | |
H70 | 0.6136 | 0.0435 | 0.8233 | 0.036* | |
C71 | 0.4706 (3) | 0.02226 (6) | 0.8334 (2) | 0.0256 (7) | |
C72 | 0.3897 (3) | 0.00667 (6) | 0.7787 (3) | 0.0291 (8) | |
H72 | 0.3280 | −0.0002 | 0.8057 | 0.035* | |
C73 | 0.3992 (3) | 0.00117 (7) | 0.6849 (3) | 0.0300 (8) | |
H73 | 0.3442 | −0.0099 | 0.6489 | 0.036* | |
C74 | 0.4629 (3) | 0.02801 (7) | 0.9354 (3) | 0.0300 (8) | |
C75 | 0.5443 (3) | 0.05179 (7) | 1.0731 (3) | 0.0373 (9) | |
H75A | 0.4719 | 0.0606 | 1.0763 | 0.056* | |
H75B | 0.6076 | 0.0637 | 1.0943 | 0.056* | |
H75C | 0.5514 | 0.0365 | 1.1149 | 0.056* | |
Ni2 | 0.83220 (4) | 0.102825 (8) | 0.88691 (3) | 0.02653 (11) | |
S3 | 0.88396 (10) | 0.07454 (2) | 0.57837 (7) | 0.0546 (3) | |
S4A | 0.74497 (12) | 0.12009 (4) | 1.19792 (10) | 0.0502 (5) | 0.734 (3) |
C32A | 0.7625 (8) | 0.11924 (11) | 1.0853 (7) | 0.0261 (15) | 0.734 (3) |
S4B | 0.7454 (3) | 0.13802 (12) | 1.1747 (3) | 0.0502 (5) | 0.266 (3) |
C32B | 0.766 (3) | 0.1271 (4) | 1.072 (2) | 0.0261 (15) | 0.266 (3) |
O9 | 0.8690 (2) | −0.03206 (4) | 1.02383 (17) | 0.0308 (5) | |
O10 | 0.87344 (19) | −0.01167 (4) | 1.16524 (16) | 0.0268 (5) | |
O11 | 0.2293 (3) | 0.09127 (6) | 0.7465 (2) | 0.0515 (7) | |
O12 | 0.2813 (2) | 0.09939 (5) | 0.6037 (2) | 0.0513 (8) | |
O13 | 0.8606 (3) | 0.22274 (5) | 0.6403 (2) | 0.0496 (7) | |
O14 | 0.6767 (2) | 0.22036 (5) | 0.65706 (18) | 0.0382 (6) | |
O15 | 1.4237 (2) | 0.10934 (5) | 1.06090 (19) | 0.0377 (6) | |
O16 | 1.35840 (19) | 0.14066 (5) | 1.14857 (18) | 0.0344 (6) | |
N7 | 0.8892 (3) | 0.08816 (6) | 0.7697 (2) | 0.0337 (7) | |
N8 | 0.7761 (3) | 0.11747 (5) | 1.0049 (2) | 0.0301 (7) | |
N9 | 0.8411 (2) | 0.06382 (5) | 0.94667 (19) | 0.0258 (6) | |
N10 | 0.6575 (2) | 0.09733 (5) | 0.8184 (2) | 0.0299 (7) | |
N11 | 0.8258 (2) | 0.14070 (5) | 0.82614 (19) | 0.0267 (6) | |
N12 | 1.0004 (2) | 0.10956 (5) | 0.9546 (2) | 0.0276 (6) | |
C31 | 0.8892 (3) | 0.08247 (7) | 0.6900 (3) | 0.0321 (8) | |
C33 | 0.8371 (3) | 0.04218 (6) | 0.8919 (2) | 0.0259 (7) | |
H33 | 0.8278 | 0.0442 | 0.8242 | 0.031* | |
C34 | 0.8458 (3) | 0.01742 (6) | 0.9295 (2) | 0.0245 (7) | |
H34 | 0.8420 | 0.0027 | 0.8886 | 0.029* | |
C35 | 0.8601 (3) | 0.01436 (6) | 1.0286 (2) | 0.0240 (7) | |
C36 | 0.8677 (3) | 0.03624 (6) | 1.0853 (2) | 0.0276 (7) | |
H36 | 0.8794 | 0.0347 | 1.1532 | 0.033* | |
C37 | 0.8580 (3) | 0.06040 (6) | 1.0421 (2) | 0.0287 (8) | |
H37 | 0.8637 | 0.0754 | 1.0819 | 0.034* | |
C38 | 0.8680 (3) | −0.01243 (6) | 1.0705 (2) | 0.0225 (7) | |
C39 | 0.8752 (3) | −0.03658 (7) | 1.2133 (3) | 0.0335 (8) | |
H39A | 0.8107 | −0.0471 | 1.1828 | 0.050* | |
H39B | 0.8694 | −0.0339 | 1.2810 | 0.050* | |
H39C | 0.9466 | −0.0456 | 1.2087 | 0.050* | |
C40 | 0.5743 (3) | 0.09550 (6) | 0.8716 (3) | 0.0293 (8) | |
H40 | 0.5952 | 0.0951 | 0.9394 | 0.035* | |
C41 | 0.4600 (3) | 0.09411 (6) | 0.8332 (3) | 0.0343 (8) | |
H41 | 0.4041 | 0.0927 | 0.8738 | 0.041* | |
C42 | 0.4284 (3) | 0.09480 (6) | 0.7358 (3) | 0.0365 (9) | |
C43 | 0.5116 (4) | 0.09653 (7) | 0.6789 (3) | 0.0403 (9) | |
H43 | 0.4916 | 0.0970 | 0.6110 | 0.048* | |
C44 | 0.6257 (3) | 0.09766 (7) | 0.7224 (3) | 0.0369 (9) | |
H44 | 0.6829 | 0.0987 | 0.6829 | 0.044* | |
C45 | 0.2981 (4) | 0.09484 (7) | 0.6986 (3) | 0.0462 (11) | |
C46 | 0.1570 (4) | 0.10232 (10) | 0.5686 (4) | 0.0576 (12) | |
H46A | 0.1177 | 0.0862 | 0.5806 | 0.086* | |
H46B | 0.1443 | 0.1059 | 0.4996 | 0.086* | |
H46C | 0.1272 | 0.1168 | 0.6024 | 0.086* | |
C47 | 0.7393 (3) | 0.15650 (7) | 0.8338 (2) | 0.0296 (8) | |
H47 | 0.6868 | 0.1514 | 0.8742 | 0.035* | |
C48 | 0.7218 (3) | 0.17988 (6) | 0.7862 (2) | 0.0275 (7) | |
H48 | 0.6577 | 0.1904 | 0.7922 | 0.033* | |
C49 | 0.7997 (3) | 0.18772 (6) | 0.7296 (2) | 0.0276 (7) | |
C50 | 0.8935 (3) | 0.17225 (7) | 0.7250 (2) | 0.0302 (8) | |
H50 | 0.9505 | 0.1777 | 0.6895 | 0.036* | |
C51 | 0.9028 (3) | 0.14879 (6) | 0.7726 (2) | 0.0285 (7) | |
H51 | 0.9660 | 0.1379 | 0.7676 | 0.034* | |
C52 | 0.7840 (3) | 0.21217 (7) | 0.6711 (2) | 0.0323 (8) | |
C53 | 0.6512 (4) | 0.24271 (8) | 0.5948 (3) | 0.0478 (11) | |
H53A | 0.6936 | 0.2578 | 0.6239 | 0.072* | |
H53B | 0.5693 | 0.2464 | 0.5861 | 0.072* | |
H53C | 0.6734 | 0.2390 | 0.5324 | 0.072* | |
C54 | 1.0313 (3) | 0.13227 (6) | 0.9971 (2) | 0.0301 (8) | |
H54 | 0.9752 | 0.1454 | 0.9979 | 0.036* | |
C55 | 1.1421 (3) | 0.13739 (7) | 1.0400 (2) | 0.0290 (8) | |
H55 | 1.1615 | 0.1537 | 1.0699 | 0.035* | |
C56 | 1.2250 (3) | 0.11826 (6) | 1.0387 (2) | 0.0261 (7) | |
C57 | 1.1926 (3) | 0.09485 (6) | 0.9948 (2) | 0.0285 (8) | |
H57 | 1.2470 | 0.0814 | 0.9929 | 0.034* | |
C58 | 1.0808 (3) | 0.09125 (7) | 0.9538 (2) | 0.0298 (8) | |
H58 | 1.0593 | 0.0751 | 0.9234 | 0.036* | |
C59 | 1.3468 (3) | 0.12197 (7) | 1.0827 (2) | 0.0291 (8) | |
C60 | 1.4748 (3) | 0.14461 (8) | 1.1971 (3) | 0.0433 (10) | |
H60A | 1.5074 | 0.1279 | 1.2213 | 0.065* | |
H60B | 1.4750 | 0.1567 | 1.2508 | 0.065* | |
H60C | 1.5205 | 0.1519 | 1.1519 | 0.065* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0325 (2) | 0.0233 (2) | 0.0250 (2) | 0.00241 (18) | 0.00283 (18) | 0.00074 (18) |
S1 | 0.1528 (14) | 0.0279 (6) | 0.0274 (6) | 0.0137 (7) | −0.0162 (7) | −0.0023 (4) |
S2 | 0.0472 (6) | 0.0572 (6) | 0.0252 (5) | 0.0133 (5) | 0.0021 (4) | 0.0005 (4) |
O1 | 0.0329 (15) | 0.0651 (19) | 0.0397 (16) | 0.0123 (13) | 0.0017 (13) | 0.0091 (14) |
O2 | 0.0318 (13) | 0.0394 (14) | 0.0338 (14) | 0.0008 (11) | 0.0059 (11) | 0.0045 (11) |
O3 | 0.0358 (14) | 0.0321 (14) | 0.0326 (14) | −0.0041 (11) | 0.0041 (11) | −0.0084 (11) |
O4 | 0.0291 (13) | 0.0282 (13) | 0.0395 (14) | 0.0030 (10) | 0.0078 (11) | −0.0042 (11) |
O5 | 0.0496 (18) | 0.059 (2) | 0.0544 (19) | −0.0086 (15) | 0.0085 (16) | 0.0111 (15) |
O6 | 0.0557 (18) | 0.0479 (18) | 0.0584 (19) | −0.0253 (15) | 0.0024 (15) | 0.0003 (15) |
O7 | 0.098 (2) | 0.0315 (15) | 0.0512 (18) | 0.0104 (15) | 0.0443 (18) | 0.0032 (13) |
O8 | 0.0478 (15) | 0.0205 (12) | 0.0297 (13) | 0.0012 (11) | 0.0095 (11) | 0.0030 (10) |
N1 | 0.0334 (16) | 0.0275 (16) | 0.0278 (17) | 0.0069 (12) | 0.0060 (13) | −0.0017 (12) |
N2 | 0.0413 (18) | 0.0279 (16) | 0.0306 (18) | 0.0011 (13) | 0.0026 (14) | 0.0000 (13) |
N3 | 0.0326 (16) | 0.0227 (15) | 0.0263 (15) | 0.0024 (12) | 0.0021 (12) | 0.0010 (12) |
N4 | 0.0292 (15) | 0.0244 (15) | 0.0306 (16) | −0.0003 (12) | 0.0029 (12) | 0.0032 (12) |
N5 | 0.0344 (16) | 0.0259 (15) | 0.0237 (15) | −0.0014 (12) | −0.0002 (12) | −0.0012 (12) |
N6 | 0.0394 (17) | 0.0279 (16) | 0.0285 (16) | −0.0003 (13) | 0.0074 (13) | 0.0023 (13) |
C1 | 0.041 (2) | 0.0297 (19) | 0.0262 (18) | 0.0081 (16) | 0.0071 (16) | 0.0048 (15) |
C2 | 0.036 (2) | 0.034 (2) | 0.0277 (19) | 0.0083 (16) | 0.0012 (16) | 0.0030 (15) |
C3 | 0.0332 (19) | 0.0288 (18) | 0.0270 (18) | 0.0008 (15) | 0.0031 (15) | −0.0046 (15) |
C4 | 0.040 (2) | 0.0278 (19) | 0.0293 (19) | −0.0018 (16) | 0.0027 (16) | 0.0023 (15) |
C5 | 0.033 (2) | 0.0302 (19) | 0.034 (2) | 0.0037 (16) | −0.0001 (16) | 0.0063 (16) |
C6 | 0.035 (2) | 0.033 (2) | 0.031 (2) | 0.0020 (16) | 0.0006 (17) | 0.0007 (16) |
C7 | 0.041 (2) | 0.046 (2) | 0.046 (2) | 0.0035 (18) | 0.0170 (19) | 0.0080 (19) |
C8 | 0.0254 (18) | 0.0296 (19) | 0.0344 (19) | 0.0023 (15) | −0.0006 (15) | −0.0021 (15) |
C9 | 0.0304 (19) | 0.031 (2) | 0.035 (2) | −0.0023 (15) | 0.0005 (16) | −0.0041 (16) |
C10 | 0.0265 (18) | 0.0230 (17) | 0.0266 (17) | −0.0040 (14) | 0.0055 (14) | 0.0001 (14) |
C11 | 0.0260 (18) | 0.0268 (18) | 0.0299 (18) | 0.0022 (14) | 0.0013 (15) | 0.0035 (14) |
C12 | 0.0284 (18) | 0.0257 (18) | 0.0316 (19) | −0.0017 (15) | −0.0024 (15) | −0.0004 (15) |
C13 | 0.0317 (19) | 0.0321 (19) | 0.0220 (17) | 0.0002 (16) | 0.0068 (15) | 0.0002 (15) |
C14 | 0.044 (2) | 0.0276 (19) | 0.039 (2) | 0.0072 (16) | 0.0103 (18) | −0.0038 (16) |
C15 | 0.039 (2) | 0.0254 (18) | 0.0268 (18) | 0.0016 (15) | 0.0007 (16) | −0.0026 (14) |
C16 | 0.037 (2) | 0.035 (2) | 0.0290 (19) | −0.0007 (16) | 0.0030 (16) | 0.0043 (16) |
C17 | 0.036 (2) | 0.0273 (19) | 0.033 (2) | −0.0026 (15) | −0.0027 (16) | 0.0093 (15) |
C18 | 0.046 (2) | 0.029 (2) | 0.032 (2) | −0.0047 (17) | −0.0066 (17) | 0.0016 (16) |
C19 | 0.040 (2) | 0.033 (2) | 0.0271 (19) | −0.0013 (17) | 0.0020 (16) | 0.0022 (15) |
C20 | 0.045 (2) | 0.038 (2) | 0.046 (2) | −0.0089 (19) | −0.009 (2) | 0.0142 (19) |
C21 | 0.063 (3) | 0.071 (4) | 0.098 (4) | −0.040 (3) | 0.001 (3) | 0.000 (3) |
C22 | 0.053 (2) | 0.0250 (19) | 0.0252 (18) | −0.0017 (16) | 0.0124 (17) | −0.0025 (15) |
C23 | 0.049 (2) | 0.0227 (18) | 0.0293 (19) | −0.0057 (16) | 0.0126 (17) | 0.0056 (15) |
C24 | 0.0353 (19) | 0.0227 (17) | 0.0310 (19) | −0.0020 (15) | 0.0122 (15) | 0.0012 (14) |
C25 | 0.055 (2) | 0.030 (2) | 0.033 (2) | 0.0023 (17) | 0.0206 (18) | 0.0019 (16) |
C26 | 0.056 (2) | 0.029 (2) | 0.0257 (19) | 0.0060 (17) | 0.0160 (17) | 0.0057 (15) |
C27 | 0.039 (2) | 0.0286 (19) | 0.034 (2) | −0.0009 (16) | 0.0124 (17) | −0.0013 (16) |
C28 | 0.061 (3) | 0.0169 (17) | 0.044 (2) | 0.0023 (17) | 0.0095 (19) | −0.0012 (16) |
C29 | 0.046 (2) | 0.0169 (17) | 0.035 (2) | 0.0038 (15) | 0.0017 (17) | −0.0055 (15) |
C30 | 0.0293 (18) | 0.0238 (18) | 0.032 (2) | 0.0039 (14) | 0.0061 (16) | −0.0027 (15) |
Ni3 | 0.0243 (3) | 0.0234 (3) | 0.0338 (3) | −0.0017 (2) | 0.0079 (3) | 0.0007 (3) |
S5 | 0.0327 (5) | 0.0304 (5) | 0.0689 (7) | −0.0021 (4) | 0.0026 (5) | 0.0157 (5) |
O17 | 0.0288 (15) | 0.094 (3) | 0.0524 (19) | 0.0042 (16) | 0.0006 (13) | −0.0318 (17) |
O18 | 0.0314 (15) | 0.085 (2) | 0.0402 (16) | 0.0223 (15) | 0.0093 (12) | 0.0043 (15) |
O19 | 0.0303 (13) | 0.0464 (16) | 0.0402 (15) | −0.0034 (12) | 0.0137 (12) | 0.0003 (12) |
O20 | 0.0368 (14) | 0.0289 (13) | 0.0321 (13) | −0.0019 (11) | 0.0067 (11) | 0.0020 (10) |
N13 | 0.0276 (15) | 0.0321 (18) | 0.0388 (17) | −0.0006 (13) | 0.0094 (13) | 0.0010 (14) |
N14 | 0.0298 (16) | 0.0306 (16) | 0.0302 (16) | −0.0002 (13) | 0.0079 (13) | 0.0006 (13) |
N15 | 0.0228 (14) | 0.0223 (14) | 0.0362 (16) | 0.0021 (12) | 0.0072 (12) | 0.0026 (12) |
C61 | 0.0202 (17) | 0.030 (2) | 0.0316 (19) | −0.0006 (14) | 0.0048 (14) | 0.0005 (15) |
C62 | 0.034 (2) | 0.032 (2) | 0.035 (2) | 0.0002 (16) | 0.0111 (16) | 0.0006 (16) |
C63 | 0.034 (2) | 0.040 (2) | 0.0296 (19) | 0.0102 (17) | 0.0104 (16) | 0.0032 (16) |
C64 | 0.0258 (18) | 0.059 (3) | 0.0216 (18) | 0.0027 (18) | 0.0053 (15) | −0.0056 (17) |
C65 | 0.031 (2) | 0.051 (2) | 0.030 (2) | −0.0062 (17) | 0.0076 (16) | −0.0112 (17) |
C66 | 0.0258 (18) | 0.037 (2) | 0.035 (2) | −0.0021 (16) | 0.0106 (15) | −0.0039 (16) |
C67 | 0.034 (2) | 0.067 (3) | 0.025 (2) | 0.015 (2) | 0.0059 (17) | −0.0121 (19) |
C68 | 0.040 (2) | 0.118 (4) | 0.045 (3) | 0.038 (3) | 0.006 (2) | −0.010 (3) |
C69 | 0.0247 (17) | 0.0214 (17) | 0.040 (2) | 0.0004 (14) | 0.0130 (15) | 0.0009 (15) |
C70 | 0.0283 (18) | 0.0204 (17) | 0.041 (2) | 0.0003 (14) | 0.0090 (16) | −0.0021 (15) |
C71 | 0.0243 (17) | 0.0195 (16) | 0.0342 (19) | 0.0059 (14) | 0.0085 (15) | 0.0020 (14) |
C72 | 0.0207 (17) | 0.0278 (18) | 0.042 (2) | 0.0011 (14) | 0.0133 (15) | 0.0079 (15) |
C73 | 0.0250 (18) | 0.0243 (18) | 0.041 (2) | −0.0011 (14) | 0.0054 (15) | 0.0005 (15) |
C74 | 0.0233 (17) | 0.0249 (18) | 0.042 (2) | 0.0033 (15) | 0.0049 (16) | 0.0050 (16) |
C75 | 0.042 (2) | 0.038 (2) | 0.032 (2) | 0.0024 (17) | 0.0079 (17) | 0.0028 (16) |
Ni2 | 0.0329 (2) | 0.0199 (2) | 0.0258 (2) | 0.00069 (18) | 0.00218 (18) | 0.00226 (17) |
S3 | 0.0630 (7) | 0.0701 (8) | 0.0310 (5) | −0.0255 (6) | 0.0088 (5) | −0.0137 (5) |
S4A | 0.0311 (6) | 0.0880 (14) | 0.0316 (7) | 0.0105 (9) | 0.0054 (5) | −0.0092 (8) |
C32A | 0.0223 (19) | 0.015 (4) | 0.038 (4) | 0.004 (4) | −0.004 (2) | 0.001 (3) |
S4B | 0.0311 (6) | 0.0880 (14) | 0.0316 (7) | 0.0105 (9) | 0.0054 (5) | −0.0092 (8) |
C32B | 0.0223 (19) | 0.015 (4) | 0.038 (4) | 0.004 (4) | −0.004 (2) | 0.001 (3) |
O9 | 0.0386 (14) | 0.0212 (12) | 0.0335 (13) | 0.0028 (10) | 0.0087 (11) | −0.0013 (10) |
O10 | 0.0343 (13) | 0.0203 (12) | 0.0260 (12) | 0.0018 (10) | 0.0053 (10) | 0.0045 (9) |
O11 | 0.0424 (17) | 0.0487 (18) | 0.063 (2) | −0.0035 (14) | 0.0072 (15) | 0.0059 (15) |
O12 | 0.0441 (17) | 0.0449 (17) | 0.0591 (19) | −0.0111 (13) | −0.0086 (14) | 0.0111 (14) |
O13 | 0.0609 (19) | 0.0380 (16) | 0.0554 (18) | 0.0027 (14) | 0.0259 (15) | 0.0181 (13) |
O14 | 0.0412 (15) | 0.0315 (14) | 0.0395 (15) | 0.0036 (12) | −0.0003 (12) | 0.0097 (11) |
O15 | 0.0317 (14) | 0.0304 (14) | 0.0524 (16) | 0.0056 (11) | 0.0114 (12) | −0.0025 (12) |
O16 | 0.0276 (13) | 0.0318 (14) | 0.0421 (15) | 0.0030 (10) | 0.0009 (11) | −0.0058 (11) |
N7 | 0.0423 (18) | 0.0252 (16) | 0.0323 (18) | 0.0009 (13) | 0.0022 (14) | 0.0036 (13) |
N8 | 0.0399 (17) | 0.0183 (15) | 0.0315 (17) | −0.0019 (12) | 0.0041 (14) | 0.0012 (12) |
N9 | 0.0282 (15) | 0.0231 (14) | 0.0249 (15) | −0.0030 (12) | 0.0004 (12) | −0.0004 (12) |
N10 | 0.0382 (17) | 0.0196 (14) | 0.0307 (16) | −0.0007 (12) | 0.0021 (13) | 0.0052 (12) |
N11 | 0.0294 (15) | 0.0244 (15) | 0.0255 (15) | 0.0023 (12) | 0.0022 (12) | 0.0042 (12) |
N12 | 0.0335 (16) | 0.0185 (14) | 0.0307 (15) | 0.0007 (12) | 0.0048 (13) | 0.0009 (12) |
C31 | 0.038 (2) | 0.0236 (18) | 0.033 (2) | −0.0029 (15) | 0.0036 (16) | 0.0046 (15) |
C33 | 0.0266 (17) | 0.0275 (18) | 0.0225 (17) | −0.0011 (14) | 0.0007 (14) | −0.0014 (14) |
C34 | 0.0240 (17) | 0.0225 (17) | 0.0270 (18) | −0.0045 (13) | 0.0039 (14) | −0.0048 (14) |
C35 | 0.0188 (16) | 0.0227 (17) | 0.0305 (18) | −0.0022 (13) | 0.0038 (14) | 0.0001 (14) |
C36 | 0.0333 (19) | 0.0273 (18) | 0.0213 (17) | 0.0025 (14) | 0.0017 (14) | −0.0008 (14) |
C37 | 0.039 (2) | 0.0195 (17) | 0.0255 (18) | 0.0022 (15) | −0.0003 (15) | −0.0036 (14) |
C38 | 0.0170 (16) | 0.0214 (17) | 0.0295 (18) | 0.0002 (13) | 0.0048 (13) | 0.0013 (14) |
C39 | 0.042 (2) | 0.0247 (18) | 0.036 (2) | 0.0033 (16) | 0.0120 (17) | 0.0096 (15) |
C40 | 0.038 (2) | 0.0172 (17) | 0.0319 (19) | −0.0026 (14) | 0.0035 (16) | 0.0003 (14) |
C41 | 0.039 (2) | 0.0164 (17) | 0.047 (2) | −0.0007 (15) | 0.0052 (18) | −0.0036 (15) |
C42 | 0.040 (2) | 0.0147 (17) | 0.052 (2) | −0.0012 (15) | −0.0005 (19) | 0.0036 (16) |
C43 | 0.055 (3) | 0.0264 (19) | 0.034 (2) | 0.0021 (17) | −0.0098 (19) | 0.0038 (16) |
C44 | 0.050 (2) | 0.0236 (19) | 0.036 (2) | 0.0017 (16) | 0.0019 (18) | 0.0047 (15) |
C45 | 0.069 (3) | 0.0144 (18) | 0.046 (3) | 0.0005 (18) | −0.018 (2) | 0.0041 (17) |
C46 | 0.045 (3) | 0.063 (3) | 0.061 (3) | 0.003 (2) | −0.001 (2) | 0.008 (2) |
C47 | 0.0297 (19) | 0.0259 (18) | 0.0340 (19) | 0.0000 (15) | 0.0081 (15) | 0.0034 (15) |
C48 | 0.0303 (18) | 0.0208 (17) | 0.0307 (18) | 0.0003 (14) | 0.0030 (15) | 0.0032 (14) |
C49 | 0.0347 (19) | 0.0212 (17) | 0.0256 (18) | −0.0033 (14) | 0.0015 (15) | −0.0017 (14) |
C50 | 0.0316 (19) | 0.0286 (19) | 0.0306 (19) | −0.0028 (15) | 0.0060 (15) | 0.0016 (15) |
C51 | 0.0287 (18) | 0.0263 (18) | 0.0306 (18) | 0.0036 (14) | 0.0050 (15) | 0.0021 (15) |
C52 | 0.044 (2) | 0.0251 (19) | 0.0279 (19) | 0.0001 (16) | 0.0068 (17) | 0.0020 (15) |
C53 | 0.068 (3) | 0.034 (2) | 0.037 (2) | 0.010 (2) | −0.001 (2) | 0.0114 (18) |
C54 | 0.036 (2) | 0.0192 (17) | 0.036 (2) | 0.0020 (15) | 0.0096 (16) | 0.0002 (15) |
C55 | 0.0300 (19) | 0.0230 (17) | 0.0332 (19) | 0.0031 (14) | 0.0031 (15) | −0.0027 (14) |
C56 | 0.0301 (18) | 0.0228 (17) | 0.0263 (17) | −0.0008 (14) | 0.0071 (14) | 0.0054 (14) |
C57 | 0.0329 (19) | 0.0215 (17) | 0.0327 (19) | 0.0051 (14) | 0.0102 (15) | 0.0016 (14) |
C58 | 0.034 (2) | 0.0214 (17) | 0.0348 (19) | 0.0026 (15) | 0.0075 (16) | 0.0000 (14) |
C59 | 0.0292 (18) | 0.0258 (18) | 0.0338 (19) | 0.0006 (15) | 0.0095 (15) | 0.0054 (15) |
C60 | 0.031 (2) | 0.046 (2) | 0.049 (2) | 0.0022 (18) | −0.0039 (18) | −0.0082 (19) |
Ni1—N2 | 2.042 (3) | C64—C65 | 1.389 (6) |
Ni1—N1 | 2.060 (3) | C64—C67 | 1.496 (5) |
Ni1—N4 | 2.112 (3) | C65—C66 | 1.381 (5) |
Ni1—N5 | 2.133 (3) | C65—H65 | 0.9500 |
Ni1—N6 | 2.139 (3) | C66—H66 | 0.9500 |
Ni1—N3 | 2.154 (3) | C68—H68A | 0.9800 |
S1—C29 | 1.639 (4) | C68—H68B | 0.9800 |
S2—C30 | 1.635 (4) | C68—H68C | 0.9800 |
O1—C6 | 1.198 (4) | C69—C70 | 1.374 (5) |
O2—C6 | 1.330 (4) | C69—H69 | 0.9500 |
O2—C7 | 1.455 (4) | C70—C71 | 1.395 (5) |
O3—C13 | 1.211 (4) | C70—H70 | 0.9500 |
O4—C13 | 1.336 (4) | C71—C72 | 1.386 (5) |
O4—C14 | 1.443 (4) | C71—C74 | 1.489 (5) |
O5—C20 | 1.220 (5) | C72—C73 | 1.378 (5) |
O6—C20 | 1.336 (5) | C72—H72 | 0.9500 |
O6—C21 | 1.451 (5) | C73—H73 | 0.9500 |
O7—C27 | 1.202 (4) | C75—H75A | 0.9800 |
O8—C27 | 1.332 (4) | C75—H75B | 0.9800 |
O8—C28 | 1.445 (4) | C75—H75C | 0.9800 |
N1—C29 | 1.147 (4) | Ni2—N7 | 2.036 (3) |
N2—C30 | 1.158 (4) | Ni2—N8 | 2.040 (3) |
N3—C5 | 1.337 (4) | Ni2—N12 | 2.100 (3) |
N3—C1 | 1.348 (4) | Ni2—N11 | 2.124 (3) |
N4—C12 | 1.335 (4) | Ni2—N10 | 2.162 (3) |
N4—C8 | 1.343 (4) | Ni2—N9 | 2.172 (3) |
N5—C19 | 1.341 (4) | S3—C31 | 1.622 (4) |
N5—C15 | 1.344 (4) | S4A—C32A | 1.641 (10) |
N6—C22 | 1.337 (4) | C32A—N8 | 1.177 (10) |
N6—C26 | 1.340 (4) | S4B—C32B | 1.61 (4) |
C1—C2 | 1.380 (5) | C32B—N8 | 1.10 (3) |
C1—H1 | 0.9500 | O9—C38 | 1.207 (4) |
C2—C3 | 1.388 (5) | O10—C38 | 1.331 (4) |
C2—H2 | 0.9500 | O10—C39 | 1.448 (4) |
C3—C4 | 1.387 (5) | O11—C45 | 1.160 (5) |
C3—C6 | 1.501 (5) | O12—C45 | 1.343 (5) |
C4—C5 | 1.385 (5) | O12—C46 | 1.487 (5) |
C4—H4 | 0.9500 | O13—C52 | 1.204 (4) |
C5—H5 | 0.9500 | O14—C52 | 1.328 (4) |
C7—H7A | 0.9800 | O14—C53 | 1.448 (4) |
C7—H7B | 0.9800 | O15—C59 | 1.203 (4) |
C7—H7C | 0.9800 | O16—C59 | 1.329 (4) |
C8—C9 | 1.367 (5) | O16—C60 | 1.455 (4) |
C8—H8 | 0.9500 | N7—C31 | 1.163 (5) |
C9—C10 | 1.391 (5) | N9—C37 | 1.342 (4) |
C9—H9 | 0.9500 | N9—C33 | 1.352 (4) |
C10—C11 | 1.391 (5) | N10—C40 | 1.342 (5) |
C10—C13 | 1.489 (5) | N10—C44 | 1.347 (5) |
C11—C12 | 1.388 (5) | N11—C47 | 1.330 (4) |
C11—H11 | 0.9500 | N11—C51 | 1.347 (4) |
C12—H12 | 0.9500 | N12—C54 | 1.336 (4) |
C14—H14A | 0.9800 | N12—C58 | 1.344 (4) |
C14—H14B | 0.9800 | C33—C34 | 1.377 (5) |
C14—H14C | 0.9800 | C33—H33 | 0.9500 |
C15—C16 | 1.376 (5) | C34—C35 | 1.392 (5) |
C15—H15 | 0.9500 | C34—H34 | 0.9500 |
C16—C17 | 1.387 (5) | C35—C36 | 1.375 (5) |
C16—H16 | 0.9500 | C35—C38 | 1.496 (4) |
C17—C18 | 1.394 (5) | C36—C37 | 1.381 (5) |
C17—C20 | 1.492 (5) | C36—H36 | 0.9500 |
C18—C19 | 1.373 (5) | C37—H37 | 0.9500 |
C18—H18 | 0.9500 | C39—H39A | 0.9800 |
C19—H19 | 0.9500 | C39—H39B | 0.9800 |
C21—H21A | 0.9800 | C39—H39C | 0.9800 |
C21—H21B | 0.9800 | C40—C41 | 1.382 (5) |
C21—H21C | 0.9800 | C40—H40 | 0.9500 |
C22—C23 | 1.382 (5) | C41—C42 | 1.366 (5) |
C22—H22 | 0.9500 | C41—H41 | 0.9500 |
C23—C24 | 1.382 (5) | C42—C43 | 1.378 (6) |
C23—H23 | 0.9500 | C42—C45 | 1.554 (6) |
C24—C25 | 1.381 (5) | C43—C44 | 1.397 (6) |
C24—C27 | 1.501 (5) | C43—H43 | 0.9500 |
C25—C26 | 1.371 (5) | C44—H44 | 0.9500 |
C25—H25 | 0.9500 | C46—H46A | 0.9800 |
C26—H26 | 0.9500 | C46—H46B | 0.9800 |
C28—H28A | 0.9800 | C46—H46C | 0.9800 |
C28—H28B | 0.9800 | C47—C48 | 1.376 (5) |
C28—H28C | 0.9800 | C47—H47 | 0.9500 |
Ni3—N13i | 2.039 (3) | C48—C49 | 1.381 (5) |
Ni3—N13 | 2.039 (3) | C48—H48 | 0.9500 |
Ni3—N15 | 2.127 (3) | C49—C50 | 1.380 (5) |
Ni3—N15i | 2.127 (3) | C49—C52 | 1.499 (5) |
Ni3—N14 | 2.207 (3) | C50—C51 | 1.377 (5) |
Ni3—N14i | 2.207 (3) | C50—H50 | 0.9500 |
S5—C61 | 1.618 (4) | C51—H51 | 0.9500 |
O17—C67 | 1.208 (5) | C53—H53A | 0.9800 |
O18—C67 | 1.327 (5) | C53—H53B | 0.9800 |
O18—C68 | 1.449 (5) | C53—H53C | 0.9800 |
O19—C74 | 1.206 (4) | C54—C55 | 1.382 (5) |
O20—C74 | 1.337 (4) | C54—H54 | 0.9500 |
O20—C75 | 1.452 (4) | C55—C56 | 1.395 (5) |
N13—C61 | 1.174 (4) | C55—H55 | 0.9500 |
N14—C62 | 1.342 (4) | C56—C57 | 1.380 (5) |
N14—C66 | 1.346 (5) | C56—C59 | 1.493 (5) |
N15—C69 | 1.336 (4) | C57—C58 | 1.373 (5) |
N15—C73 | 1.350 (4) | C57—H57 | 0.9500 |
C62—C63 | 1.384 (5) | C58—H58 | 0.9500 |
C62—H62 | 0.9500 | C60—H60A | 0.9800 |
C63—C64 | 1.381 (5) | C60—H60B | 0.9800 |
C63—H63 | 0.9500 | C60—H60C | 0.9800 |
N2—Ni1—N1 | 177.90 (11) | N14—C66—H66 | 118.4 |
N2—Ni1—N4 | 90.28 (11) | C65—C66—H66 | 118.4 |
N1—Ni1—N4 | 87.62 (11) | O17—C67—O18 | 124.7 (4) |
N2—Ni1—N5 | 89.97 (11) | O17—C67—C64 | 123.9 (4) |
N1—Ni1—N5 | 90.11 (11) | O18—C67—C64 | 111.4 (4) |
N4—Ni1—N5 | 93.72 (11) | O18—C68—H68A | 109.5 |
N2—Ni1—N6 | 92.05 (11) | O18—C68—H68B | 109.5 |
N1—Ni1—N6 | 90.04 (11) | H68A—C68—H68B | 109.5 |
N4—Ni1—N6 | 177.65 (11) | O18—C68—H68C | 109.5 |
N5—Ni1—N6 | 86.49 (11) | H68A—C68—H68C | 109.5 |
N2—Ni1—N3 | 89.31 (11) | H68B—C68—H68C | 109.5 |
N1—Ni1—N3 | 90.87 (11) | N15—C69—C70 | 123.3 (3) |
N4—Ni1—N3 | 93.19 (10) | N15—C69—H69 | 118.3 |
N5—Ni1—N3 | 173.06 (10) | C70—C69—H69 | 118.3 |
N6—Ni1—N3 | 86.63 (11) | C69—C70—C71 | 119.4 (3) |
C6—O2—C7 | 114.3 (3) | C69—C70—H70 | 120.3 |
C13—O4—C14 | 115.3 (3) | C71—C70—H70 | 120.3 |
C20—O6—C21 | 115.8 (4) | C72—C71—C70 | 117.5 (3) |
C27—O8—C28 | 115.3 (3) | C72—C71—C74 | 120.5 (3) |
C29—N1—Ni1 | 173.2 (3) | C70—C71—C74 | 122.0 (3) |
C30—N2—Ni1 | 177.7 (3) | C73—C72—C71 | 119.7 (3) |
C5—N3—C1 | 117.0 (3) | C73—C72—H72 | 120.1 |
C5—N3—Ni1 | 123.5 (2) | C71—C72—H72 | 120.1 |
C1—N3—Ni1 | 118.6 (2) | N15—C73—C72 | 122.6 (3) |
C12—N4—C8 | 117.8 (3) | N15—C73—H73 | 118.7 |
C12—N4—Ni1 | 124.7 (2) | C72—C73—H73 | 118.7 |
C8—N4—Ni1 | 117.5 (2) | O19—C74—O20 | 124.6 (3) |
C19—N5—C15 | 117.9 (3) | O19—C74—C71 | 124.0 (3) |
C19—N5—Ni1 | 118.9 (2) | O20—C74—C71 | 111.4 (3) |
C15—N5—Ni1 | 122.6 (2) | O20—C75—H75A | 109.5 |
C22—N6—C26 | 117.4 (3) | O20—C75—H75B | 109.5 |
C22—N6—Ni1 | 120.1 (2) | H75A—C75—H75B | 109.5 |
C26—N6—Ni1 | 122.4 (2) | O20—C75—H75C | 109.5 |
N3—C1—C2 | 122.9 (3) | H75A—C75—H75C | 109.5 |
N3—C1—H1 | 118.5 | H75B—C75—H75C | 109.5 |
C2—C1—H1 | 118.5 | N7—Ni2—N8 | 179.63 (13) |
C1—C2—C3 | 119.5 (3) | N7—Ni2—N12 | 90.69 (12) |
C1—C2—H2 | 120.2 | N8—Ni2—N12 | 88.97 (11) |
C3—C2—H2 | 120.2 | N7—Ni2—N11 | 90.27 (11) |
C4—C3—C2 | 117.7 (3) | N8—Ni2—N11 | 89.86 (11) |
C4—C3—C6 | 123.8 (3) | N12—Ni2—N11 | 90.07 (11) |
C2—C3—C6 | 118.4 (3) | N7—Ni2—N10 | 90.64 (12) |
C5—C4—C3 | 119.1 (3) | N8—Ni2—N10 | 89.70 (12) |
C5—C4—H4 | 120.5 | N12—Ni2—N10 | 177.92 (11) |
C3—C4—H4 | 120.5 | N11—Ni2—N10 | 88.32 (10) |
N3—C5—C4 | 123.6 (3) | N7—Ni2—N9 | 88.48 (11) |
N3—C5—H5 | 118.2 | N8—Ni2—N9 | 91.38 (11) |
C4—C5—H5 | 118.2 | N12—Ni2—N9 | 89.61 (10) |
O1—C6—O2 | 124.3 (3) | N11—Ni2—N9 | 178.71 (11) |
O1—C6—C3 | 123.7 (3) | N10—Ni2—N9 | 92.02 (10) |
O2—C6—C3 | 112.0 (3) | N8—C32A—S4A | 177.0 (5) |
O2—C7—H7A | 109.5 | N8—C32B—S4B | 173.5 (19) |
O2—C7—H7B | 109.5 | C38—O10—C39 | 116.2 (3) |
H7A—C7—H7B | 109.5 | C45—O12—C46 | 109.1 (4) |
O2—C7—H7C | 109.5 | C52—O14—C53 | 116.2 (3) |
H7A—C7—H7C | 109.5 | C59—O16—C60 | 114.3 (3) |
H7B—C7—H7C | 109.5 | C31—N7—Ni2 | 159.1 (3) |
N4—C8—C9 | 123.1 (3) | C32B—N8—Ni2 | 166.9 (16) |
N4—C8—H8 | 118.5 | C32A—N8—Ni2 | 158.9 (4) |
C9—C8—H8 | 118.5 | C37—N9—C33 | 116.9 (3) |
C8—C9—C10 | 119.2 (3) | C37—N9—Ni2 | 120.1 (2) |
C8—C9—H9 | 120.4 | C33—N9—Ni2 | 122.8 (2) |
C10—C9—H9 | 120.4 | C40—N10—C44 | 117.1 (3) |
C11—C10—C9 | 118.3 (3) | C40—N10—Ni2 | 120.1 (2) |
C11—C10—C13 | 123.1 (3) | C44—N10—Ni2 | 122.6 (3) |
C9—C10—C13 | 118.5 (3) | C47—N11—C51 | 117.7 (3) |
C12—C11—C10 | 118.5 (3) | C47—N11—Ni2 | 120.3 (2) |
C12—C11—H11 | 120.8 | C51—N11—Ni2 | 121.9 (2) |
C10—C11—H11 | 120.8 | C54—N12—C58 | 118.2 (3) |
N4—C12—C11 | 123.0 (3) | C54—N12—Ni2 | 121.3 (2) |
N4—C12—H12 | 118.5 | C58—N12—Ni2 | 120.5 (2) |
C11—C12—H12 | 118.5 | N7—C31—S3 | 177.8 (4) |
O3—C13—O4 | 124.1 (3) | N9—C33—C34 | 123.1 (3) |
O3—C13—C10 | 124.1 (3) | N9—C33—H33 | 118.4 |
O4—C13—C10 | 111.7 (3) | C34—C33—H33 | 118.4 |
O4—C14—H14A | 109.5 | C33—C34—C35 | 118.8 (3) |
O4—C14—H14B | 109.5 | C33—C34—H34 | 120.6 |
H14A—C14—H14B | 109.5 | C35—C34—H34 | 120.6 |
O4—C14—H14C | 109.5 | C36—C35—C34 | 118.6 (3) |
H14A—C14—H14C | 109.5 | C36—C35—C38 | 121.9 (3) |
H14B—C14—H14C | 109.5 | C34—C35—C38 | 119.4 (3) |
N5—C15—C16 | 122.9 (3) | C35—C36—C37 | 119.1 (3) |
N5—C15—H15 | 118.5 | C35—C36—H36 | 120.5 |
C16—C15—H15 | 118.5 | C37—C36—H36 | 120.5 |
C15—C16—C17 | 118.8 (3) | N9—C37—C36 | 123.4 (3) |
C15—C16—H16 | 120.6 | N9—C37—H37 | 118.3 |
C17—C16—H16 | 120.6 | C36—C37—H37 | 118.3 |
C16—C17—C18 | 118.6 (3) | O9—C38—O10 | 124.8 (3) |
C16—C17—C20 | 119.0 (4) | O9—C38—C35 | 124.0 (3) |
C18—C17—C20 | 122.4 (3) | O10—C38—C35 | 111.1 (3) |
C19—C18—C17 | 118.7 (3) | O10—C39—H39A | 109.5 |
C19—C18—H18 | 120.6 | O10—C39—H39B | 109.5 |
C17—C18—H18 | 120.6 | H39A—C39—H39B | 109.5 |
N5—C19—C18 | 123.0 (3) | O10—C39—H39C | 109.5 |
N5—C19—H19 | 118.5 | H39A—C39—H39C | 109.5 |
C18—C19—H19 | 118.5 | H39B—C39—H39C | 109.5 |
O5—C20—O6 | 124.7 (4) | N10—C40—C41 | 123.5 (3) |
O5—C20—C17 | 124.1 (4) | N10—C40—H40 | 118.2 |
O6—C20—C17 | 111.2 (4) | C41—C40—H40 | 118.2 |
O6—C21—H21A | 109.5 | C42—C41—C40 | 119.0 (4) |
O6—C21—H21B | 109.5 | C42—C41—H41 | 120.5 |
H21A—C21—H21B | 109.5 | C40—C41—H41 | 120.5 |
O6—C21—H21C | 109.5 | C41—C42—C43 | 119.1 (4) |
H21A—C21—H21C | 109.5 | C41—C42—C45 | 115.8 (4) |
H21B—C21—H21C | 109.5 | C43—C42—C45 | 125.1 (4) |
N6—C22—C23 | 123.0 (3) | C42—C43—C44 | 119.1 (4) |
N6—C22—H22 | 118.5 | C42—C43—H43 | 120.5 |
C23—C22—H22 | 118.5 | C44—C43—H43 | 120.5 |
C22—C23—C24 | 118.5 (3) | N10—C44—C43 | 122.3 (4) |
C22—C23—H23 | 120.7 | N10—C44—H44 | 118.9 |
C24—C23—H23 | 120.7 | C43—C44—H44 | 118.9 |
C25—C24—C23 | 119.0 (3) | O11—C45—O12 | 127.4 (4) |
C25—C24—C27 | 119.2 (3) | O11—C45—C42 | 124.2 (4) |
C23—C24—C27 | 121.7 (3) | O12—C45—C42 | 108.3 (4) |
C26—C25—C24 | 118.6 (3) | O12—C46—H46A | 109.5 |
C26—C25—H25 | 120.7 | O12—C46—H46B | 109.5 |
C24—C25—H25 | 120.7 | H46A—C46—H46B | 109.5 |
N6—C26—C25 | 123.4 (3) | O12—C46—H46C | 109.5 |
N6—C26—H26 | 118.3 | H46A—C46—H46C | 109.5 |
C25—C26—H26 | 118.3 | H46B—C46—H46C | 109.5 |
O7—C27—O8 | 123.9 (3) | N11—C47—C48 | 123.4 (3) |
O7—C27—C24 | 124.4 (3) | N11—C47—H47 | 118.3 |
O8—C27—C24 | 111.8 (3) | C48—C47—H47 | 118.3 |
O8—C28—H28A | 109.5 | C47—C48—C49 | 118.4 (3) |
O8—C28—H28B | 109.5 | C47—C48—H48 | 120.8 |
H28A—C28—H28B | 109.5 | C49—C48—H48 | 120.8 |
O8—C28—H28C | 109.5 | C50—C49—C48 | 119.0 (3) |
H28A—C28—H28C | 109.5 | C50—C49—C52 | 119.0 (3) |
H28B—C28—H28C | 109.5 | C48—C49—C52 | 122.0 (3) |
N1—C29—S1 | 178.4 (4) | C51—C50—C49 | 118.8 (3) |
N2—C30—S2 | 179.4 (3) | C51—C50—H50 | 120.6 |
N13i—Ni3—N13 | 180.00 (6) | C49—C50—H50 | 120.6 |
N13i—Ni3—N15 | 89.65 (11) | N11—C51—C50 | 122.5 (3) |
N13—Ni3—N15 | 90.35 (11) | N11—C51—H51 | 118.7 |
N13i—Ni3—N15i | 90.35 (11) | C50—C51—H51 | 118.7 |
N13—Ni3—N15i | 89.65 (11) | O13—C52—O14 | 124.8 (3) |
N15—Ni3—N15i | 180.0 | O13—C52—C49 | 123.0 (3) |
N13i—Ni3—N14 | 89.46 (11) | O14—C52—C49 | 112.2 (3) |
N13—Ni3—N14 | 90.54 (11) | O14—C53—H53A | 109.5 |
N15—Ni3—N14 | 86.23 (10) | O14—C53—H53B | 109.5 |
N15i—Ni3—N14 | 93.77 (10) | H53A—C53—H53B | 109.5 |
N13i—Ni3—N14i | 90.53 (11) | O14—C53—H53C | 109.5 |
N13—Ni3—N14i | 89.47 (11) | H53A—C53—H53C | 109.5 |
N15—Ni3—N14i | 93.77 (10) | H53B—C53—H53C | 109.5 |
N15i—Ni3—N14i | 86.23 (10) | N12—C54—C55 | 122.4 (3) |
N14—Ni3—N14i | 180.0 | N12—C54—H54 | 118.8 |
C67—O18—C68 | 116.1 (4) | C55—C54—H54 | 118.8 |
C74—O20—C75 | 116.1 (3) | C54—C55—C56 | 119.0 (3) |
C61—N13—Ni3 | 169.4 (3) | C54—C55—H55 | 120.5 |
C62—N14—C66 | 116.9 (3) | C56—C55—H55 | 120.5 |
C62—N14—Ni3 | 120.2 (2) | C57—C56—C55 | 118.4 (3) |
C66—N14—Ni3 | 122.9 (2) | C57—C56—C59 | 118.6 (3) |
C69—N15—C73 | 117.4 (3) | C55—C56—C59 | 123.0 (3) |
C69—N15—Ni3 | 121.4 (2) | C58—C57—C56 | 119.1 (3) |
C73—N15—Ni3 | 121.1 (2) | C58—C57—H57 | 120.5 |
N13—C61—S5 | 179.4 (3) | C56—C57—H57 | 120.5 |
N14—C62—C63 | 123.2 (3) | N12—C58—C57 | 123.0 (3) |
N14—C62—H62 | 118.4 | N12—C58—H58 | 118.5 |
C63—C62—H62 | 118.4 | C57—C58—H58 | 118.5 |
C64—C63—C62 | 119.5 (3) | O15—C59—O16 | 125.1 (3) |
C64—C63—H63 | 120.2 | O15—C59—C56 | 123.5 (3) |
C62—C63—H63 | 120.2 | O16—C59—C56 | 111.5 (3) |
C63—C64—C65 | 117.7 (3) | O16—C60—H60A | 109.5 |
C63—C64—C67 | 123.3 (4) | O16—C60—H60B | 109.5 |
C65—C64—C67 | 119.0 (4) | H60A—C60—H60B | 109.5 |
C66—C65—C64 | 119.5 (3) | O16—C60—H60C | 109.5 |
C66—C65—H65 | 120.3 | H60A—C60—H60C | 109.5 |
C64—C65—H65 | 120.3 | H60B—C60—H60C | 109.5 |
N14—C66—C65 | 123.1 (3) | ||
N2—Ni1—N3—C5 | −27.1 (3) | C63—C64—C67—O17 | −172.0 (4) |
N1—Ni1—N3—C5 | 150.9 (3) | C65—C64—C67—O17 | 7.4 (5) |
N4—Ni1—N3—C5 | 63.2 (3) | C63—C64—C67—O18 | 8.8 (5) |
N6—Ni1—N3—C5 | −119.2 (3) | C65—C64—C67—O18 | −171.8 (3) |
N2—Ni1—N3—C1 | 142.0 (3) | C73—N15—C69—C70 | 2.3 (5) |
N1—Ni1—N3—C1 | −40.1 (3) | Ni3—N15—C69—C70 | −174.6 (3) |
N4—Ni1—N3—C1 | −127.8 (3) | N15—C69—C70—C71 | −1.7 (5) |
N6—Ni1—N3—C1 | 49.9 (3) | C69—C70—C71—C72 | −0.7 (5) |
N2—Ni1—N4—C12 | −53.2 (3) | C69—C70—C71—C74 | −179.6 (3) |
N1—Ni1—N4—C12 | 126.7 (3) | C70—C71—C72—C73 | 2.2 (5) |
N5—Ni1—N4—C12 | 36.8 (3) | C74—C71—C72—C73 | −178.9 (3) |
N3—Ni1—N4—C12 | −142.5 (3) | C69—N15—C73—C72 | −0.7 (5) |
N2—Ni1—N4—C8 | 128.7 (3) | Ni3—N15—C73—C72 | 176.3 (2) |
N1—Ni1—N4—C8 | −51.4 (3) | C71—C72—C73—N15 | −1.6 (5) |
N5—Ni1—N4—C8 | −141.4 (2) | C75—O20—C74—O19 | −3.1 (5) |
N3—Ni1—N4—C8 | 39.3 (3) | C75—O20—C74—C71 | 176.8 (3) |
N2—Ni1—N5—C19 | −45.8 (3) | C72—C71—C74—O19 | 1.2 (5) |
N1—Ni1—N5—C19 | 136.3 (3) | C70—C71—C74—O19 | −180.0 (3) |
N4—Ni1—N5—C19 | −136.0 (3) | C72—C71—C74—O20 | −178.7 (3) |
N6—Ni1—N5—C19 | 46.3 (3) | C70—C71—C74—O20 | 0.2 (4) |
N2—Ni1—N5—C15 | 142.9 (3) | N12—Ni2—N7—C31 | −153.5 (8) |
N1—Ni1—N5—C15 | −35.0 (3) | N11—Ni2—N7—C31 | −63.4 (8) |
N4—Ni1—N5—C15 | 52.6 (3) | N10—Ni2—N7—C31 | 24.9 (8) |
N6—Ni1—N5—C15 | −125.0 (3) | N9—Ni2—N7—C31 | 116.9 (8) |
N2—Ni1—N6—C22 | 150.7 (3) | N12—Ni2—N8—C32B | 15 (5) |
N1—Ni1—N6—C22 | −29.3 (3) | N11—Ni2—N8—C32B | −75 (5) |
N5—Ni1—N6—C22 | 60.8 (3) | N10—Ni2—N8—C32B | −163 (5) |
N3—Ni1—N6—C22 | −120.1 (3) | N9—Ni2—N8—C32B | 105 (5) |
N2—Ni1—N6—C26 | −26.8 (3) | N12—Ni2—N8—C32A | −63.0 (13) |
N1—Ni1—N6—C26 | 153.2 (3) | N11—Ni2—N8—C32A | −153.0 (13) |
N5—Ni1—N6—C26 | −116.7 (3) | N10—Ni2—N8—C32A | 118.6 (13) |
N3—Ni1—N6—C26 | 62.3 (3) | N9—Ni2—N8—C32A | 26.6 (13) |
C5—N3—C1—C2 | 2.6 (5) | N7—Ni2—N9—C37 | 152.6 (3) |
Ni1—N3—C1—C2 | −167.1 (3) | N8—Ni2—N9—C37 | −27.0 (3) |
N3—C1—C2—C3 | 1.3 (5) | N12—Ni2—N9—C37 | 61.9 (3) |
C1—C2—C3—C4 | −4.2 (5) | N10—Ni2—N9—C37 | −116.8 (3) |
C1—C2—C3—C6 | 174.6 (3) | N7—Ni2—N9—C33 | −23.3 (3) |
C2—C3—C4—C5 | 3.3 (5) | N8—Ni2—N9—C33 | 157.1 (3) |
C6—C3—C4—C5 | −175.4 (3) | N12—Ni2—N9—C33 | −114.0 (3) |
C1—N3—C5—C4 | −3.5 (5) | N10—Ni2—N9—C33 | 67.3 (3) |
Ni1—N3—C5—C4 | 165.7 (3) | N7—Ni2—N10—C40 | 157.7 (2) |
C3—C4—C5—N3 | 0.6 (5) | N8—Ni2—N10—C40 | −22.2 (2) |
C7—O2—C6—O1 | −3.8 (5) | N11—Ni2—N10—C40 | −112.1 (2) |
C7—O2—C6—C3 | 174.1 (3) | N9—Ni2—N10—C40 | 69.2 (2) |
C4—C3—C6—O1 | −158.0 (4) | N7—Ni2—N10—C44 | −27.7 (3) |
C2—C3—C6—O1 | 23.2 (5) | N8—Ni2—N10—C44 | 152.4 (3) |
C4—C3—C6—O2 | 24.0 (5) | N11—Ni2—N10—C44 | 62.5 (3) |
C2—C3—C6—O2 | −154.7 (3) | N9—Ni2—N10—C44 | −116.2 (3) |
C12—N4—C8—C9 | 1.5 (5) | N7—Ni2—N11—C47 | 139.4 (3) |
Ni1—N4—C8—C9 | 179.8 (3) | N8—Ni2—N11—C47 | −40.9 (3) |
N4—C8—C9—C10 | −3.2 (5) | N12—Ni2—N11—C47 | −129.9 (3) |
C8—C9—C10—C11 | 2.6 (5) | N10—Ni2—N11—C47 | 48.8 (3) |
C8—C9—C10—C13 | −178.5 (3) | N7—Ni2—N11—C51 | −35.2 (3) |
C9—C10—C11—C12 | −0.5 (5) | N8—Ni2—N11—C51 | 144.5 (3) |
C13—C10—C11—C12 | −179.3 (3) | N12—Ni2—N11—C51 | 55.5 (3) |
C8—N4—C12—C11 | 0.7 (5) | N10—Ni2—N11—C51 | −125.8 (3) |
Ni1—N4—C12—C11 | −177.4 (2) | N7—Ni2—N12—C54 | 132.7 (3) |
C10—C11—C12—N4 | −1.2 (5) | N8—Ni2—N12—C54 | −47.5 (3) |
C14—O4—C13—O3 | −2.3 (5) | N11—Ni2—N12—C54 | 42.4 (3) |
C14—O4—C13—C10 | 177.5 (3) | N9—Ni2—N12—C54 | −138.8 (3) |
C11—C10—C13—O3 | 167.5 (3) | N7—Ni2—N12—C58 | −45.3 (3) |
C9—C10—C13—O3 | −11.3 (5) | N8—Ni2—N12—C58 | 134.6 (3) |
C11—C10—C13—O4 | −12.3 (4) | N11—Ni2—N12—C58 | −135.6 (3) |
C9—C10—C13—O4 | 168.9 (3) | N9—Ni2—N12—C58 | 43.2 (3) |
C19—N5—C15—C16 | −0.8 (5) | C37—N9—C33—C34 | 2.1 (5) |
Ni1—N5—C15—C16 | 170.7 (3) | Ni2—N9—C33—C34 | 178.2 (2) |
N5—C15—C16—C17 | −0.5 (5) | N9—C33—C34—C35 | −0.4 (5) |
C15—C16—C17—C18 | 0.4 (5) | C33—C34—C35—C36 | −1.5 (5) |
C15—C16—C17—C20 | 179.6 (3) | C33—C34—C35—C38 | 179.1 (3) |
C16—C17—C18—C19 | 1.0 (5) | C34—C35—C36—C37 | 1.5 (5) |
C20—C17—C18—C19 | −178.2 (3) | C38—C35—C36—C37 | −179.0 (3) |
C15—N5—C19—C18 | 2.3 (5) | C33—N9—C37—C36 | −2.1 (5) |
Ni1—N5—C19—C18 | −169.5 (3) | Ni2—N9—C37—C36 | −178.2 (3) |
C17—C18—C19—N5 | −2.4 (6) | C35—C36—C37—N9 | 0.2 (5) |
C21—O6—C20—O5 | 2.5 (6) | C39—O10—C38—O9 | −3.0 (4) |
C21—O6—C20—C17 | −178.7 (4) | C39—O10—C38—C35 | 176.8 (3) |
C16—C17—C20—O5 | −13.2 (6) | C36—C35—C38—O9 | −175.2 (3) |
C18—C17—C20—O5 | 166.0 (4) | C34—C35—C38—O9 | 4.3 (5) |
C16—C17—C20—O6 | 168.0 (3) | C36—C35—C38—O10 | 5.0 (4) |
C18—C17—C20—O6 | −12.8 (5) | C34—C35—C38—O10 | −175.6 (3) |
C26—N6—C22—C23 | 0.9 (6) | C44—N10—C40—C41 | −0.4 (5) |
Ni1—N6—C22—C23 | −176.7 (3) | Ni2—N10—C40—C41 | 174.5 (2) |
N6—C22—C23—C24 | −0.3 (6) | N10—C40—C41—C42 | −0.5 (5) |
C22—C23—C24—C25 | −0.6 (5) | C40—C41—C42—C43 | 0.8 (5) |
C22—C23—C24—C27 | −179.7 (3) | C40—C41—C42—C45 | −176.4 (3) |
C23—C24—C25—C26 | 0.8 (6) | C41—C42—C43—C44 | −0.3 (5) |
C27—C24—C25—C26 | 179.9 (4) | C45—C42—C43—C44 | 176.6 (3) |
C22—N6—C26—C25 | −0.7 (6) | C40—N10—C44—C43 | 0.9 (5) |
Ni1—N6—C26—C25 | 176.9 (3) | Ni2—N10—C44—C43 | −173.9 (3) |
C24—C25—C26—N6 | −0.2 (6) | C42—C43—C44—N10 | −0.6 (5) |
C28—O8—C27—O7 | 0.6 (5) | C46—O12—C45—O11 | 6.6 (6) |
C28—O8—C27—C24 | 179.7 (3) | C46—O12—C45—C42 | −174.0 (3) |
C25—C24—C27—O7 | −11.2 (6) | C41—C42—C45—O11 | −9.5 (5) |
C23—C24—C27—O7 | 167.9 (4) | C43—C42—C45—O11 | 173.5 (4) |
C25—C24—C27—O8 | 169.7 (3) | C41—C42—C45—O12 | 171.1 (3) |
C23—C24—C27—O8 | −11.2 (5) | C43—C42—C45—O12 | −6.0 (5) |
N15—Ni3—N13—C61 | −102.2 (15) | C51—N11—C47—C48 | 3.4 (5) |
N15i—Ni3—N13—C61 | 77.8 (15) | Ni2—N11—C47—C48 | −171.4 (3) |
N14—Ni3—N13—C61 | −16.0 (15) | N11—C47—C48—C49 | −1.8 (5) |
N14i—Ni3—N13—C61 | 164.0 (15) | C47—C48—C49—C50 | −1.8 (5) |
N13i—Ni3—N14—C62 | 159.3 (3) | C47—C48—C49—C52 | 176.6 (3) |
N13—Ni3—N14—C62 | −20.7 (3) | C48—C49—C50—C51 | 3.6 (5) |
N15—Ni3—N14—C62 | 69.6 (3) | C52—C49—C50—C51 | −174.8 (3) |
N15i—Ni3—N14—C62 | −110.4 (3) | C47—N11—C51—C50 | −1.4 (5) |
N13i—Ni3—N14—C66 | −20.3 (3) | Ni2—N11—C51—C50 | 173.4 (3) |
N13—Ni3—N14—C66 | 159.7 (3) | C49—C50—C51—N11 | −2.1 (5) |
N15—Ni3—N14—C66 | −110.0 (3) | C53—O14—C52—O13 | 4.1 (5) |
N15i—Ni3—N14—C66 | 70.0 (3) | C53—O14—C52—C49 | −175.2 (3) |
N13i—Ni3—N15—C69 | 137.8 (3) | C50—C49—C52—O13 | −20.1 (5) |
N13—Ni3—N15—C69 | −42.2 (3) | C48—C49—C52—O13 | 161.5 (4) |
N14—Ni3—N15—C69 | −132.7 (3) | C50—C49—C52—O14 | 159.2 (3) |
N14i—Ni3—N15—C69 | 47.3 (3) | C48—C49—C52—O14 | −19.2 (5) |
N13i—Ni3—N15—C73 | −39.0 (3) | C58—N12—C54—C55 | −0.3 (5) |
N13—Ni3—N15—C73 | 141.0 (3) | Ni2—N12—C54—C55 | −178.3 (3) |
N14—Ni3—N15—C73 | 50.5 (3) | N12—C54—C55—C56 | 0.3 (5) |
N14i—Ni3—N15—C73 | −129.5 (3) | C54—C55—C56—C57 | −0.3 (5) |
C66—N14—C62—C63 | −1.3 (5) | C54—C55—C56—C59 | 179.8 (3) |
Ni3—N14—C62—C63 | 179.1 (3) | C55—C56—C57—C58 | 0.2 (5) |
N14—C62—C63—C64 | −0.9 (5) | C59—C56—C57—C58 | −179.8 (3) |
C62—C63—C64—C65 | 2.2 (5) | C54—N12—C58—C57 | 0.3 (5) |
C62—C63—C64—C67 | −178.4 (3) | Ni2—N12—C58—C57 | 178.3 (3) |
C63—C64—C65—C66 | −1.4 (5) | C56—C57—C58—N12 | −0.2 (5) |
C67—C64—C65—C66 | 179.3 (3) | C60—O16—C59—O15 | −1.8 (5) |
C62—N14—C66—C65 | 2.2 (5) | C60—O16—C59—C56 | 177.7 (3) |
Ni3—N14—C66—C65 | −178.2 (3) | C57—C56—C59—O15 | 21.1 (5) |
C64—C65—C66—N14 | −0.9 (5) | C55—C56—C59—O15 | −158.9 (3) |
C68—O18—C67—O17 | 2.6 (5) | C57—C56—C59—O16 | −158.4 (3) |
C68—O18—C67—C64 | −178.2 (3) | C55—C56—C59—O16 | 21.5 (4) |
Symmetry code: (i) −x+1, −y, −z+1. |
C50H36N6NiO4S2 | F(000) = 940 |
Mr = 907.68 | Dx = 1.454 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9821 reflections |
a = 8.9345 (3) Å | θ = 2.5–33.3° |
b = 20.8306 (6) Å | µ = 0.63 mm−1 |
c = 11.1406 (3) Å | T = 100 K |
β = 90.660 (1)° | Block, blue |
V = 2073.25 (11) Å3 | 0.23 × 0.21 × 0.20 mm |
Z = 2 |
Bruker APEX-II CCD diffractometer | 6132 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
φ and ω scans | θmax = 31.0°, θmin = 2.0° |
Absorption correction: multi-scan SADABS (Bruker, 2008) | h = −12→12 |
Tmin = 0.868, Tmax = 0.883 | k = −30→29 |
73945 measured reflections | l = −16→16 |
6604 independent 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)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.072 | H-atom parameters constrained |
S = 0.88 | w = 1/[σ2(Fo2) + (0.0395P)2 + 1.5386P] where P = (Fo2 + 2Fc2)/3 |
6604 reflections | (Δ/σ)max = 0.002 |
286 parameters | Δρmax = 0.49 e Å−3 |
0 restraints | Δρmin = −0.43 e Å−3 |
C50H36N6NiO4S2 | V = 2073.25 (11) Å3 |
Mr = 907.68 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 8.9345 (3) Å | µ = 0.63 mm−1 |
b = 20.8306 (6) Å | T = 100 K |
c = 11.1406 (3) Å | 0.23 × 0.21 × 0.20 mm |
β = 90.660 (1)° |
Bruker APEX-II CCD diffractometer | 6604 independent reflections |
Absorption correction: multi-scan SADABS (Bruker, 2008) | 6132 reflections with I > 2σ(I) |
Tmin = 0.868, Tmax = 0.883 | Rint = 0.028 |
73945 measured reflections |
R[F2 > 2σ(F2)] = 0.027 | 0 restraints |
wR(F2) = 0.072 | H-atom parameters constrained |
S = 0.88 | Δρmax = 0.49 e Å−3 |
6604 reflections | Δρmin = −0.43 e Å−3 |
286 parameters |
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 | 0.5000 | 0.5000 | 0.5000 | 0.00931 (4) | |
S1 | 0.00788 (3) | 0.452494 (14) | 0.65065 (2) | 0.01886 (6) | |
O1 | 0.30714 (9) | 0.42017 (4) | −0.09757 (7) | 0.02088 (15) | |
O2 | 0.36910 (12) | 0.79801 (4) | 0.20182 (7) | 0.02781 (19) | |
N1 | 0.28873 (9) | 0.48979 (4) | 0.56630 (7) | 0.01282 (14) | |
N2 | 0.42649 (9) | 0.45719 (4) | 0.33272 (7) | 0.01185 (14) | |
N3 | 0.44349 (9) | 0.59323 (4) | 0.42740 (7) | 0.01170 (14) | |
C1 | 0.17098 (10) | 0.47491 (4) | 0.60157 (8) | 0.01185 (15) | |
C2 | 0.50511 (10) | 0.46678 (5) | 0.23202 (8) | 0.01318 (16) | |
H2 | 0.5953 | 0.4908 | 0.2374 | 0.016* | |
C3 | 0.46089 (11) | 0.44330 (5) | 0.12080 (8) | 0.01344 (16) | |
H3 | 0.5194 | 0.4516 | 0.0519 | 0.016* | |
C4 | 0.33011 (10) | 0.40746 (5) | 0.11097 (8) | 0.01248 (16) | |
C5 | 0.24812 (11) | 0.39702 (5) | 0.21489 (9) | 0.01552 (17) | |
H5 | 0.1584 | 0.3726 | 0.2121 | 0.019* | |
C6 | 0.29965 (11) | 0.42296 (5) | 0.32268 (8) | 0.01519 (17) | |
H6 | 0.2422 | 0.4161 | 0.3928 | 0.018* | |
C7 | 0.28077 (11) | 0.38548 (5) | −0.01204 (8) | 0.01409 (16) | |
C8 | 0.20366 (11) | 0.32269 (5) | −0.02899 (8) | 0.01377 (16) | |
C9 | 0.11775 (11) | 0.31398 (5) | −0.13376 (9) | 0.01688 (18) | |
H9 | 0.1064 | 0.3482 | −0.1895 | 0.020* | |
C10 | 0.04931 (12) | 0.25522 (6) | −0.15584 (9) | 0.01966 (19) | |
H10 | −0.0098 | 0.2494 | −0.2264 | 0.024* | |
C11 | 0.06708 (12) | 0.20484 (5) | −0.07489 (10) | 0.01912 (19) | |
H11 | 0.0203 | 0.1647 | −0.0905 | 0.023* | |
C12 | 0.15312 (13) | 0.21312 (5) | 0.02873 (10) | 0.01990 (19) | |
H12 | 0.1658 | 0.1786 | 0.0836 | 0.024* | |
C13 | 0.22070 (12) | 0.27208 (5) | 0.05197 (9) | 0.01764 (18) | |
H13 | 0.2786 | 0.2779 | 0.1232 | 0.021* | |
C15 | 0.32319 (11) | 0.62434 (5) | 0.46824 (9) | 0.01432 (17) | |
H15 | 0.2609 | 0.6031 | 0.5242 | 0.017* | |
C16 | 0.28511 (11) | 0.68630 (5) | 0.43272 (9) | 0.01547 (17) | |
H16 | 0.1996 | 0.7069 | 0.4649 | 0.019* | |
C17 | 0.37364 (11) | 0.71766 (5) | 0.34957 (8) | 0.01316 (16) | |
C18 | 0.49500 (11) | 0.68444 (5) | 0.30248 (8) | 0.01441 (17) | |
H18 | 0.5552 | 0.7036 | 0.2425 | 0.017* | |
C19 | 0.52683 (11) | 0.62331 (5) | 0.34403 (8) | 0.01391 (16) | |
H19 | 0.6111 | 0.6015 | 0.3125 | 0.017* | |
C20 | 0.33871 (12) | 0.78402 (5) | 0.30513 (9) | 0.01593 (17) | |
C21 | 0.26953 (11) | 0.83200 (5) | 0.38672 (9) | 0.01444 (17) | |
C22 | 0.19060 (11) | 0.88318 (5) | 0.33464 (10) | 0.01767 (18) | |
H22 | 0.1749 | 0.8843 | 0.2502 | 0.021* | |
C23 | 0.13520 (12) | 0.93228 (5) | 0.40574 (11) | 0.0207 (2) | |
H23 | 0.0811 | 0.9668 | 0.3701 | 0.025* | |
C24 | 0.15925 (12) | 0.93078 (5) | 0.52941 (11) | 0.0215 (2) | |
H24 | 0.1220 | 0.9645 | 0.5781 | 0.026* | |
C25 | 0.23751 (13) | 0.88025 (5) | 0.58189 (10) | 0.01986 (19) | |
H25 | 0.2536 | 0.8796 | 0.6663 | 0.024* | |
C26 | 0.29246 (12) | 0.83053 (5) | 0.51114 (9) | 0.01643 (18) | |
H26 | 0.3452 | 0.7958 | 0.5472 | 0.020* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.00923 (8) | 0.00948 (8) | 0.00924 (7) | −0.00045 (5) | 0.00058 (5) | −0.00010 (5) |
S1 | 0.01119 (10) | 0.02633 (13) | 0.01909 (11) | −0.00239 (9) | 0.00190 (8) | 0.00632 (9) |
O1 | 0.0269 (4) | 0.0232 (4) | 0.0125 (3) | −0.0063 (3) | −0.0008 (3) | 0.0026 (3) |
O2 | 0.0499 (6) | 0.0185 (4) | 0.0151 (3) | 0.0079 (4) | 0.0036 (3) | 0.0035 (3) |
N1 | 0.0126 (3) | 0.0136 (3) | 0.0122 (3) | 0.0003 (3) | −0.0001 (3) | 0.0004 (3) |
N2 | 0.0130 (3) | 0.0115 (3) | 0.0111 (3) | −0.0003 (3) | 0.0005 (3) | 0.0000 (3) |
N3 | 0.0128 (3) | 0.0109 (3) | 0.0114 (3) | −0.0003 (3) | −0.0003 (3) | −0.0007 (3) |
C1 | 0.0127 (4) | 0.0119 (4) | 0.0109 (4) | 0.0014 (3) | −0.0014 (3) | 0.0004 (3) |
C2 | 0.0128 (4) | 0.0144 (4) | 0.0124 (4) | −0.0018 (3) | 0.0010 (3) | −0.0001 (3) |
C3 | 0.0146 (4) | 0.0146 (4) | 0.0111 (4) | −0.0007 (3) | 0.0015 (3) | 0.0005 (3) |
C4 | 0.0146 (4) | 0.0126 (4) | 0.0102 (4) | 0.0004 (3) | 0.0000 (3) | −0.0003 (3) |
C5 | 0.0155 (4) | 0.0184 (4) | 0.0126 (4) | −0.0049 (3) | 0.0013 (3) | −0.0020 (3) |
C6 | 0.0162 (4) | 0.0176 (4) | 0.0118 (4) | −0.0046 (3) | 0.0023 (3) | −0.0017 (3) |
C7 | 0.0143 (4) | 0.0162 (4) | 0.0117 (4) | 0.0001 (3) | −0.0004 (3) | −0.0011 (3) |
C8 | 0.0140 (4) | 0.0155 (4) | 0.0118 (4) | 0.0004 (3) | 0.0006 (3) | −0.0022 (3) |
C9 | 0.0169 (4) | 0.0207 (5) | 0.0130 (4) | 0.0001 (3) | −0.0012 (3) | −0.0017 (3) |
C10 | 0.0172 (4) | 0.0247 (5) | 0.0170 (4) | −0.0021 (4) | −0.0018 (3) | −0.0053 (4) |
C11 | 0.0173 (4) | 0.0189 (5) | 0.0213 (5) | −0.0029 (4) | 0.0039 (4) | −0.0068 (4) |
C12 | 0.0243 (5) | 0.0157 (4) | 0.0197 (4) | −0.0007 (4) | 0.0005 (4) | −0.0005 (4) |
C13 | 0.0213 (5) | 0.0168 (4) | 0.0148 (4) | −0.0002 (4) | −0.0031 (3) | −0.0009 (3) |
C15 | 0.0148 (4) | 0.0122 (4) | 0.0160 (4) | −0.0003 (3) | 0.0030 (3) | 0.0005 (3) |
C16 | 0.0151 (4) | 0.0123 (4) | 0.0190 (4) | 0.0015 (3) | 0.0032 (3) | 0.0000 (3) |
C17 | 0.0160 (4) | 0.0108 (4) | 0.0126 (4) | 0.0000 (3) | −0.0012 (3) | 0.0000 (3) |
C18 | 0.0169 (4) | 0.0137 (4) | 0.0127 (4) | −0.0001 (3) | 0.0017 (3) | 0.0013 (3) |
C19 | 0.0145 (4) | 0.0139 (4) | 0.0134 (4) | 0.0013 (3) | 0.0017 (3) | 0.0007 (3) |
C20 | 0.0206 (4) | 0.0117 (4) | 0.0155 (4) | 0.0011 (3) | −0.0018 (3) | 0.0006 (3) |
C21 | 0.0152 (4) | 0.0108 (4) | 0.0173 (4) | −0.0001 (3) | −0.0001 (3) | 0.0009 (3) |
C22 | 0.0164 (4) | 0.0150 (4) | 0.0215 (5) | 0.0005 (3) | −0.0028 (3) | 0.0028 (4) |
C23 | 0.0168 (4) | 0.0152 (4) | 0.0301 (5) | 0.0043 (3) | 0.0009 (4) | 0.0031 (4) |
C24 | 0.0211 (5) | 0.0157 (5) | 0.0279 (5) | 0.0031 (4) | 0.0064 (4) | −0.0015 (4) |
C25 | 0.0247 (5) | 0.0167 (5) | 0.0184 (4) | 0.0015 (4) | 0.0041 (4) | −0.0008 (4) |
C26 | 0.0195 (4) | 0.0127 (4) | 0.0171 (4) | 0.0017 (3) | 0.0009 (3) | 0.0017 (3) |
Ni1—N1i | 2.0459 (8) | C10—C11 | 1.3917 (16) |
Ni1—N1 | 2.0459 (8) | C10—H10 | 0.9500 |
Ni1—N3 | 2.1613 (8) | C11—C12 | 1.3903 (15) |
Ni1—N3i | 2.1613 (8) | C11—H11 | 0.9500 |
Ni1—N2i | 2.1613 (8) | C12—C13 | 1.3917 (15) |
Ni1—N2 | 2.1613 (8) | C12—H12 | 0.9500 |
S1—C1 | 1.6306 (10) | C13—H13 | 0.9500 |
O1—C7 | 1.2210 (12) | C15—C16 | 1.3909 (13) |
O2—C20 | 1.2208 (13) | C15—H15 | 0.9500 |
N1—C1 | 1.1691 (12) | C16—C17 | 1.3884 (13) |
N2—C6 | 1.3425 (12) | C16—H16 | 0.9500 |
N2—C2 | 1.3454 (12) | C17—C18 | 1.3938 (13) |
N3—C15 | 1.3393 (12) | C17—C20 | 1.5000 (13) |
N3—C19 | 1.3512 (12) | C18—C19 | 1.3834 (13) |
C2—C3 | 1.3854 (13) | C18—H18 | 0.9500 |
C2—H2 | 0.9500 | C19—H19 | 0.9500 |
C3—C4 | 1.3899 (13) | C20—C21 | 1.4899 (14) |
C3—H3 | 0.9500 | C21—C26 | 1.3992 (14) |
C4—C5 | 1.3942 (13) | C21—C22 | 1.4005 (13) |
C4—C7 | 1.5059 (13) | C22—C23 | 1.3882 (15) |
C5—C6 | 1.3904 (13) | C22—H22 | 0.9500 |
C5—H5 | 0.9500 | C23—C24 | 1.3923 (17) |
C6—H6 | 0.9500 | C23—H23 | 0.9500 |
C7—C8 | 1.4894 (14) | C24—C25 | 1.3891 (15) |
C8—C13 | 1.3946 (14) | C24—H24 | 0.9500 |
C8—C9 | 1.4013 (13) | C25—C26 | 1.3942 (14) |
C9—C10 | 1.3890 (15) | C25—H25 | 0.9500 |
C9—H9 | 0.9500 | C26—H26 | 0.9500 |
N1i—Ni1—N1 | 180.0 | C9—C10—H10 | 119.9 |
N1i—Ni1—N3 | 89.08 (3) | C11—C10—H10 | 119.9 |
N1—Ni1—N3 | 90.92 (3) | C12—C11—C10 | 120.16 (10) |
N1i—Ni1—N3i | 90.91 (3) | C12—C11—H11 | 119.9 |
N1—Ni1—N3i | 89.08 (3) | C10—C11—H11 | 119.9 |
N3—Ni1—N3i | 180.0 | C11—C12—C13 | 119.90 (10) |
N1i—Ni1—N2i | 89.77 (3) | C11—C12—H12 | 120.0 |
N1—Ni1—N2i | 90.23 (3) | C13—C12—H12 | 120.0 |
N3—Ni1—N2i | 91.11 (3) | C12—C13—C8 | 120.19 (9) |
N3i—Ni1—N2i | 88.90 (3) | C12—C13—H13 | 119.9 |
N1i—Ni1—N2 | 90.23 (3) | C8—C13—H13 | 119.9 |
N1—Ni1—N2 | 89.77 (3) | N3—C15—C16 | 123.16 (9) |
N3—Ni1—N2 | 88.89 (3) | N3—C15—H15 | 118.4 |
N3i—Ni1—N2 | 91.10 (3) | C16—C15—H15 | 118.4 |
N2i—Ni1—N2 | 180.0 | C17—C16—C15 | 119.15 (9) |
C1—N1—Ni1 | 170.56 (8) | C17—C16—H16 | 120.4 |
C6—N2—C2 | 117.24 (8) | C15—C16—H16 | 120.4 |
C6—N2—Ni1 | 122.60 (6) | C16—C17—C18 | 117.98 (9) |
C2—N2—Ni1 | 120.09 (6) | C16—C17—C20 | 122.41 (9) |
C15—N3—C19 | 117.38 (8) | C18—C17—C20 | 119.55 (9) |
C15—N3—Ni1 | 119.52 (6) | C19—C18—C17 | 119.27 (9) |
C19—N3—Ni1 | 123.08 (6) | C19—C18—H18 | 120.4 |
N1—C1—S1 | 178.73 (9) | C17—C18—H18 | 120.4 |
N2—C2—C3 | 123.17 (9) | N3—C19—C18 | 122.97 (9) |
N2—C2—H2 | 118.4 | N3—C19—H19 | 118.5 |
C3—C2—H2 | 118.4 | C18—C19—H19 | 118.5 |
C2—C3—C4 | 119.41 (8) | O2—C20—C21 | 120.89 (9) |
C2—C3—H3 | 120.3 | O2—C20—C17 | 118.91 (9) |
C4—C3—H3 | 120.3 | C21—C20—C17 | 120.20 (8) |
C3—C4—C5 | 117.88 (8) | C26—C21—C22 | 119.62 (9) |
C3—C4—C7 | 118.17 (8) | C26—C21—C20 | 122.19 (9) |
C5—C4—C7 | 123.86 (9) | C22—C21—C20 | 117.93 (9) |
C6—C5—C4 | 118.99 (9) | C23—C22—C21 | 120.38 (10) |
C6—C5—H5 | 120.5 | C23—C22—H22 | 119.8 |
C4—C5—H5 | 120.5 | C21—C22—H22 | 119.8 |
N2—C6—C5 | 123.31 (9) | C22—C23—C24 | 119.74 (10) |
N2—C6—H6 | 118.3 | C22—C23—H23 | 120.1 |
C5—C6—H6 | 118.3 | C24—C23—H23 | 120.1 |
O1—C7—C8 | 120.92 (9) | C25—C24—C23 | 120.31 (10) |
O1—C7—C4 | 118.24 (9) | C25—C24—H24 | 119.8 |
C8—C7—C4 | 120.83 (8) | C23—C24—H24 | 119.8 |
C13—C8—C9 | 119.71 (9) | C24—C25—C26 | 120.25 (10) |
C13—C8—C7 | 122.34 (8) | C24—C25—H25 | 119.9 |
C9—C8—C7 | 117.86 (9) | C26—C25—H25 | 119.9 |
C10—C9—C8 | 119.82 (10) | C25—C26—C21 | 119.69 (9) |
C10—C9—H9 | 120.1 | C25—C26—H26 | 120.2 |
C8—C9—H9 | 120.1 | C21—C26—H26 | 120.2 |
C9—C10—C11 | 120.21 (9) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Experimental details
(I) | (II) | (III) | |
Crystal data | |||
Chemical formula | C34H36N6NiO8S2 | C30H28N6NiO8S2 | C50H36N6NiO4S2 |
Mr | 779.52 | 723.41 | 907.68 |
Crystal system, space group | Monoclinic, P21 | Monoclinic, P21/n | Monoclinic, P21/c |
Temperature (K) | 100 | 100 | 100 |
a, b, c (Å) | 11.8719 (4), 14.1629 (5), 21.9663 (7) | 11.8991 (3), 51.4066 (12), 14.1366 (3) | 8.9345 (3), 20.8306 (6), 11.1406 (3) |
β (°) | 95.342 (1) | 99.498 (1) | 90.660 (1) |
V (Å3) | 3677.4 (2) | 8528.7 (3) | 2073.25 (11) |
Z | 4 | 10 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.70 | 0.75 | 0.63 |
Crystal size (mm) | 0.45 × 0.14 × 0.12 | 0.57 × 0.19 × 0.15 | 0.23 × 0.21 × 0.20 |
Data collection | |||
Diffractometer | Bruker APEX-II CCD diffractometer | Bruker APEX-II CCD diffractometer | Bruker APEX-II CCD diffractometer |
Absorption correction | Multi-scan SADABS (Bruker, 2008) | Multi-scan SADABS (Bruker, 2008) | Multi-scan SADABS (Bruker, 2008) |
Tmin, Tmax | 0.745, 0.922 | 0.843, 0.894 | 0.868, 0.883 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 50874, 14290, 12276 | 79032, 14949, 11076 | 73945, 6604, 6132 |
Rint | 0.000 | 0.078 | 0.028 |
(sin θ/λ)max (Å−1) | 0.617 | 0.595 | 0.725 |
Refinement | |||
R[F2 > 2σ(F2)], wR(F2), S | 0.030, 0.072, 0.96 | 0.050, 0.127, 1.07 | 0.027, 0.072, 0.88 |
No. of reflections | 14290 | 14949 | 6604 |
No. of parameters | 938 | 1078 | 286 |
No. of restraints | 1 | 0 | 0 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.55, −0.35 | 1.00, −0.55 | 0.49, −0.43 |
Absolute structure | Flack (1983), 6750 Friedel pairs | ? | ? |
Absolute structure parameter | −0.008 (6) | ? | ? |
Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SAINT, SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Bruker, 2008), SHELXTL.