Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805032046/cv6583sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805032046/cv6583Isup2.hkl |
CCDC reference: 289703
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.
[Ni(C14H12N4)2](ClO4)2·2CHCl3 | F(000) = 3920 |
Mr = 968.90 | Dx = 1.571 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1006 reflections |
a = 22.297 (6) Å | θ = 3.0–22.6° |
b = 17.257 (5) Å | µ = 1.05 mm−1 |
c = 23.801 (7) Å | T = 293 K |
β = 116.551 (4)° | Block, purple |
V = 8192 (4) Å3 | 0.36 × 0.30 × 0.30 mm |
Z = 8 |
Bruker SMART CCD area-detector diffractometer | 8395 independent reflections |
Radiation source: fine-focus sealed tube | 4749 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.055 |
φ and ω scans | θmax = 26.4°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −27→27 |
Tmin = 0.703, Tmax = 0.743 | k = −18→21 |
23272 measured reflections | l = −29→27 |
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)] = 0.060 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.166 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0746P)2 + 8.6393P] where P = (Fo2 + 2Fc2)/3 |
8395 reflections | (Δ/σ)max = 0.002 |
552 parameters | Δρmax = 0.62 e Å−3 |
13 restraints | Δρmin = −0.39 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ni1 | 0.0000 | 1.28352 (5) | −0.2500 | 0.0438 (2) | |
Ni2 | 0.5000 | 0.75080 (4) | 0.2500 | 0.0379 (2) | |
N1 | 0.06784 (18) | 1.2008 (2) | −0.18690 (17) | 0.0484 (9) | |
N2 | −0.0297 (2) | 1.2772 (2) | −0.1824 (2) | 0.0614 (11) | |
N3 | −0.0704 (2) | 1.3185 (3) | −0.1688 (2) | 0.0750 (13) | |
N4 | −0.07487 (19) | 1.3747 (2) | −0.2917 (2) | 0.0575 (10) | |
N5 | 0.51876 (16) | 0.83151 (19) | 0.19123 (16) | 0.0433 (8) | |
N6 | 0.41159 (16) | 0.75905 (19) | 0.17589 (16) | 0.0417 (8) | |
N7 | 0.35199 (16) | 0.7249 (2) | 0.16049 (16) | 0.0451 (8) | |
N8 | 0.54203 (18) | 0.6570 (2) | 0.21789 (16) | 0.0443 (8) | |
Cl1 | 0.22217 (5) | 0.85253 (7) | 0.21369 (5) | 0.0527 (3) | |
Cl2 | 0.31475 (7) | 0.94498 (8) | −0.07571 (6) | 0.0636 (4) | |
Cl3 | 0.0704 (9) | 0.9713 (9) | 0.0293 (5) | 0.220 (7) | 0.446 (12) |
Cl4 | 0.0794 (6) | 0.8234 (7) | −0.0067 (6) | 0.182 (5) | 0.446 (12) |
Cl5 | 0.1768 (6) | 0.9234 (7) | −0.0014 (6) | 0.166 (5) | 0.446 (12) |
Cl3' | 0.1260 (7) | 0.9974 (4) | 0.0607 (4) | 0.177 (4) | 0.554 (12) |
Cl4' | 0.0536 (5) | 0.8596 (10) | −0.0089 (5) | 0.267 (8) | 0.554 (12) |
Cl5' | 0.1765 (5) | 0.9079 (5) | −0.0035 (4) | 0.136 (3) | 0.554 (12) |
Cl6 | 0.37780 (18) | 1.29730 (18) | −0.09952 (14) | 0.1876 (13) | |
Cl7 | 0.25214 (15) | 1.30647 (17) | −0.08823 (15) | 0.1887 (14) | |
Cl8 | 0.33786 (12) | 1.17873 (15) | −0.04279 (14) | 0.1537 (10) | |
C1 | 0.1137 (2) | 1.1599 (3) | −0.1955 (2) | 0.0562 (12) | |
H1A | 0.1149 | 1.1636 | −0.2340 | 0.067* | |
C2 | 0.1590 (3) | 1.1127 (3) | −0.1507 (3) | 0.0696 (14) | |
H2A | 0.1908 | 1.0858 | −0.1583 | 0.083* | |
C3 | 0.1571 (3) | 1.1056 (3) | −0.0943 (3) | 0.0754 (16) | |
H3A | 0.1874 | 1.0736 | −0.0630 | 0.090* | |
C4 | 0.1094 (3) | 1.1467 (3) | −0.0844 (2) | 0.0679 (14) | |
H4A | 0.1071 | 1.1427 | −0.0464 | 0.081* | |
C5 | 0.0656 (2) | 1.1936 (3) | −0.1317 (2) | 0.0531 (11) | |
C6 | 0.0131 (3) | 1.2408 (3) | −0.1274 (2) | 0.0651 (14) | |
C7 | −0.0034 (3) | 1.2628 (4) | −0.0811 (3) | 0.095 (2) | |
H7A | 0.0177 | 1.2480 | −0.0391 | 0.113* | |
C8 | −0.0582 (3) | 1.3122 (4) | −0.1093 (3) | 0.0810 (17) | |
H8A | −0.0816 | 1.3360 | −0.0901 | 0.097* | |
C9 | −0.1293 (3) | 1.3516 (4) | −0.2194 (3) | 0.0813 (17) | |
H9A | −0.1507 | 1.3856 | −0.2013 | 0.098* | |
H9B | −0.1605 | 1.3099 | −0.2404 | 0.098* | |
C10 | −0.1183 (2) | 1.3977 (3) | −0.2694 (3) | 0.0628 (14) | |
C11 | −0.1607 (3) | 1.4589 (3) | −0.2958 (3) | 0.0759 (16) | |
H11A | −0.1892 | 1.4749 | −0.2791 | 0.091* | |
C12 | −0.1613 (3) | 1.4969 (3) | −0.3469 (4) | 0.091 (2) | |
H12A | −0.1905 | 1.5380 | −0.3653 | 0.110* | |
C13 | −0.1183 (3) | 1.4729 (3) | −0.3699 (3) | 0.0834 (18) | |
H13A | −0.1179 | 1.4970 | −0.4046 | 0.100* | |
C14 | −0.0761 (3) | 1.4128 (3) | −0.3408 (3) | 0.0747 (16) | |
H14A | −0.0463 | 1.3974 | −0.3563 | 0.090* | |
C15 | 0.5765 (2) | 0.8667 (3) | 0.2021 (2) | 0.0586 (13) | |
H15A | 0.6121 | 0.8633 | 0.2421 | 0.070* | |
C16 | 0.5856 (3) | 0.9075 (3) | 0.1570 (3) | 0.0687 (15) | |
H16A | 0.6266 | 0.9305 | 0.1661 | 0.082* | |
C17 | 0.5329 (3) | 0.9137 (3) | 0.0983 (3) | 0.0743 (16) | |
H17A | 0.5376 | 0.9416 | 0.0671 | 0.089* | |
C18 | 0.4728 (3) | 0.8782 (3) | 0.0858 (2) | 0.0632 (13) | |
H18A | 0.4367 | 0.8817 | 0.0461 | 0.076* | |
C19 | 0.4673 (2) | 0.8375 (2) | 0.13311 (19) | 0.0444 (10) | |
C20 | 0.4061 (2) | 0.7983 (2) | 0.12562 (19) | 0.0424 (10) | |
C21 | 0.3416 (2) | 0.7918 (3) | 0.0779 (2) | 0.0581 (13) | |
H21A | 0.3243 | 0.8145 | 0.0383 | 0.070* | |
C22 | 0.3086 (2) | 0.7448 (3) | 0.1015 (2) | 0.0567 (12) | |
H22A | 0.2640 | 0.7295 | 0.0804 | 0.068* | |
C23 | 0.3396 (2) | 0.6870 (3) | 0.2087 (2) | 0.0524 (11) | |
H23A | 0.2980 | 0.6581 | 0.1883 | 0.063* | |
H23B | 0.3329 | 0.7267 | 0.2342 | 0.063* | |
C24 | 0.4977 (2) | 0.6089 (3) | 0.1751 (2) | 0.0529 (12) | |
H24A | 0.4532 | 0.6247 | 0.1543 | 0.063* | |
C25 | 0.5142 (3) | 0.5384 (3) | 0.1603 (3) | 0.0704 (15) | |
H25A | 0.4819 | 0.5078 | 0.1294 | 0.085* | |
C26 | 0.5792 (3) | 0.5132 (3) | 0.1915 (3) | 0.0742 (16) | |
H26A | 0.5916 | 0.4650 | 0.1828 | 0.089* | |
C27 | 0.6255 (3) | 0.5610 (3) | 0.2359 (2) | 0.0634 (14) | |
H27A | 0.6697 | 0.5448 | 0.2579 | 0.076* | |
C28 | 0.6068 (2) | 0.6325 (2) | 0.2482 (2) | 0.0443 (10) | |
C29 | 0.1283 (3) | 0.9023 (3) | 0.0362 (3) | 0.107 (2) | |
H29A | 0.1549 | 0.8847 | 0.0784 | 0.128* | |
C30 | 0.3092 (4) | 1.2459 (5) | −0.0986 (4) | 0.125 (3) | |
H30A | 0.2857 | 1.2200 | −0.1382 | 0.150* | |
O1 | 0.25559 (18) | 0.8520 (2) | 0.17488 (18) | 0.0793 (11) | |
O2 | 0.2480 (2) | 0.7929 (3) | 0.25923 (19) | 0.0984 (14) | |
O3 | 0.2340 (2) | 0.9252 (3) | 0.2451 (2) | 0.1095 (16) | |
O4 | 0.15180 (17) | 0.8421 (2) | 0.17710 (18) | 0.0812 (11) | |
O5 | 0.3265 (2) | 0.8645 (2) | −0.0641 (2) | 0.0921 (13) | |
O6' | 0.3635 (11) | 0.9920 (8) | −0.0317 (8) | 0.231 (13) | 0.554 (12) |
O7' | 0.3113 (10) | 0.9569 (9) | −0.1350 (5) | 0.143 (6) | 0.554 (12) |
O8' | 0.2458 (5) | 0.9536 (7) | −0.0905 (11) | 0.162 (7) | 0.554 (12) |
O6 | 0.3821 (5) | 0.9690 (8) | −0.0537 (8) | 0.104 (5) | 0.446 (12) |
O7 | 0.2801 (10) | 0.9736 (12) | −0.1364 (5) | 0.145 (9) | 0.446 (12) |
O8 | 0.2932 (11) | 0.9742 (9) | −0.0326 (8) | 0.128 (6) | 0.446 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0397 (4) | 0.0493 (5) | 0.0469 (5) | 0.000 | 0.0234 (4) | 0.000 |
Ni2 | 0.0344 (4) | 0.0381 (4) | 0.0389 (4) | 0.000 | 0.0142 (3) | 0.000 |
N1 | 0.049 (2) | 0.049 (2) | 0.047 (2) | −0.0031 (18) | 0.0219 (18) | −0.0014 (17) |
N2 | 0.053 (2) | 0.073 (3) | 0.071 (3) | −0.012 (2) | 0.039 (2) | −0.019 (2) |
N3 | 0.062 (3) | 0.099 (4) | 0.076 (3) | −0.011 (3) | 0.042 (3) | −0.027 (3) |
N4 | 0.049 (2) | 0.051 (2) | 0.067 (3) | 0.0024 (19) | 0.022 (2) | 0.000 (2) |
N5 | 0.038 (2) | 0.042 (2) | 0.046 (2) | 0.0008 (16) | 0.0162 (17) | 0.0038 (16) |
N6 | 0.0354 (19) | 0.043 (2) | 0.046 (2) | −0.0020 (16) | 0.0181 (16) | −0.0024 (16) |
N7 | 0.0345 (19) | 0.051 (2) | 0.049 (2) | −0.0017 (16) | 0.0177 (17) | −0.0023 (17) |
N8 | 0.050 (2) | 0.043 (2) | 0.044 (2) | 0.0021 (17) | 0.0236 (17) | −0.0023 (16) |
Cl1 | 0.0449 (6) | 0.0615 (7) | 0.0548 (7) | 0.0060 (5) | 0.0252 (5) | 0.0012 (6) |
Cl2 | 0.0596 (8) | 0.0631 (8) | 0.0684 (9) | 0.0054 (6) | 0.0288 (7) | 0.0121 (7) |
Cl3 | 0.281 (14) | 0.251 (11) | 0.128 (7) | 0.158 (11) | 0.092 (9) | 0.007 (7) |
Cl4 | 0.262 (14) | 0.191 (8) | 0.148 (9) | −0.040 (8) | 0.141 (10) | −0.024 (7) |
Cl5 | 0.136 (8) | 0.177 (8) | 0.190 (10) | −0.045 (6) | 0.078 (7) | 0.064 (7) |
Cl3' | 0.258 (10) | 0.161 (5) | 0.131 (6) | 0.081 (6) | 0.104 (6) | 0.021 (4) |
Cl4' | 0.138 (6) | 0.450 (19) | 0.149 (7) | −0.133 (10) | 0.005 (5) | 0.116 (10) |
Cl5' | 0.158 (7) | 0.146 (5) | 0.117 (5) | 0.059 (4) | 0.072 (5) | −0.009 (4) |
Cl6 | 0.247 (3) | 0.173 (3) | 0.144 (2) | −0.076 (2) | 0.089 (2) | −0.0144 (18) |
Cl7 | 0.160 (2) | 0.137 (2) | 0.191 (3) | 0.0398 (19) | 0.009 (2) | −0.0127 (19) |
Cl8 | 0.1279 (18) | 0.1214 (18) | 0.183 (2) | 0.0053 (14) | 0.0441 (17) | 0.0252 (17) |
C1 | 0.056 (3) | 0.063 (3) | 0.054 (3) | 0.004 (3) | 0.028 (2) | 0.000 (2) |
C2 | 0.064 (3) | 0.068 (3) | 0.077 (4) | 0.016 (3) | 0.031 (3) | 0.006 (3) |
C3 | 0.071 (4) | 0.071 (4) | 0.074 (4) | 0.015 (3) | 0.022 (3) | 0.019 (3) |
C4 | 0.074 (4) | 0.078 (4) | 0.048 (3) | 0.006 (3) | 0.023 (3) | 0.009 (3) |
C5 | 0.054 (3) | 0.056 (3) | 0.049 (3) | −0.001 (2) | 0.023 (2) | −0.003 (2) |
C6 | 0.061 (3) | 0.086 (4) | 0.047 (3) | −0.002 (3) | 0.023 (3) | −0.008 (3) |
C7 | 0.079 (4) | 0.148 (6) | 0.069 (4) | 0.007 (4) | 0.043 (3) | −0.002 (4) |
C8 | 0.074 (4) | 0.115 (5) | 0.073 (4) | −0.005 (4) | 0.050 (3) | −0.022 (4) |
C9 | 0.067 (4) | 0.085 (4) | 0.096 (4) | 0.016 (3) | 0.040 (4) | −0.002 (4) |
C10 | 0.053 (3) | 0.054 (3) | 0.078 (4) | 0.001 (3) | 0.027 (3) | −0.015 (3) |
C11 | 0.065 (4) | 0.058 (3) | 0.103 (5) | 0.010 (3) | 0.035 (3) | −0.014 (3) |
C12 | 0.075 (4) | 0.062 (4) | 0.123 (6) | 0.018 (3) | 0.031 (4) | 0.006 (4) |
C13 | 0.086 (4) | 0.062 (4) | 0.100 (5) | 0.013 (3) | 0.039 (4) | 0.022 (3) |
C14 | 0.064 (4) | 0.062 (3) | 0.101 (5) | 0.010 (3) | 0.039 (3) | 0.011 (3) |
C15 | 0.048 (3) | 0.059 (3) | 0.062 (3) | −0.010 (2) | 0.018 (2) | 0.008 (2) |
C16 | 0.059 (3) | 0.066 (3) | 0.086 (4) | −0.012 (3) | 0.037 (3) | 0.013 (3) |
C17 | 0.075 (4) | 0.081 (4) | 0.073 (4) | 0.001 (3) | 0.039 (3) | 0.029 (3) |
C18 | 0.060 (3) | 0.075 (3) | 0.053 (3) | 0.002 (3) | 0.023 (3) | 0.018 (3) |
C19 | 0.044 (2) | 0.044 (2) | 0.043 (2) | 0.002 (2) | 0.017 (2) | 0.004 (2) |
C20 | 0.043 (2) | 0.043 (2) | 0.036 (2) | 0.0013 (19) | 0.013 (2) | −0.0004 (19) |
C21 | 0.048 (3) | 0.077 (3) | 0.039 (3) | 0.000 (3) | 0.010 (2) | 0.008 (2) |
C22 | 0.032 (2) | 0.076 (3) | 0.048 (3) | 0.000 (2) | 0.005 (2) | −0.003 (2) |
C23 | 0.041 (2) | 0.059 (3) | 0.061 (3) | −0.005 (2) | 0.026 (2) | 0.000 (2) |
C24 | 0.056 (3) | 0.052 (3) | 0.048 (3) | 0.004 (2) | 0.021 (2) | −0.009 (2) |
C25 | 0.079 (4) | 0.058 (3) | 0.065 (3) | 0.000 (3) | 0.024 (3) | −0.020 (3) |
C26 | 0.088 (4) | 0.058 (3) | 0.072 (4) | 0.022 (3) | 0.031 (3) | −0.012 (3) |
C27 | 0.060 (3) | 0.058 (3) | 0.071 (3) | 0.022 (3) | 0.028 (3) | 0.002 (3) |
C28 | 0.046 (3) | 0.043 (2) | 0.048 (3) | 0.005 (2) | 0.026 (2) | 0.005 (2) |
C29 | 0.127 (6) | 0.120 (6) | 0.060 (4) | 0.021 (5) | 0.029 (4) | 0.019 (4) |
C30 | 0.153 (7) | 0.109 (6) | 0.090 (5) | −0.036 (6) | 0.035 (5) | −0.027 (4) |
O1 | 0.077 (2) | 0.099 (3) | 0.083 (3) | 0.019 (2) | 0.055 (2) | 0.017 (2) |
O2 | 0.101 (3) | 0.117 (3) | 0.088 (3) | 0.043 (3) | 0.052 (3) | 0.050 (3) |
O3 | 0.093 (3) | 0.097 (3) | 0.139 (4) | −0.010 (3) | 0.052 (3) | −0.054 (3) |
O4 | 0.048 (2) | 0.103 (3) | 0.083 (3) | −0.008 (2) | 0.0209 (19) | −0.002 (2) |
O5 | 0.086 (3) | 0.064 (3) | 0.126 (3) | 0.004 (2) | 0.047 (3) | 0.023 (2) |
O6' | 0.35 (3) | 0.078 (9) | 0.108 (11) | −0.018 (13) | −0.038 (14) | −0.023 (7) |
O7' | 0.186 (16) | 0.144 (11) | 0.123 (11) | 0.036 (10) | 0.091 (11) | 0.083 (8) |
O8' | 0.132 (11) | 0.128 (10) | 0.27 (2) | 0.061 (8) | 0.131 (13) | 0.055 (11) |
O6 | 0.065 (7) | 0.076 (9) | 0.152 (15) | −0.040 (6) | 0.031 (8) | 0.007 (7) |
O7 | 0.118 (14) | 0.158 (14) | 0.075 (9) | 0.058 (11) | −0.033 (9) | 0.020 (9) |
O8 | 0.146 (15) | 0.151 (12) | 0.131 (13) | 0.003 (10) | 0.100 (12) | −0.029 (10) |
Ni1—N2 | 1.997 (4) | C2—C3 | 1.368 (7) |
Ni1—N2i | 1.997 (4) | C2—H2A | 0.9300 |
Ni1—N1i | 2.133 (4) | C3—C4 | 1.382 (8) |
Ni1—N1 | 2.133 (4) | C3—H3A | 0.9300 |
Ni1—N4i | 2.184 (4) | C4—C5 | 1.377 (7) |
Ni1—N4 | 2.184 (4) | C4—H4A | 0.9300 |
Ni2—N6 | 1.977 (3) | C5—C6 | 1.466 (7) |
Ni2—N6ii | 1.977 (3) | C6—C7 | 1.363 (7) |
Ni2—N5ii | 2.143 (3) | C7—C8 | 1.391 (8) |
Ni2—N5 | 2.143 (3) | C7—H7A | 0.9300 |
Ni2—N8ii | 2.173 (3) | C8—H8A | 0.9300 |
Ni2—N8 | 2.173 (3) | C9—C10 | 1.540 (8) |
N1—C1 | 1.333 (6) | C9—H9A | 0.9700 |
N1—C5 | 1.343 (5) | C9—H9B | 0.9700 |
N2—N3 | 1.304 (5) | C10—C11 | 1.369 (7) |
N2—C6 | 1.381 (6) | C11—C12 | 1.374 (9) |
N3—C8 | 1.322 (7) | C11—H11A | 0.9300 |
N3—C9 | 1.445 (7) | C12—C13 | 1.364 (9) |
N4—C14 | 1.330 (7) | C12—H12A | 0.9300 |
N4—C10 | 1.355 (6) | C13—C14 | 1.364 (7) |
N5—C15 | 1.341 (5) | C13—H13A | 0.9300 |
N5—C19 | 1.350 (5) | C14—H14A | 0.9300 |
N6—C20 | 1.331 (5) | C15—C16 | 1.372 (7) |
N6—N7 | 1.346 (4) | C15—H15A | 0.9300 |
N7—C22 | 1.345 (5) | C16—C17 | 1.369 (7) |
N7—C23 | 1.452 (5) | C16—H16A | 0.9300 |
N8—C24 | 1.343 (5) | C17—C18 | 1.378 (7) |
N8—C28 | 1.362 (5) | C17—H17A | 0.9300 |
Cl1—O2 | 1.417 (4) | C18—C19 | 1.379 (6) |
Cl1—O1 | 1.423 (3) | C18—H18A | 0.9300 |
Cl1—O3 | 1.423 (4) | C19—C20 | 1.461 (6) |
Cl1—O4 | 1.425 (3) | C20—C21 | 1.382 (6) |
Cl2—O6' | 1.385 (9) | C21—C22 | 1.373 (7) |
Cl2—O7 | 1.390 (9) | C21—H21A | 0.9300 |
Cl2—O7' | 1.393 (8) | C22—H22A | 0.9300 |
Cl2—O8 | 1.407 (8) | C23—C28ii | 1.505 (6) |
Cl2—O6 | 1.414 (7) | C23—H23A | 0.9700 |
Cl2—O5 | 1.418 (4) | C23—H23B | 0.9700 |
Cl2—O8' | 1.423 (8) | C24—C25 | 1.363 (7) |
Cl3—C29 | 1.708 (8) | C24—H24A | 0.9300 |
Cl4—C29 | 1.759 (8) | C25—C26 | 1.370 (7) |
Cl5—C29 | 1.722 (8) | C25—H25A | 0.9300 |
Cl3'—C29 | 1.750 (7) | C26—C27 | 1.374 (7) |
Cl4'—C29 | 1.695 (8) | C26—H26A | 0.9300 |
Cl5'—C29 | 1.721 (7) | C27—C28 | 1.375 (6) |
Cl6—C30 | 1.777 (9) | C27—H27A | 0.9300 |
Cl7—C30 | 1.747 (9) | C28—C23ii | 1.505 (6) |
Cl8—C30 | 1.660 (8) | C29—H29A | 0.9600 |
C1—C2 | 1.363 (7) | C30—H30A | 0.9599 |
C1—H1A | 0.9300 | ||
N2—Ni1—N2i | 173.8 (3) | C6—C7—C8 | 106.1 (5) |
N2—Ni1—N1i | 98.32 (15) | C6—C7—H7A | 127.0 |
N2i—Ni1—N1i | 77.45 (16) | C8—C7—H7A | 127.0 |
N2—Ni1—N1 | 77.45 (16) | N3—C8—C7 | 106.5 (5) |
N2i—Ni1—N1 | 98.32 (15) | N3—C8—H8A | 126.8 |
N1i—Ni1—N1 | 96.02 (19) | C7—C8—H8A | 126.8 |
N2—Ni1—N4i | 97.70 (16) | N3—C9—C10 | 116.6 (5) |
N2i—Ni1—N4i | 86.81 (17) | N3—C9—H9A | 108.1 |
N1i—Ni1—N4i | 163.72 (15) | C10—C9—H9A | 108.1 |
N1—Ni1—N4i | 90.26 (14) | N3—C9—H9B | 108.1 |
N2—Ni1—N4 | 86.81 (17) | C10—C9—H9B | 108.1 |
N2i—Ni1—N4 | 97.70 (16) | H9A—C9—H9B | 107.3 |
N1i—Ni1—N4 | 90.26 (14) | N4—C10—C11 | 120.9 (6) |
N1—Ni1—N4 | 163.72 (15) | N4—C10—C9 | 122.8 (5) |
N4i—Ni1—N4 | 87.7 (2) | C11—C10—C9 | 115.9 (5) |
N6—Ni2—N6ii | 171.7 (2) | C10—C11—C12 | 120.4 (6) |
N6—Ni2—N5ii | 97.35 (13) | C10—C11—H11A | 119.8 |
N6ii—Ni2—N5ii | 77.21 (13) | C12—C11—H11A | 119.8 |
N6—Ni2—N5 | 77.21 (13) | C13—C12—C11 | 118.6 (6) |
N6ii—Ni2—N5 | 97.35 (13) | C13—C12—H12A | 120.7 |
N5ii—Ni2—N5 | 98.95 (19) | C11—C12—H12A | 120.7 |
N6—Ni2—N8ii | 87.29 (14) | C12—C13—C14 | 118.5 (6) |
N6ii—Ni2—N8ii | 98.89 (13) | C12—C13—H13A | 120.8 |
N5ii—Ni2—N8ii | 90.80 (13) | C14—C13—H13A | 120.8 |
N5—Ni2—N8ii | 162.57 (13) | N4—C14—C13 | 124.0 (6) |
N6—Ni2—N8 | 98.89 (13) | N4—C14—H14A | 118.0 |
N6ii—Ni2—N8 | 87.29 (14) | C13—C14—H14A | 118.0 |
N5ii—Ni2—N8 | 162.57 (13) | N5—C15—C16 | 123.1 (5) |
N5—Ni2—N8 | 90.80 (13) | N5—C15—H15A | 118.4 |
N8ii—Ni2—N8 | 83.70 (19) | C16—C15—H15A | 118.4 |
C1—N1—C5 | 117.9 (4) | C17—C16—C15 | 118.6 (5) |
C1—N1—Ni1 | 126.7 (3) | C17—C16—H16A | 120.7 |
C5—N1—Ni1 | 115.2 (3) | C15—C16—H16A | 120.7 |
N3—N2—C6 | 106.0 (4) | C16—C17—C18 | 119.6 (5) |
N3—N2—Ni1 | 133.6 (4) | C16—C17—H17A | 120.2 |
C6—N2—Ni1 | 116.9 (3) | C18—C17—H17A | 120.2 |
N2—N3—C8 | 112.9 (5) | C17—C18—C19 | 118.9 (5) |
N2—N3—C9 | 118.9 (5) | C17—C18—H18A | 120.5 |
C8—N3—C9 | 126.9 (5) | C19—C18—H18A | 120.5 |
C14—N4—C10 | 117.6 (5) | N5—C19—C18 | 122.0 (4) |
C14—N4—Ni1 | 117.8 (3) | N5—C19—C20 | 114.2 (4) |
C10—N4—Ni1 | 124.5 (4) | C18—C19—C20 | 123.8 (4) |
C15—N5—C19 | 117.8 (4) | N6—C20—C21 | 110.0 (4) |
C15—N5—Ni2 | 128.3 (3) | N6—C20—C19 | 114.8 (4) |
C19—N5—Ni2 | 113.2 (3) | C21—C20—C19 | 135.1 (4) |
C20—N6—N7 | 107.1 (3) | C22—C21—C20 | 105.1 (4) |
C20—N6—Ni2 | 119.6 (3) | C22—C21—H21A | 127.4 |
N7—N6—Ni2 | 132.9 (3) | C20—C21—H21A | 127.4 |
C22—N7—N6 | 109.5 (4) | N7—C22—C21 | 108.2 (4) |
C22—N7—C23 | 129.6 (4) | N7—C22—H22A | 125.9 |
N6—N7—C23 | 119.7 (3) | C21—C22—H22A | 125.9 |
C24—N8—C28 | 117.2 (4) | N7—C23—C28ii | 116.5 (4) |
C24—N8—Ni2 | 116.1 (3) | N7—C23—H23A | 108.2 |
C28—N8—Ni2 | 124.5 (3) | C28ii—C23—H23A | 108.2 |
O2—Cl1—O1 | 109.9 (2) | N7—C23—H23B | 108.2 |
O2—Cl1—O3 | 108.8 (3) | C28ii—C23—H23B | 108.2 |
O1—Cl1—O3 | 108.6 (3) | H23A—C23—H23B | 107.3 |
O2—Cl1—O4 | 109.6 (3) | N8—C24—C25 | 123.7 (5) |
O1—Cl1—O4 | 110.8 (2) | N8—C24—H24A | 118.1 |
O3—Cl1—O4 | 109.1 (3) | C25—C24—H24A | 118.1 |
O6'—Cl2—O7 | 117.5 (12) | C24—C25—C26 | 119.1 (5) |
O6'—Cl2—O7' | 110.4 (13) | C24—C25—H25A | 120.5 |
O7—Cl2—O7' | 30.8 (9) | C26—C25—H25A | 120.5 |
O6'—Cl2—O8 | 69.3 (11) | C25—C26—C27 | 118.4 (5) |
O7—Cl2—O8 | 114.8 (10) | C25—C26—H26A | 120.8 |
O7'—Cl2—O8 | 143.5 (9) | C27—C26—H26A | 120.8 |
O6'—Cl2—O6 | 37.2 (11) | C26—C27—C28 | 120.5 (5) |
O7—Cl2—O6 | 106.6 (12) | C26—C27—H27A | 119.7 |
O7'—Cl2—O6 | 84.3 (10) | C28—C27—H27A | 119.7 |
O8—Cl2—O6 | 106.1 (9) | N8—C28—C27 | 121.0 (4) |
O6'—Cl2—O5 | 114.4 (8) | N8—C28—C23ii | 119.9 (4) |
O7—Cl2—O5 | 121.3 (9) | C27—C28—C23ii | 118.8 (4) |
O7'—Cl2—O5 | 105.2 (7) | Cl4'—C29—Cl3 | 75.9 (6) |
O8—Cl2—O5 | 107.7 (7) | Cl4'—C29—Cl5' | 110.7 (6) |
O6—Cl2—O5 | 98.2 (6) | Cl3—C29—Cl5' | 122.6 (6) |
O6'—Cl2—O8' | 121.4 (12) | Cl4'—C29—Cl5 | 115.5 (7) |
O7—Cl2—O8' | 70.7 (10) | Cl3—C29—Cl5 | 115.2 (7) |
O7'—Cl2—O8' | 99.8 (9) | Cl5'—C29—Cl5 | 9.1 (6) |
O8—Cl2—O8' | 57.3 (8) | Cl4'—C29—Cl3' | 116.9 (7) |
O6—Cl2—O8' | 155.8 (8) | Cl3—C29—Cl3' | 41.0 (5) |
O5—Cl2—O8' | 103.6 (5) | Cl5'—C29—Cl3' | 104.5 (5) |
N1—C1—C2 | 123.2 (5) | Cl5—C29—Cl3' | 95.5 (6) |
N1—C1—H1A | 118.4 | Cl4'—C29—Cl4 | 27.9 (7) |
C2—C1—H1A | 118.4 | Cl3—C29—Cl4 | 103.8 (7) |
C1—C2—C3 | 119.0 (5) | Cl5'—C29—Cl4 | 95.9 (5) |
C1—C2—H2A | 120.5 | Cl5—C29—Cl4 | 103.5 (6) |
C3—C2—H2A | 120.5 | Cl3'—C29—Cl4 | 144.8 (6) |
C2—C3—C4 | 119.0 (5) | Cl4'—C29—H29A | 119.8 |
C2—C3—H3A | 120.5 | Cl3—C29—H29A | 114.0 |
C4—C3—H3A | 120.5 | Cl5'—C29—H29A | 110.4 |
C5—C4—C3 | 118.7 (5) | Cl5—C29—H29A | 111.9 |
C5—C4—H4A | 120.6 | Cl3'—C29—H29A | 92.5 |
C3—C4—H4A | 120.6 | Cl4—C29—H29A | 107.1 |
N1—C5—C4 | 122.1 (4) | Cl8—C30—Cl7 | 110.5 (5) |
N1—C5—C6 | 113.4 (4) | Cl8—C30—Cl6 | 109.5 (5) |
C4—C5—C6 | 124.5 (5) | Cl7—C30—Cl6 | 112.9 (5) |
C7—C6—N2 | 108.5 (5) | Cl8—C30—H30A | 107.8 |
C7—C6—C5 | 136.4 (5) | Cl7—C30—H30A | 107.7 |
N2—C6—C5 | 114.9 (4) | Cl6—C30—H30A | 108.4 |
N2—Ni1—N1—C1 | 174.6 (4) | C2—C3—C4—C5 | −0.1 (8) |
N2i—Ni1—N1—C1 | −0.8 (4) | C1—N1—C5—C4 | 1.0 (7) |
N1i—Ni1—N1—C1 | 77.4 (4) | Ni1—N1—C5—C4 | −175.4 (4) |
N4i—Ni1—N1—C1 | −87.6 (4) | C1—N1—C5—C6 | −179.7 (4) |
N4—Ni1—N1—C1 | −170.5 (5) | Ni1—N1—C5—C6 | 3.9 (5) |
N2—Ni1—N1—C5 | −9.4 (3) | C3—C4—C5—N1 | −0.2 (8) |
N2i—Ni1—N1—C5 | 175.2 (3) | C3—C4—C5—C6 | −179.5 (5) |
N1i—Ni1—N1—C5 | −106.6 (3) | N3—N2—C6—C7 | −0.8 (6) |
N4i—Ni1—N1—C5 | 88.4 (3) | Ni1—N2—C6—C7 | 160.8 (4) |
N4—Ni1—N1—C5 | 5.6 (7) | N3—N2—C6—C5 | −177.3 (4) |
N2i—Ni1—N2—N3 | −143.8 (4) | Ni1—N2—C6—C5 | −15.7 (6) |
N1i—Ni1—N2—N3 | −97.0 (4) | N1—C5—C6—C7 | −168.1 (7) |
N1—Ni1—N2—N3 | 168.6 (5) | C4—C5—C6—C7 | 11.2 (10) |
N4i—Ni1—N2—N3 | 80.1 (4) | N1—C5—C6—N2 | 7.1 (6) |
N4—Ni1—N2—N3 | −7.2 (4) | C4—C5—C6—N2 | −173.6 (5) |
N2i—Ni1—N2—C6 | 61.0 (4) | N2—C6—C7—C8 | 1.4 (7) |
N1i—Ni1—N2—C6 | 107.8 (4) | C5—C6—C7—C8 | 176.8 (6) |
N1—Ni1—N2—C6 | 13.4 (4) | N2—N3—C8—C7 | 1.0 (7) |
N4i—Ni1—N2—C6 | −75.1 (4) | C9—N3—C8—C7 | 167.7 (6) |
N4—Ni1—N2—C6 | −162.4 (4) | C6—C7—C8—N3 | −1.4 (7) |
C6—N2—N3—C8 | −0.2 (6) | N2—N3—C9—C10 | −50.7 (7) |
Ni1—N2—N3—C8 | −157.3 (4) | C8—N3—C9—C10 | 143.4 (6) |
C6—N2—N3—C9 | −168.0 (5) | C14—N4—C10—C11 | −1.3 (7) |
Ni1—N2—N3—C9 | 34.9 (7) | Ni1—N4—C10—C11 | 175.6 (4) |
N2—Ni1—N4—C14 | 173.0 (4) | C14—N4—C10—C9 | 170.8 (5) |
N2i—Ni1—N4—C14 | −11.3 (4) | Ni1—N4—C10—C9 | −12.3 (7) |
N1i—Ni1—N4—C14 | −88.7 (4) | N3—C9—C10—N4 | 40.3 (8) |
N1—Ni1—N4—C14 | 158.3 (5) | N3—C9—C10—C11 | −147.2 (5) |
N4i—Ni1—N4—C14 | 75.1 (4) | N4—C10—C11—C12 | 2.0 (8) |
N2—Ni1—N4—C10 | −3.9 (4) | C9—C10—C11—C12 | −170.7 (5) |
N2i—Ni1—N4—C10 | 171.8 (4) | C10—C11—C12—C13 | −0.9 (9) |
N1i—Ni1—N4—C10 | 94.4 (4) | C11—C12—C13—C14 | −0.6 (9) |
N1—Ni1—N4—C10 | −18.6 (7) | C10—N4—C14—C13 | −0.3 (8) |
N4i—Ni1—N4—C10 | −101.8 (4) | Ni1—N4—C14—C13 | −177.4 (5) |
N6—Ni2—N5—C15 | −179.3 (4) | C12—C13—C14—N4 | 1.3 (9) |
N6ii—Ni2—N5—C15 | 7.0 (4) | C19—N5—C15—C16 | −0.6 (7) |
N5ii—Ni2—N5—C15 | 85.1 (4) | Ni2—N5—C15—C16 | 169.0 (4) |
N8ii—Ni2—N5—C15 | −151.6 (4) | N5—C15—C16—C17 | 1.0 (8) |
N8—Ni2—N5—C15 | −80.4 (4) | C15—C16—C17—C18 | −0.8 (9) |
N6—Ni2—N5—C19 | −9.3 (3) | C16—C17—C18—C19 | 0.3 (8) |
N6ii—Ni2—N5—C19 | 177.0 (3) | C15—N5—C19—C18 | 0.0 (6) |
N5ii—Ni2—N5—C19 | −104.9 (3) | Ni2—N5—C19—C18 | −171.2 (4) |
N8ii—Ni2—N5—C19 | 18.4 (6) | C15—N5—C19—C20 | −179.3 (4) |
N8—Ni2—N5—C19 | 89.6 (3) | Ni2—N5—C19—C20 | 9.6 (4) |
N6ii—Ni2—N6—C20 | 57.0 (3) | C17—C18—C19—N5 | 0.2 (7) |
N5ii—Ni2—N6—C20 | 105.2 (3) | C17—C18—C19—C20 | 179.3 (5) |
N5—Ni2—N6—C20 | 7.6 (3) | N7—N6—C20—C21 | 2.2 (5) |
N8ii—Ni2—N6—C20 | −164.3 (3) | Ni2—N6—C20—C21 | 175.5 (3) |
N8—Ni2—N6—C20 | −81.1 (3) | N7—N6—C20—C19 | −178.2 (3) |
N6ii—Ni2—N6—N7 | −131.7 (4) | Ni2—N6—C20—C19 | −4.8 (5) |
N5ii—Ni2—N6—N7 | −83.5 (4) | N5—C19—C20—N6 | −3.7 (5) |
N5—Ni2—N6—N7 | 178.9 (4) | C18—C19—C20—N6 | 177.0 (4) |
N8ii—Ni2—N6—N7 | 6.9 (4) | N5—C19—C20—C21 | 175.8 (5) |
N8—Ni2—N6—N7 | 90.1 (4) | C18—C19—C20—C21 | −3.4 (8) |
C20—N6—N7—C22 | −2.1 (5) | N6—C20—C21—C22 | −1.4 (5) |
Ni2—N6—N7—C22 | −174.1 (3) | C19—C20—C21—C22 | 179.0 (5) |
C20—N6—N7—C23 | −171.2 (4) | N6—N7—C22—C21 | 1.2 (5) |
Ni2—N6—N7—C23 | 16.7 (6) | C23—N7—C22—C21 | 169.0 (4) |
N6—Ni2—N8—C24 | −25.2 (3) | C20—C21—C22—N7 | 0.1 (5) |
N6ii—Ni2—N8—C24 | 160.3 (3) | C22—N7—C23—C28ii | 145.4 (5) |
N5ii—Ni2—N8—C24 | 133.3 (4) | N6—N7—C23—C28ii | −48.0 (6) |
N5—Ni2—N8—C24 | −102.3 (3) | C28—N8—C24—C25 | −0.7 (7) |
N8ii—Ni2—N8—C24 | 61.1 (3) | Ni2—N8—C24—C25 | −164.8 (4) |
N6—Ni2—N8—C28 | 172.0 (3) | N8—C24—C25—C26 | 1.8 (8) |
N6ii—Ni2—N8—C28 | −2.5 (3) | C24—C25—C26—C27 | −1.1 (8) |
N5ii—Ni2—N8—C28 | −29.5 (6) | C25—C26—C27—C28 | −0.5 (8) |
N5—Ni2—N8—C28 | 94.8 (3) | C24—N8—C28—C27 | −1.0 (6) |
N8ii—Ni2—N8—C28 | −101.8 (3) | Ni2—N8—C28—C27 | 161.7 (4) |
C5—N1—C1—C2 | −1.5 (7) | C24—N8—C28—C23ii | 173.0 (4) |
Ni1—N1—C1—C2 | 174.4 (4) | Ni2—N8—C28—C23ii | −24.3 (5) |
N1—C1—C2—C3 | 1.2 (8) | C26—C27—C28—N8 | 1.6 (7) |
C1—C2—C3—C4 | −0.3 (8) | C26—C27—C28—C23ii | −172.5 (5) |
Symmetry codes: (i) −x, y, −z−1/2; (ii) −x+1, y, −z+1/2. |